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By Vinod K. Sikka, René Cooper

"Cohoes, New York 12047 Intermetallics are an attractive class of advanced materials. The aluminide intermetallics offer advantages including: (1) lower density, (2) oxidation resistance, (3) carburization resistance, and (4) interesting mechanical properties because of their ordered crystal structure. Even though the attractive properties of the aluminides and other intermetallics have been known for nearly four decades, their practical applications have not been developed for two reasons: (1) the poor ductility (in some cases, both ambient and high temperatures) and (2) the lack of processability into meaningful components. Recent advances such as ductilization of Ni3Al by small additions of boron and the knowledge that environmental effects are the major cause of poor ductility in Fe3Al and FeAl systems have brought the intelmetallics into the forefront of research and their commercial applications. This paper has described a method for melting Ni3AI-based alloys that successfully utilize the exotherrn for the formation of NiAl from the elemental materials. The reaction-synthesis method has also been utilized for the production of NiAI and NiAI-based alloy powders from the elemental powders. The reaction-synthesized powders of NiAI and NiAI-based alloys were consolidated by hot extrusion and evaluated for tensile properties over a temperature range from room temperature to 1050ºC. The powder-processing conditions have been found to have more influence on the ductile-to-brittle transition temperature of NiAI than the powder-production method.IntroductionIntermetallics are an attractive class of advanced materials [1-11]. The alum in ide interrnetallics offer advantages including: (1) lower density, (2) oxidation resistance, (3) carburization resistance, and (4) interesting mechanical properties because of their ordered crystal structure. Even though the attractive properties of the aluminides and other interrnetallics have been known for nearly four decades, their practical applications have not been developed for two reasons: (I) the poor ductility (in some cases, both ambient and high temperatures) and (2) the lack of processability into meaningful components. Recent advances such as ductilization of Ni3Al by small additions of boron and the knowledge that environmental effects are the major cause of poor ductility in Fe3Al and FeAl systems have brought the intermetallics into the forefront of research and their commercial applications. The paper will briefly review the processing techniques being pursued for the commercial applications of Ni3Al-based intermetallics. The major emphasis of the paper will deal with synthesis of Ni3Al and NiAI intelmetallics."

Jan 1, 1994

By A. Kar, J. Mazumder

"Inherent rapid cooling in laser processing often produces novel materials due to nonequilibrium partitioning during solidification. This paper reports theoretical and experimental investigations on in situ alloy formation with extended solid solution.A mathematical model for determining the composition of metastable alloys and the effects of various process parameters on the composition of extended solid solution is presented. To model the nonequilibrium partitioning of solute in concentrated solution, rate equations and conservation of mass equations are used and an expression for nonequilibrium partition coefficients is derived for concentrated solution, which is realistic for laser alloying and cladding. Effect of rapid cooling on solute segregation is presented by deriving an expression for nonequilibrium partition coefficient.Experiments were performed with Ni-AI and Ni-Hf systems to obtain the composition of solute in the extended solid solution produced during laser cladding."

Jan 1, 1988

By P. G. McCormick

The refining of rare earth metals by the direct solid state reduction of their respective chlorides during mechanical alloying has been studied. Erbium and gadolinium were synthesised by milling their respective chlorides with calcium. The mechanical alloying of SmC13 with calcium resulted in partial reduction of SmC12. Examination of the milled powders using X- ray diffraction and analytical electron microscopy has enabled characterisation of product structure and morphology. The synthesis of Fe17Nd2 by the mechanical alloying of NdC13 and Fe with calcium has also been studied. The Fe17Nd2 phase forms during heat treatment of the mechanically alloyed powder.

Jan 1, 1992

By Nathalie Neveux

For the first time, dehydrated ferrous sulfate was successfully used for the dry synthesis of potassium ferrate. In addition, ferrate ion is stabilized as a solid solution where hexavalent iron is partially substituted by S(V1) leading to a sulfato-ferrate having the following formula K2(Fe,S)04. This substance has an efficient life time of about six months. Ferrate ion is a powerful oxidant ( EO = 2.2V ), a bactericidal agent and possesses coagulant, flocculant properties. Its reduction generates nascent oxygen, hydroxyl groups and Fe(OH)3. Alkali metal ferrate is probably the future global agent for water treatment. Applications of this material in the field of urban and industrial effluents treatment have been investigated. Heavy metals cations such as Cu, Cd, Mn, Ni, Pb, Zn, ... were successfully removed. The results of sulfato-ferrate use for cyanide destruction, decrease in COD, soil, discoloration of pulp and paper effluents will be summarized.

