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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.

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 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 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

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

By L. Lü, M. O. Lai

"Mechanical alloying is a dry, high energy ball milling process which has been used to synthesize metallic powders in the solid state. The present study use this technique to synthesize Cu-base shape memory alloy powder from commercial Cu70Zn30, Cu86Zn14 and element AI powders. The evolution and formation of shape memory alloy powder were monitored using X-ray diffraction and microscopy. It was observed that shape memory alloy powder started to form after 1.8 ks of mechanical alloying. ? phase was clearly detected after 3.6 ks of mechanical alloying. The intensity of X-ray diffraction of the y phase increased when mechanical alloying duration was prolonged indicating an increase in the amount of y phase. Microstructure observation showed different stages of formation of alloyed powders: welding between powders and formation of layered structure, deformation and fracturing of layered structure, and finally the formation of alloyed powders.IntroductionMechanical alloying (MA) is a process used for producing powders with controlled and extremely fine microstructure. It was original developed in 1966 (1) to produce aNi-based superalloy combining oxide dispersion strengthening with gamma prime precipitation hardening. In recent years this technique has been used in producing a wide range of materials including intermetallic compounds (2, 3), amorphous materials (4-6) and other materials (7-9). In MA, a blend of powders is subjected to highly energetic compressive collision. The powder panicles are welded and fractured during ball milling. Therefore, it is essential that at least one of powders should be ductile to act as combiner. It has however been found that brittle components without soft element can also be mechanically alloyed (10), even ceramic powders (11).The present work aims to study the mechanism of formation of shape memory alloy powder during MA."

Jan 1, 1994

By Enrui Dai, Weibing Chen, Bin Yang, Wenhui Ma, Haisheng Fang, Hui Wang

LiMn0.8Fe0.2PO4/C composite was prepared by an improved solid-state method and the effect of calcination temperature on properties of the obtained materials was investigated. The results showed that increasing calcination temperature from 600 to 700 oC improved the performance of the LiMn0.8Fe0.2PO4/C due to enhanced crystallinity and increased conductivity, but further increase in calcination temperature to 800 oC led to degraded performance due to particle growth and decrease in porosity. Therefore, the LiMn0.8Fe0.2PO4/C composite prepared at 700 oC exhibited the best electrochemical performance, and could deliver a high capacity of 152 mAh g−1 at 0.1 C, 147 mAh g−1 at 1 C and 114 mAh g−1 at 10 C. In addition, the performance of the LiMn0.8Fe0.2PO4/C and LiMn0.8Fe0.19Mg0.01PO4/C was compared when they were obtained at the optimum calcination temperature.

Jan 1, 2015

By Noritaka Horii, Katsuyoshi Kakinuma, Hiroshi Yamamura

"ZrO2 and Y2O 3-doped ZrO2 gel film were obtained by spin coating of sol from Zr-n-propoxide, n-propanol, acetylacetone, nitric acid, and water on a silica glass as a substrate. ·Dried gel films crystallized to monoclinic, tetragonal, cubic and their mixed phases, depending on the chemical composition of sol, .firing temperature, and coating cycles. ZrO2 films with highly preferential orientation were successfully obtained from a solution containing a large amount of n-propanol. The highly oriented ZrO2 film was found to have high transparency compared with non-oriented 'films. Electrical conductivity of 8 mol% Y2O 3 doped ZrO2 film was also measured.Introduction3 mol% Y2O 3 doped ZrO2, which has a tetragonal symmetry is ·well known to have a strong mechanical property and a high toughness. (1) On the other hand, 8 mol % Y 2O 3-doped ZrO2 is high oxide-ion conducting material and is applied to oxygen sensor, oxygen pump, and solid oxide fuel cell (SOFC). (2) Sol-gel methods using metallic alkoxide are widely applied for synthesizing ceramics such as high-purity fine particles, thin film, and fiber. (3) For ceramics films, many reports have been made on SiO2, (4) TiO2, (5) and PZT. (6) Several case studies have been done on zirconia film based on the sol-gel method, (7) - (11) but very few on preferentially oriented film and on systematic Y zO3 doping. Almost zirconia ceramic· films reported were prepared by means of dip-coating. Kamiya et al. (12) and Ganguli et al (13) converted zirconia into fiber. Sol from Zr alkoxide is usually very unstable, and a stabilizing agent such as glycol or ß-keton is used beforehand (7) (14)."

