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By J. H. Baek, S. Alexandrovskii, D. W. Lee, B. K. Kim

Nano-phase titanium carbide was synthesized by Mg-thermal reduction process using a novel route of Mg-thermal reduction. The processes are based on I) feeding of TiC14+CxC14 x = 1, 2 ) solution into liquid magnesium, 2) Mg-reduction of metal chlorides, 3) TiC formation by the reaction of released Ti and C atoms, and 4) vacuum separation of residual liquid phases of Mg and MgCl2. In this study, the process for titanium carbide production with composition close to stoichiometry and the minimum content of impurities was optimized with the various process parameters such as concentration of initial solution, its feeding rate and reaction temperature, as well as a kinetic study.

Jan 1, 2004

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 T Perera, B Fan, S Thang, T Hsia

The mining industry is currently focusing to develop and adopt sustainable collector chemistry that can efficiently recover valuable minerals from their natural state. However, a limited number of research can be seen on the design and synthesis of polymeric flotation collectors. The focal objective of this research is to synthesise a more effective polymeric collector with advanced architecture to utilise in the mineral processing industry. Reversible Addition-Fragmentation Chain Transfer (RAFT) co-polymers with cardanol derivatives have the potential to selectively trap valuable metals in the flotation process in a more efficient way. Cardanol exhibits amenability to chemical modification for making tailor-made monomers that can further produce polymers with high value. The synthesis of a series of fit for purpose copolymers in this study was accomplished by RAFT polymerisation. The ability to design complex architecture is a significant advantage in engineering polymeric collectors by RAFT polymerisation. Initially, commercially available cardanol was converted to a cardanol based monomer and copolymerised with commercially available monomers to synthesise a series of novel cardanol based copolymers with predetermined molecular weights. The side groups of the copolymer were chemically modified to incorporate functionality that can be selectively adsorbed on the chalcopyrite surface.

Aug 24, 2022

By Anna Arkhireeva, John N. Hay

Considerable interest has been shown recently in organically modified silicates (ormosils) because of the wide range of possible applications for these interesting organic-inorganic hybrids. These applications include the use of the hybrids as modifiers of a range of host polymer proper- ties. The ormosils can be synthesised by the conventional hydrolytic sol-gel process, as well as by the non-hydrolytic sol-gel route. To date, however, there are relatively few reports of the synthesis of sub-micron size ormosil particles of well-defined spherical morphology. Here, we report work to date on synthesis of such nanoparticles and also introduce our own work in the area.

Jan 1, 2003

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 E. van Steen, G. M. Leteba

Optimizing the catalytic performance of multimetallic nanoparticle (NP) catalysts demands a concrete understanding of their design, while preferentially deploying wet chemical synthesis procedures to precisely control surface structural properties. Here we report the influence of reductants such as hydrogen-rich tetrabutylammonium borohydride (TBAB) and carbon monoxide-rich molybdenum carbonyl (Mo(CO)6) on the shape and morphological evolution of Pt-based binary (PtNi and PtCo) and ternary (PtNiAu and PtCoAu) nanostructures derived from a homogeneous solution of aminebased surface active agents (surfactants) in a high boiling point solvent. We successfully synthesized nanostructures exhibiting well-defined and composition-controlled surfaces deploying a one-pot synthetic approach. The development of the surface properties was, however, observed to be alloyspecific. The resultant highly monodisperse alloy NP with narrow size distributions and facet-oriented surfaces are expected to display enhanced functionality as catalysts for utilization in specific chemical reactions.