Jan 1, 1999

By V. I. Lakshmanan, R. Roy

"TiO2 is used in paints, plastics, rubber, paper, inks, textiles and other miscellaneous applications. The demand for the pigment grade Ti02 is growing at 3.0%/year on average and this invites the development of innovative and cost effective processes. The current processes are not designed to recycle the reagents and thereby discharge the effluents into the environment, causing an environmental concern.During this study, synthesis of TiO2 from an ilmenite concentrate was investigated using an innovative atmospheric mixed-chloride leach process. The solution purification was carried out using solvent extraction in two stages. In the first stage iron removal was carried out and in the second stage titanium was extracted. The strip solution obtained from the second stage solvent extraction contained the purified titanium and from this stream pigment grade Ti02 was recovered. The barren solution was used for reagent recovery and the regenerated leach liquor was recycled."

Jan 1, 2011

By F. H. Froes, O. N. Senkov, N. Srisukhumbowornchai

"Mechanical alloying (MA) and thermohydrogen processing (THP) approaches were used to synthesize amorphous or nanocrystalline powders of the titanium-aluminide-based alloys and composites. Fully dense samples with nanocrystalline and bimodal structures were produced from these powders by hot isostatic pressing. The stability of the microstructures during continuous heating at high temperatures was studied. Characterization techniques including X-ray diffraction, scanning and transmission electron microscopy, energy dispersive spectroscopy, and differential thermal analysis were used in this work.IntroductionAs performance demands increase, so do the demands for enhanced mechanical property combinations at reduced overall weight; and reduced weight can most efficiently be realized by the use of low-density metals with high specific strength, such as titanium alloys and titanium-aluminum intermetallics [l]. The TiAl-based alloys are attractive for high temperature applications, however, they exhibit poor ambient temperature ductility and fracture toughness [2-4]. Incremental improvements can be obtained using ingot metallurgy processing [1,2] but more substantial developments require ""far from equilibrium"" (FFE) synthesis [5-8] which allows development of novel constitutional and microstructural effects, leading to enhanced physical and mechanical properties. Improved ductility of titanium aluminide intermetallics can be achieved by disordering, grain refinement and deoxidation of the matrix, while good elevated temperature properties are achieved due to a dispersion of fine, thermodynamically stable, second phase particles.The approaches for producing nanocrystalline and amorphous TiAl-based alloys and composites used in this work included FFE powder metallurgy techniques such as rapid solidification, mechanical alloying and thermohydrogen processing. The rapid solidification (RS) technique allows extension of solubility limits, production of novel phases, and much more refined microstructures (down to nanostructure or even amorphous range) than is possible using the ingot metallurgy technique [9]. Mechanical alloying (MA) is a process in which heavy working of powder particles results in intimate alloying by repeated deformation, fracturing and welding. This process can produce greater departure from FFE than RS, leading to greater refinement effects; and additionally allows production of a dispersion of second phase particles [10]. Thermohydrogen processing involves hydrogen as a temporary alloying element in titanium to facilitate processes, refine microstructure, and improve final mechanical properties [11]; it was used in the present work to improve MA process. The combination of these three processes was expected to control the final microstructure even better than either process used alone."