Jan 1, 2000

By Sun-Hee Cheong

This study sought to produce L(+)-calcium lactate using precipitated calcium carbonate as a starter culture composite of lactic acid bacteria in lactic acid fermentation. Specifically, precipitated calcium carbonate was synthesized by reacting calcium hydroxide with sodium carbonate in the previous study by the authors. Synthetic precipitated calcium carbonate was then used as the calcium source of lactic acid bacteria during the fermentation process. In general, precipitated calcium carbonate has low absorption rate in the human body. On the other hand, calcium lactate has high absorption rate; it is commonly used in food and drug industries as calcium additives in various foods such as cookies, beverages, bread, sauces, powdered milk, and fruit juice. Calcium lactate has two racemates, e.g., L(+)-lactate and D(-)-lactate. In particular, L(+)-lactate is known to be more soluble than D(-)-lactate and generally produced from lactose by homo-fermentative lactic acid bacteria such as Lactococcus spp., Lactobacillus plantarum, Lactobacillus casei, Lactobacillus curvatus, and Pediococcus spp. Thus, the characteristics of the pertinent lactic acid bacteria and optimal condition such as temperature, pH, precipitated calcium carbonate addition rate, and content of fermentation for increasing formation yield and purity were investigated. The findings suggested the possibility of manufacturing L(+)-calcium lactate using precipitated calcium carbonate as a calcium source with high value-added instead of commercial calcium lactate.

Jan 1, 2006

By Leo Brewer, Kazuyoshi Shimakage, Mamoru Mitomo, Toshiyuki Nishimura, Yoichiro Uemura, Shinji Hirai

"In the synthesis process of ß -La2S3 via the sulfurization of La2O3 powder using CS2 gas, La2O2S was formed. This occurred at an initial stage of the reaction for sulfurization temperatures below 973K, and ß -La2S3 was also formed at a shorter period for higher sulfurization temperatures. It was found that the oxygen content in ß -La2S3 powders decreased gradually with an increase in sulfurization temperature. On the other hand, the carbon content in these powders increased gradually with an increase in the sulfurization temperature. Though it has been reported that ß -La2S3 was transformed to Y -La2S3 at 1723K± 50K, the sintered compact of double-phase Y -La2S3 and ß. -La2S3 was formed at a rather higher temperature of 1973K when the synthetic powder of ß -La2S3 containing a high amount of oxygen was used. However, phase transformation of -La2S3 to Y -La2S3 progressed preferentially with a decrease in the oxygen content of synthetic ß -La2S3 powder. The Seebeck coefficient of the sintered double-phase Y -La2S3 and -La2S3 was higher than that of the single-phase Y -La2S3, reported previously.Introduction La2S3 exists in three polymorphic forms that are similar to a series of Ce2S3, Pr2S3 and Nd2S3: a, ß , and Y'. The a -La2S3, which is stable at low temperature, is irreversibly transformed to ß -La2S3 of various compositions in the solid-solution range between La2S3 and La3S4, at 923 ± 50K. The -La2S3 may also be an oxysulfide of La10S14O2. Moreover, the ß .-La2S3 phase is transformed to Y -La2S3 ,which has a Th3P4 structure, at 1573 ± 100K. The melting point of Y -La2S3 is 2398 ± 30K where this temperature is similar to those of common refractory materials such as silica and alumina. Therefore, it can be predicted that y -La2S3 which has a high melting point and a thermodynamic stability due to the strong affinity of La for S, would have &high refractory character and chemical inertness in many molten metals. The y -La2S3, colored vivid faint yellow is stable up to 623K in air, where oxidation starts. y -La2S3 is frequently used as pigments for plastics and paints3. Furthermore, Y -La2S3 which is a semiconductor, is considered to be useful as a thermoelectric conversion materials, because it has a high Seebeck coefficient."

Jan 1, 2000

By Hee Dong Jang

Crystalline metal oxide nanoparticles such as lithium cobalt oxide (LiCoO2) and indium tin oxide (ITO) were synthesized from sprayed droplets of aqueous precursor solution by flame spray pyrolysis. Complete thermal decomposition of the aerosol precursors was obtained at high flame temperature. Molar concentrations of the precursor solution, and the flow rate of combustion gas such as hydrogen, oxygen and air were varied to control particle size, size distribution and crystal structure. The crystalline nanoparticles synthesized were nearly spherical, and their average primary particle diameters ranged from 11 to 35 nm for LiCoO2 and from 8 to 15 nm for ITO.

Jan 1, 2006

By Marcelo R. Esquivel

A MmNi5 alloy is synthesized by a combination of mechanical milling and low temperature heating processes. Synthesis time is 40 h for powders milled in a low energy ball mill at room temperature. A reduction in milling time is obtained if massive sample is mechanically milled at shorter times (2 h to 10 h) and heated at temperatures lower (600 ºC) than the usual temperatures used in equilibrium methods (>800 ºC). The alloy formation is detected even at a combination of temperatures as low as 200 ºC and milling times as short as 5 h. The temporal evolution of mechanical milling process was followed by both X-ray diffraction (XRD) and scanning electron microscopy (SEM) to detect the main stages of milling. Four stages were detected: Initial, Intermediate, Final and Completion. These stages were correlated to an enhancement of the synthesis method by combination of times of milling shorter than 10 h and temperatures of heating lower than 600 ºC.

