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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 A. Yudiarto, M. Z. Mubarok

At the present paper, synthesis of magnesia from ferronickel smelting slag is discussed. The first stage was extracting magnesium from the slag by leaching in HCl solution. Magnesium extraction of 97% was obtained from the slag leaching with HCl 8 molar, solid:liquid ratio 1:40 (g/ml) and temperature 80 °C after 24 h. Solution purification was performed by adjusting solution’s pH at 95 °C with addition of MgO powder. At pH range range of 3–4, co-dissolved iron was removed as akagenite (b-FeOOH) precipitate. Dissolved nickel precipitation was detected at pH range of 4–6, while dissolved Mg and Al started to precipitate in the forms of pyroaurite (Mg6Fe2CO3(OH)16∙4H2O) and hydrotalcite (Mg6Al2CO3(OH)16∙4H2O) at pH range of 8–9. High purity of brucite (Mg(OH)2) was obtained by Mg precipitation at pH range of 11–12, under stirring speed of 300 rpm and stirring time of 4 h. Calcination of brucite at temperature of 1000 °C completely converted brucite to periclase (MgO) powder after 240 min.

Mar 1, 2017

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 S. Gupta, M. Fuka

This paper reports for the first time the synthesis of deintercalated MoAlB particulates which belongs to a family of novel ternary borides called MAB phases by selected etching of Al from these particulates by treating them with a solution of LiF and HCl. The FESEM analysis showed that these particulates hada stacked 2D-particles like morphology reminiscent of multilayered MXenes, but unlike MXenes, the 2D layers were interconnected with anisotropic porosity between them with an average length and width of pores being 257 ± 126 nm and 35 ± 10 nm, respectively. The EDS analysis of particulates showed that a typical particulate had a chemistry of (Mo Al )B{O F } which indicate partial 0.67 0.33 0.19 0.02 deintercalation of Al from the particulates. These novel particulates were also referred to as MABenes due to their microstructural similarity with multilayered MXenes.

Mar 1, 2018

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 Alaina Mallard, Katie Schumacher, Jannette Chorney, Grant C. Wallace, Jerome P. Downey

Commercial ceramic carbide operations require large thermal and mechanical energy inputs in order to produce a powder product. A process that could reduce the energy requirements needed to make these materials would allow for these materials to be implemented in a greater number of industrial applications. In this study, silicon carbide (SiC), tungsten carbide (WC), and molybdenum carbide (Mo2C) were synthesized via the carbothermal reduction of activated carbon loaded with silicate, tungstate, and molybdate anions adsorbed from aqueous solutions. Carburization was carried out under reducing and inert gas atmospheres, at temperatures lower than those utilized by commercial operations. Silicon carbide “whiskers” were synthesized under H2 at 1400 °C, while molybdenum carbide and mixed crystals of WC, W2C, and W were synthesized at temperatures below 1000 °C. X-ray diffraction and scanning electron microscopy were used to characterize the carburization products, and inductively coupled plasma-optical emission spectroscopy (ICP-OES) was used to determine the degree of adsorption onto the activated carbon matrix.

Mar 1, 2018

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

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 Duclerc Fernandes Parra, Ademar B. Lugão, Nilton Lincopan, Fernanda Esposito, Vijaya Rangari

Polymeric hydrogels are natural or synthetic systems, which have gained interest due to their high biocompatibility with soft tissues. These types of hydrogels have been used for wound dressing as a drug delivery system. Here in this study the polymeric hydrogels based wound healing systems were prepared using poly (N-vinyl-2-pyrrolidone) (PVP), poly (ethylene glycol) (PEG), agar and neomycin drug followed by gamma irradiation to promote crosslinking and sterilization. The influence of irradiation process with 25 kGy dose was investigated. The gel fraction and maximum swelling were estimated using physicochemical methods and found about 95% gel fraction and 1100% swelling after 8 h of immersion. Neomycin released from hydrogel was carried out by Liquid Chromatography-Mass Spectrometry method and the drug concentration remained constant for 48 h. Hydrogel/neomycin exhibited antibacterial effects against Staphylococcus aureus. With these results, it can be inferred that hydrogel/neomycin is a suitable candidate for wound dressing.

Mar 1, 2018

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