Jan 1, 1998

By Hongbo Zhu, Kun Yang, Jingyan Jia, Jinhui Peng, Libo Zhang, Yi Xia

"Titanium dioxide is broadly considered as the most potential useful photocatalytic material. In this work, titanium dioxide was synthetized by microwave solid-state method and characterized by thermogravimetry-differential scanning calorimetry (TG-DSC), X-ray diffraction (XRD) and scanning electron microscopy (SEM). The result demonstrates that through microwave solid-state synthesis, we can obtain uniform size and anatase TiO2 photocatalyst, with the precursor being Ti(C2O4)2·2H2O. And its degradation kinetic parameter of MO can reach to 0.21232.IntroductionSince Fujishima and Honda found the photovoltaic property of titanium dioxide TiO2 [l], it has been widely used in the field of pollutant degradation, virus killer and environment protection [2-5]. Compared to other semiconductors, TiO2 has the advantage of low toxicity/cost, chemical stability, excellent photocatalytic activity, and long lifetime of electron/hole pairs, thus it is considered to be a most potential useful photocatalyst material [ 6]. Solid-state synthesis of oxide nanoparticle is a new method developed in recent years, which not only overcomes the shortcomings of easily aggregation existing in traditional hydrometallurgical process, but also fully demonstrates the unique technologic advantages of without solvents, high yield, easy control, less environmental pollution in solid-state reaction [7-11]. Researches show that the new method of microwave synthesis shows a lot of advantages such as fast reaction rate, efficient, high purity of product, uniform morphology, energy-efficient, and nonpolluting [12-15].In this work, we associated microwave heating and solid-state synthesis to prepare TiO2 photocatalyst material. Its photocatalytic activity was studied in the degradation of MO queous solution. Meanwhile, the formation process as well as the crystal structure and morphology of the synthesized powders were characterized by means of chermogravimetrydifferential scanning calorimetry (TG-DSC), X-ray diffractometry (XRD) and scanning electron microscopy (SEM) techniques."

Jan 1, 2014

By Patrick R. Taylor

Titanium nitride has been synthesized in a thermal plasma reactor from ilmenite ore concentrate using methane and ammonia as the reactive gases. The product has been characterized by x-ray diffraction and SEM. Results show that a high concentration of methane favors the formation of iron, titanium nitride and titanium carbonitride. The formation of titanium carbonitride can be minimized by controlling the concentration of methane. The formation of TiN proceeds by the progressive reduction of the oxides of titanium to titanium, which is converted to titanium nitride.

Jan 1, 1998

By Takeo Fujino, Nobuaki Sato, Yarong Wang, Kohta Yamada

"Ternary mixed sulfides of some transition metals MTS3 (M=Ba, ·Pb, T=Ti, Zr) were synthesized by a relatively low temperature process using sulfur melt. The mixture of starting materials, such as, metals and/or binary sulfides and a large excess of sulfur was reacted in a vacuum-sealed Pyrex or quartz ampoule at 350- 600 °C for one to three weeks. After the reaction, the remaining sulfur was completely removed by a process composed of filtration of sulfur melt and followed dissolution in CS2• The binary sulfides impurities coexisted in the products were removed by rinsing the products in water and acetone. By using the above method, BaTiS3, PbTiS3 and BaZrS3 'Were obtained in pure form. The effect of addition of halides on the yields of these ternary sulfides were also discussed.IntroductionThere have been a vast number of studies on the preparation and physical and /or chemical properties of mixed metal oxides. As is well known, some of such compounds exhibit excellent materials properties, causing them for use in mechanical, electronic, magnetic and chemical devices. Not a few mixed metal sulfides show similar physico-chemical properties to those of the corresponding mixed metal oxides. However, the study of the mixed sulfide crystals is rather sparse mainly due to difficulties in preparing these compounds. In various methods which have been adopted for preparing mixed sulfides, the simplest method would be the solid-solid reaction of the component binary sulfides or elements. However, there are always diffusional constraints with regard to the reactions in solid phases causing it necessary to heat the reactants at sufficiently high temperatures, viz. 800-1200°C. On the other hand, some mixed sulfides are unstable at high temperatures or to change their materials properties due to sulfur nonstoichiometry and structural modification depending on temperature, i.e., synthesis of such compounds needs to be made at lower temperatures. Processing in alkali halide melts is hopeful to overcome the above problems but to obtain the halide melts the temperatures above ~ 600 °C is needed. Low temperature reaction has been carried out for the preparation of Hg1.24TiS4, which was formed by the ·combination of TiS2 and molten Hg metal at 320°C[l]. Reaction of WS2 with LiBH4 melt at 350°C yielded LixWS2[2]. These sophisticated methods, however, can be applied only to the vary special cases."