Jan 1, 2006

By Tae-Hyun Kim, Shun Myung Shin, Jin-gu Kang, Jeong-Soo Sohn

We investigated about synthesis of Mn-Zn ferrite with spinel structure using sulfuric acid leaching solution of mixed spent zinc-carbon batteries and spent alkaline batteries. The waste batteries were prepared by physical treatment such as crushing, magnetic separation, and screening. After screening, the crushed batteries were separated to +8 mesh and -8 mesh powder. Among these, under 8 mesh powder was selected for leaching test. The leaching test was investigated at 2 M H2SO4, 4 vol.% H2O2, reaction temperature 60 ?, agitation speed 250 rpm, solid/liquid ratio 50 g/ 500 ml, reaction time 1 h. The leaching efficiency of zinc, manganese and iron were 99.0%, 98.9%, 58.5%, respectively. For co-precipitation of zinc, manganese and iron, 5M NaOH solution was used for pH control. Then in order to synthesize Mn-Zn ferrite powder, it was investigated according to reaction temperature, agitation speed and O2 partial pressure. We could synthesize about 20 nm of Mn-Zn ferrite with spinel structure.

Jan 1, 2008

By Mikiya Tanaka, Mikio Kobayashi, Kazuya Koyama, Yoshihiro Nishisu

Preparation of multicomponent powders are very useful and important for producing the materials with complicated and homogeneous structure. Therefore multicomponent powders have a lot of attention in the field of advanced value-added materials. The aqueous processing in hydrometallurgy has a broad potential for producing multicomponent homogeneous precipitates. Furthermore the aqueous processing has a future potential for integrating the separation, precipitation and synthesis processes. In this presentation the precipitation from homogeneous solution including rare-earths and/or common metals is presented. These precipitates probably consist of almost monodispersed, multicomponent and spherical particles by precisely controlling several reaction factors, reaction temperature, concentrations of starting materials, pH and so on. The separation of the nucleation stage and the growth stage of the particles is very important and how to control the reaction factors to realize enough separation is discussed. In this presentation the systems of Y-Eu-0, Y-Fe-0 and Y-Al-0 are mainly presented. In addition the precipitation-stripping method from organic phase is presented focusing the synthesis of multicomponent powders of Ni-La-0 system. These precipitates have multicomponents homogeneously and so they are converted to multicomponent ceramic powders by calcination. They are important compounds as phosphor, opto-magnetic materials, optical materials, hydrogen storage alloy or as the related precursors. In this presentation some characterization of these particulate materials is included.

Jan 1, 1998

By J. Huot

It has been shown that magnesium-based metal hydrides such as Mg2Ni could be synthesized by high energy mechanical alloying. This process creates a nanocrystalline alloy that has enhanced hydrogen sorption properties due to the high density of defects and grain boundaries. Unfortunately, this process also requires a long synthesis time (up to 100 hours in some cases). In order lo reduce processing time and cost of synthesis, we have investigated the effect of milling at elevated temperature under an inert atmosphere. Milling at high temperature improves interdiffusion of the elements and reduces the number of structural defects such as vacancies, dislocations and internal strain. It was found that by milling elemental powders at 200°C. a complete synthesis of Mg2Ni could be achieved in 8 hours. This synthesis time is roughly an order of magnitude lower than that of the process conducted at room temperature. The hydrogen sorption kinetics and capacity of this material are comparable to Mg2Ni synthesized at room temperature.

Jan 1, 2002

By Taegong Ryu

The thermal plasma process has been applied to the preparation of nanosized tungsten carbide (WC1-x). The reduction and carburization of the vaporized chloride by methane-hydrogen mixtures produced nanosized WC1-x powder, with a small amount of WC or W2C phase. The products were characterized using XRD, carbon analyzer, and TEM. The effects of plasma torch power, the flow rate of primary plasma gas (Ar) to generate plasma flame, and the addition of secondary plasma gas (H2) on the product composition were investigated. The tungsten carbide (WC1-x) powder had a particle size less than 30 nm. The powder was treated under hydrogen atmosphere to fully carburize the WC1-x, and W2C phases to WC as well as remove excess carbon in the product. Finally, WC powder with a grain size less than 40 nm was obtained.

Jan 1, 2008

By Taegong Ryu

Nanosized tungsten powder was synthesized by the hydrogen reduction of ammonium paratungstate (APT) in thermal plasma. The effects of operating conditions on the product composition and particle size were investigated. The particle size of synthesized W powder was less than 30 nm in all cases tested. The sintering behavior of the synthesized powder (25 nm average size) was then investigated and compared with those of commercial W powder of 500 nm average size and W powder of 23 nm average size produced by milling the commercial powder. The sintering was done at 1400oC with various holding times. The hardness of the resulting compact from the synthesized W powder (315 VHN) was similar to that from the milled W powder (309 VHN), but the plasma-synthesized powder had a much lower tendency to form cracks. The compacts of both nanopowders were significantly harder than that of the commercial powder (192 VHN).

Jan 1, 2009