Jan 1, 2000

By Hong Liang-shi

Olivine lithium iron phosphate (LiFePO4) is considered as one of the most promising materials for lithium-ion secondary batteries because of its high theoretical capacity, low cost, good safety, benign environment and good cycle performance. In this paper, carbon-free and/or carbon-coated olivine lithium iron phosphate composite ultrafine powders were successfully synthesized from aqueous precursor solutions of (NH4)2Fe(SO4)2?6H2O, H3PO4 and LiOH?H2O by co-precipitation method. The obtained LiFePO4 or LiFePO4/C powders were characterized by X-ray diffraction (XRD) and scanning electron microscope (SEM). Their electrochemical performance was investigated in terms of cycling behavior. As confirmed by X-ray diffraction and scanning electron microscope, the material obtained by co-precipitation within the temperature range of 60ºC to 100ºC and then followed by moderate heat treatment are a single-phase olivine LiFePO4with the particle size of about 300nm. An improved carbon-coated olivine LiFePO4/C material was prepared by adding conductive carbon materials, such as glucose, activated carbon and acetylene black, into the precursor. The carbon dispersed in the materials increases the electronic conductivity of LiFePO4/C composite, and consequently, leads to high rechargeable capacity of the material. The carbon-coated material with carbon amount of 7.64%wt obtained from glucose has the first discharge capacity of 150.3mAh/g at the rate of 0.1C and 129.3mAh/g at the rate of 1.0C, respectively. After cycled for 50 times, the capacity retention rate is 95.13% at the rate of 1.0C in the voltage range of 2.5 to 4.3 V vs. Li/Li+.

Jan 1, 2006

By H. Y. Sohn, S. PalDey

"Fine particles of nickel aluminides and Ni4Mo were synthesized by reducing mixtures of, respectively, A1Cl3 + NiC12 and NiC12 + MoC12 vapors with hydrogen. Though thermodynamically favorable, the coreduction of NiC12 and A1Cl3 by H2 to form Ni3Al did not readily happen experimentally. The addition of a small amount of aluminum vapor was needed to initiate the coreduction reaction. The product particles as observed by TEM were very fine but usually agglomerated. The electron diffraction pattern of particles identified NiAl and NiA13 along with Ni3Al and metallic Ni. The content of Ni3Al was maximized at 52 mol% at 1050°C under the partial pressures ofH2, A1Cl3, and NiC12 at 57, 1.4, and 0.5 kPa, respectively. When a mixture of NiC12 + MoC15 was reduced by hydrogen, Ni4Mo particles with some Ni or Mo particles were obtained, the maximum content of Ni4Mo obtained being 93 mol % . The particle size was in the range of 100 to 200 nm. An Ni4Mo coating of 700 nm thickness on an Ni substrate was also prepared.IntroductionThe search for new high-temperature structural materials has stimulated much research on intermetallic compounds. Nickel aluminides have low densities, relatively high melting points, and good high-temperature strength properties. They show an increase, rather than a decrease, in yield strength with increasing temperature (1). Ni4Mo is also of interest as a high-temperature structural material. The major shortcomings of these intermetallics are their inherent brittleness at room temperature when they are in polycrystalline form. For much the same reason, the conventional casting of intermetallics is difficult. Ingot metallurgy and powder metallurgy are two other processing techniques. The first technique is quite energy consuming. In powder metallurgy, the powders of metals and alloys are consolidated in near net shape and then subjected to secondary processing. It would, therefore, be advantageous if intermetallic compounds can be produced in fine powder form from inexpensive raw materials, using less energy."

Jan 1, 1998

By Seiji Yokoyama

As a series of fundamental study on the gas evaporation method, a levitation-melted aluminum was evaporated in the gas mixture of argon and ammonia to synthesize ultrafine particles of aluminum nitride. When the ammonia partial pressure were more than 2kPa, the formation ratio of aluminum nitride was about 95%. The particles of aluminum nitride were mainly hexagonal. The mean size of the particles of aluminum nitride was about 57 nm, and it was constant without depending on the temperature of the levitated aluminum and the partial pressure pf ammonia. The aluminum nitride was formed by the reaction between ammonia and condensed liquid aluminum particle whose size was relatively small.

Jan 1, 2006

By H. Y. Sohn, S. PalDey

"A new chemical synthesis process for the preparation of intermetallic compounds has been developed. It involves the vapor-phase reduction of mixtures of constituent metal chlorides by magnesium vapor to produce intermetallic compounds in the form of fine powder. The advantages of the process include (a) the use of inexpensive raw materials, (b) low reaction temperatures, and (c) products in the form of fine particles. Titanium and nickel aluminides were prepared by this method. The effect of AlCl/TiCl3 partial pressure ratio on the formation of different titanium aluminides was studied. A two-phase mixture containing 80 mol % of TiAl and 20 mol % of TiA13 formed at an AlC13/TiC13 ratio of 10. The amount of TiA13 was maximized to 72 mol% at an AlC13/TiC13 ratio of 16. The maximum conversion of the limiting chloride TiCl3 was 94 % . In the case of nickel aluminides, NiAI, NiAl3, and Ni2Al3 were formed by reducing mixtures of NiC12 and A1Cl3 vapors. The effect of the partial pressure ratios AlCl3/NiC12 and Mg/NiC12 on the formation of nickel aluminides was studied. The maximum content of NiAl obtained was 98 mol % . At the AlC13/NiC12 ratio of 19, a two-phase mixture of 17 mol% of NiAl and 83 mol% of NiA13 was produced. The product particles were very fine in the size range of 0.05 to 0.2 µm.A. IntroductionIntermetallic compounds are attracting much attention [1]. Titanium and nickel aluminides have attracted a great deal of attention from the aerospace as well as automobile industries because of their potential for high-temperature application (e.g., low density, good oxidation resistance, and high-temperature strength retention [2, 3]). Gamma TiAl and two-phase (TiAl and Ti3Al) alloys [4] are used for gas turbine engine rotational components as well as automobile exhaust valves. TiAl3 is one of the most extensively investigated aluminum-rich intermetallics. Nickel aluminides are attractive because of their low densities, relatively high melting point and good high-temperature strength properties. For example, Ni3Al shows increasing rather than decreasing yield strength with increasing temperature [5]."

Jan 1, 1998

By Jin-Chun Kim

Nanosized W based powders (W, WC, WC-Co) were produced by chemical vapor condensation (CVC) process. Two different solid W(CO)6 and Co2(CO)8 metal-organic materials were used as precursors. CVC experiment was conducted in the temperature range of 400-1100. As-CVC WC1-x powder which had non-stoichiometric composition was carburized by using of the CH4-H2 mixed gas in temperature range of 750-850. The CVC W and WC1-x powders showed loosely agglomeration structure, and the Co powder had intricate long stand structure because of intrinsic magnetic properties of Co phase. Carbon content of the CVC powders controlled by gas-phase carburization was well matched with theoretical WC stoichiometry (6.13wt%).

Jan 1, 2006

By Milton Manrique, Edgar E. Vidal, Patrick R. Taylor

"Ultrafine zirconium carbide powder has been synthesized using zircon concentrate and methane in a thermal plasma reactor. The effect of several experimental variables, such as power used and zircon particle size, on the conversion has been studied. A thermodynamic analysis of the possible reactions and stable compounds was performed. A mathematical model that describes the in-flight decomposition of zircon particles was developed based on a description of the temperature and velocity profiles calculated in the reactor. It was shown that the formation of zirconium carbide from zircon and methane is thermodynamically possible. Complete 'vaporization of zircon in the reactor is predicted when the particle size is below 45flm and the effective power entering the reactor is 15 kW. The powders were collected and characterized by XRD, SEM, TEM and chemical analysis using ICP. Results of the product analysis indicated the presence of zirconium carbide, zirconium oxide, silicon carbide and silicon oxide.IntroductionIn recent years there has been an increased interest in the production of nanometric sized powders of ceramic materials for use in advanced materials applications. One possible method to produce these powders is with a thermal plasma reactor, which offers high temperatures and fast quenching rates. This technology has been called - Thermal Plasma Synthesis - [1].Zirconium Carbide (ZrCx) has typical properties of transition metal carbides: elevated hardness - between alumina and diamond - a high melting temperature of 3420°C and high chemical stability at room temperature [2]. ZrCx has a Bl crystal structure with deficiencies in the number of carbon atoms in the cell with x between 0.6 and 1 [3]. Different methods have been used to produce ZrC, one method is by direct reaction of zirconium hydride or halide with carbon. Other methods used are direct reduction and carburization of zirconium oxide (Zr02) and reaction of metallic zirconium with a caburizing gas such as acetylene [3]. Recently small films of ZrC have been obtained using a sputtering device [4,5]. ZrC has been used in nuclear plants as a low neutron absorbing and high mechanical resistant refractory material and also as a constituent in cathodes made of UC-ZrC [6]. It is also used in the form of tubes, boats and crucibles to handle molten metals and as part of electronic devices used for thermoionic transducers. Recently ZrC has been used along with zirconium diboride (ZrB2) to produce composite materials [7,8]."

Jan 1, 1996

By P. Lussiez

Precipitates consisting of amorphous ferrihydrite and crystalline goethite have been prepared by aging hydrolyzed Fe (III) solutions at room temperature. The precipitates have been characterized by x-ray diffraction and differential thermal analysis. The amorphous ferrihydrite transforms to goethite with time. The ferrihydrite to goethite transformation is affected by the presence of small amounts of copper or nickel coprecipitated with the iron. .The addition of copper decreases the amount of goethite at a given aging time and increases the amount of coprecipitate which is initially dissolved in sulfuric acid, but it does not seem to affect the dissolution of the crystalline part'. It is proposed that adsorption of copper hydroxo species on goethite nuclei delays the ferrihydrite to goethite transformation. The effect of nickel is less dramatic than that of copper. Apparently a portion of the added nickel is adsorbed on the goethite crystallite surface rather than incorporated into the goethite lattice.

Jan 1, 1981

By Phillip B. Messersmith, Emmanuel P. Giannelis

"A versatile in-situ polymerization approach is described for the synthesis of polymerceramic nanocomposites consisting of two-dimensional layers of mica-type silicate (MTS) within polymer matrices. Functionalized, organically modified mica-type silicates (OMTS) were used to promote delamination/dispersion of the host layers and initiate polymerization of organic rrionomer. Epoxy nanocomposites prepared in this manner exhibit substantial modulus reinforcement at low silicate loadings. The water vapor permeability of the poly(?-caprolactone) nanocomposite containing 4.8% silicate by volume was reduced by nearly an order of magnitude compared to pure poly (?-caprolactone).IntroductionPolymer matrix nanocomposites are a relatively new class of materials with dimensions typically in the range of 1-100 nm.1 In general, because of the ultrafine phase dimensions involved, nanocomposites exhibit new and improved properties when compared to their micro- or macrocomposite counterparts. We as well as others are currently investigating the design, synthesis and characterization of polymer-ceramic nanocomposites. Our effort, in particular, has focused on the use of mica-type silicates (MTS) with various thermoplastic and thermosetting matrices.2-5MTS's belong to the general family of 2: 1 layered silicates. Their crystal structure consists of layers of two silica tetrahedral sheets fused to an edge-shared octahedral sheet of either aluminum or magnesium hydroxide. Stacking of the layers leads to a regular van der Waals gap or interlayer.6 Isomorphic substitution within the layers generates negative charges that are counterbalanced by cations residing in the interlayers. Although the natural forms of MTS's usually contain hydrated Na+ or K+ ions, ion exchange reactions with organic cations (e.g. alkylammonium ions) can render the normally hydrophilic MTS's organophilic."

Jan 1, 1994

By Gopalakrishna B. Prabhu, David L. Bourell

"Three mol% Yttria-Stabilized Tetragonal Zirconia (YSTZ) was prepared by a sol-gel synthesis technique using zirconium tetrachloride and hydrated yttrium chloride precursors. After drying and annealing at 823K, the particle size was in the range 10 to 20 nm. The zirconia powder was sintered using a uniaxial hot press at an applied stress of 20 to 40 MPa. One hour, isothermal sintering was performed in air after initial heating at 50K/min. Theoretical density was obtained at densification temperatures above 1498K. After sintering, grain coarsening characteristics were studied using constant heating rate anneals followed by quenching, based on a model for grain coarsening in a linear heating rate cycle. The microstructural change was studied using SEM and TEM and the phases were determined using x-ray diffraction.IntroductionThe ability to sinter nanocrystalline materials to full density several hundred degrees below the normal sintering temperatures is one reason for their current interest. [1-5] Yttria Stabilized Tetragonal Zirconia (YSTZ) of grain size of about 300 nm has exhibited superplasticity, with elongations as large as 800%.[6-7] Fine grain size is critical for superplasticity. Retention of the fine grain size during sintering of nanocrystalline powder is important if a material is to exhibit superplasticity or to exhibit physical or mechanical properties associated with the ultra fine structure. This paper investigates the sintering behavior and the grain coarsening characteristics ofnanocrystalline YSTZ.Techniques for synthesizing nanocrystalline materials have been studied in great detail earlier. [8-12] The techniques used to synthesize nanocrystalline zirconia include alkoxide synthesis [9], the chloride method [11], the peroxide method [13] and the acetone-toluene method. [13] In this paper the method used in the synthesis of zirconia is the chloride technique. With this precipitation technique, either zirconium chloride or oxychloride and a corresponding yttrium salt or even pure yttria are used."

Jan 1, 1994

By H. Kung, T. R. Jervis, M. Nastasi, T. E. Mitchell

"A systematic study of the structure-mechanical properties relationship is reported for nanolayered composites of MoSh-SiC, Mo-MoSh, Mo-MoShNx, MoSi2-MoSi2Nx, and Mo-MoShMoSi2Nx (x=3-4) synthesised by sputtering techniques. These composites have been studied by nano-indentation and cross-sectional TEM as a function of annealing temperature. As-deposited layers are amorphous except for Mo. With increasing annealing temperature, first MoSh and then SiC crystallize, while the hardness progressively increases until the layers start to spheroidize and grain growth sets in at 900ºC. For the case of Mo-MoSi2, the layers react and the composite deteriorates rapidly. However, MoSi2Nx remains amorphous up to 1000ºC, suggesting that it could act as a diffusion barrier between Mo and MoSi2. In fact the Mo. MoSi2Nx, MoSi2-MoSi2Nx and Mo-MoSi2-MoSi2Nx nanolayers are found to remain stable up to such temperatures. IntroductionMolybdenum dislicide, MoSh, is a potential matrix material for high temperature structural composites due to its high melting point and good oxidation resistance at elevated temperature [1]. The two major drawbacks for structural applications are inadequate high temperature strength and poor low temperature ductility. Silicon Carbide (SiC) being hard and thermally compatible with most ceramics and intermetallic compounds, has been found to be suitable for second phase reinforcement in various structural applications and, in particular, the addition of SiC whiskers improves the high temperature yield strength of MoSi2 [2]. While most of the research in MoSb-SiC composites has been on the particulate form of SiC, laminated composites may offer unique properties. It has been shown that synthetic multilayers with alternating layers of metal and/or compounds may exhibit interesting mechanical properties [3]. Enhancement in mechanical properties by decreasing the wavelength of multilayer spacing has been studied extensively. In general, two types of strengthening have been proposed: (1) Hall-Petch strengthening [4,5], where the strength increase is inversely proportional to the square root of the layer thickness; (2) Koehler modulus strengthening [6], which increases with modulus difference and decreasing layer thickness. In the present study, we have performed a systematic study of the relationship between strength and structure in a number of different nanolayered systems based on MoSh. Layer thicknesses have been varied and their nanostructures have been varied by heat treatment. Previous work on MoSi2-SiC is summarized [7]. In an attempt to improve fracture toughness, MoSh-Mo nanolayered materials have been prepared but are found to react and deteriorate. Previous work has shown that nitrided MoSi2 (MoSi2Nx with x=3-4) is highly stable [8] and so nanolayered composites of MoSi2-MoSi2Nx and Mo-MoSi2-MoSi2Nx have been prepared to assess the' stability and mechanical properties of these composites. Preliminary results are presented."

Jan 1, 1994

By Xi Dai

The LiFe1-xNixPO4(x=0, 0.05, 0.10) cathode materials for Li-ion battery were synthesized with Fe1xNixC2O4?2H2O(x=0, 0.05, 0.10) as Fe sources by high temperature solid-state reaction method. The Fe1xNixC2O4?2H2O(x=0, 0.05, 0.10) materials were produced by liquid co-precipitation method and crystal structure and morphology of cathode materials were characterized by X-ray diffraction and scanning electron microscopy. The composition contents and charge-discharge performances were measured by chemistry analysis and charge-discharge apparatus. The XRD patterns showed that LiFe1-xNixPO4(x=0, 0.05, 0.10) cathode material samples were well-crystallized homogeneous olivine-type phase, with only tiny trivalent iron impurities according to chemistry analysis results. Charge-discharge test showed that cathode materials possessed excellent charge/discharge capacities, about 150mAh/g at 0.1C rate and more than 120mAh/g at 0.4C rate. The polarization of cathode in charge-discharge process can be restrained effectively, for the potential offset between oxidative peak and reductive peak of doped LiFePO4 material was only 0.079V, lower than pure LiFePO4 markedly.

Jan 1, 2006