Jun 1, 2021

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 Pingchao Ke, Zhihong Liu

"To overcome the problem that scoroditeis not stable in neutral and alkaline solutions, we proposed and investigated a synthesis method of scorodite coated in-situ with hydrated ferric oxide in the Fe(II)-As(V)-H2O system at the initial Fe(III)/As(V) molar ratios larger than 1.0.The synthesis was carried out at 90?,pH 1.5 under atmospheric pressure. During the synthesis, oxygen gas was conducted and bubbled into the system to oxidize Fe(II) ions into Fe(III)ions, and Na2CO3aqueous solution as neutralizing agent was added controllably into the system for keeping the pH constant at 1.5. In this study, three samples of scorodite were synthesized at the controlled initial Fe(II)/As(V) molar ratios of 1.0, 2.0 and 3.0, respectively. The characterizations of the samples by HRTEM, TEM/EDX, and chemical composition indicated that the particle surfaces of scorodite synthesized at the initial Fe(II)/As(V) molar ratio of 2.0 and 3.0 were coated in situ by a film of hydrated ferric oxide with the thickness of several nanometers, while the sample synthesized at the initial Fe(II)/As(V) molar ratio of 1.0 was uncoated scorodite. The TCLP and long-term leaching for the toxicity characteristic of the samples showed that scorodite coated in situ with hydrated ferric oxide was stable in a wide pH range from 3.0 to 10.0, with the arsenic concentrations in the leaching solutions less than 1.0mg/L. Nevertheless, uncoated scorodite was unstable under the conditions from weak acidity to alkalinity, with the arsenic concentrations in the leaching solutions larger than 5.0 mg/L.INTRODUCTIONArsenic pollution is a challenge for environment and health and has been an important issue for scientists (Hopkin, 1989).Arsenicis commonly associated with ores or concentrates of nonferrous metals, mainly as independent arsenic bearing minerals such as arsenopyrite (FeAsS), tennantite(Cu12As4S13), enargite (Cu3AsS4), cobaltite (CoAsS), and gersdorffite (NiAsS), realgar (As2S2), orpiment(As2S3), etc.(Matschullat, 2000; Mandal & Suzuki, 2002; Long & Peng, 2012). In the nonferrous metallurgical processes, arsenic is enriched mainly in such arsenic bearing materials as various flue dusts, residues, and anode slimes, which results in the accumulation of arsenic in the system owing to the circulation of those arsenic-bearing materials back to the system and the pollution to the environment (Harris, et al, 2003).In addition, the utilization of arsenic is limited and has been decreasing owing to its toxicity and carcinogenicity. Therefore, arsenic has to be removed from those arsenic-bearing materials and discarded safely (Dutrizac & Jambor, 1988; Monhemius & Swash, 1999; Drahota & Fillippi, 2009).In this case, how to immobilize arsenic has become a difficult problem which must be solved. Among the methods of immobilizing arsenic which have been proposed and investigated, immobilizing arsenic into a stable mineral to fix it, has been realized as a promising method and becomes a research focus(Dutrizac et al, 1987; Dutrizac & Jambor, 1988; Demopoulos et al, 1995; Fujita et al, 2008a; 2008b).Scorodite has been known as one of the best minerals for immobilizing arsenic, owing to its high stability under weak acidic condition, the arsenic content as high as 32wt%,and good crystallinity benefiting the separation of solid to liquid(Daivid et al, 1999; Zhu & Merkel, 2001). Scorodite can be synthesized from arsenic containing solutions under both hydrothermal and atmospheric conditions, and a lot of work has been done on the synthesis of scorodite and its leaching stability characterization (Filippou & Demopoulos, 1999; Gomez et al, 2011).Two plants for the immobilization of arsenic as scorodite have been putin to operation in Chile and Japan, respectively (Filippou & Demopoulos, 1999; Amir et al, 2016)."

Jan 1, 2017

By Arthur Tauber, Horst Kedesdy

FERRITES are sintered metallic oxides of the spinel structure type1 and belong to the class of soft ferromagnetic materials. Similar to a ceramic, they can be formed and fired to a dense body, exhibiting a high electrical volume resistivity ranging from 102 to 102 ohm-cm as compared with 10-6 ohmcm for some of the metallic magnetic materials. This high resistivity, with resulting low eddy current losses, finds special application at high frequencies. The dispersive susceptibility of ferrites at microwave frequencies has also led to many applications in this field. Where high resistivity with high permeability is desirable, ferrites are used in low frequency applications. During the last few years ferrites exhibiting rectangular hysteresis loops have been developed for computer and magnetic memory systems. The general formula for ferrites is MeFe2O4 where Me is a divalent metal ion such as Ni, Zn, Mg, Mn, Cu, Cd, and Fe. Only two of these ferrites are nonferromagnetic, namely, those with Zn and Cd. Solid solutions can be formed between different ferrites, and it is of interest to note that solid solutions of a ferromagnetic ferrite with a nonferromagnetic ferrite yield much better magnetic materials than the basic ferrite body. In general, it can be said that the solid solution formation between ferrites has widened the field of ferrite synthesis and has led to methods of preparing materials with a large variety of magnetic properties.

Jan 7, 1957

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 James Ransford Dankwah

High sulphur carbonaceous materials like petroleum coke and rubber tyre are unsuitable as reductants in ironmaking because part of the sulphur is transferred to the reduced metal. Globally, while large amounts of petroleum coke are produced annually from the industrial processing of crude oil, billions of end-of-life rubber tyres are held in landfills and stockpiles. This work therefore investigates the potential feasibility of utilising these high sulphur carbonaceous materials as reductants in ironmaking without transferring the sulphur into the reduced metal. Composite pellets of iron oxide containing end-of-life rubber tyre (RT), petroleum coke and blends of RT/petroleum coke and petroleum coke/high density polyethylene (HDPE) were heated under argon atmosphere in a horizontal tube furnace. Reduced pellets were analysed after 10 minutes of reduction for their sulphur content. The results showed that sulphur-free metallic iron can be successfully synthesized using RT and petroleum coke as reductants. The level of desulphurisation depends on the nature of blending of the carbonaceous materials.

Jan 1, 2014

By Xuyang Liu, Xuewei Lv, Yu Zhang, Xiaolong Wu, Chunxin Li

Titanium nitride is a broad-spectrum specific functional material because of its many superior properties. Therefore, it is necessary to investigate synthesis methods of TiN and alloys containing TiN reinforcement. In the current study, with the increase of nitrogen gas pressure and the optimization of routine ball milling parameters, the conventional mechanical ball-milling method can be improved, the nanometers TiH2-TiN composite powder can be synthesized successfully in a shorter time. Nitrogen gas filled in ball mill jar in which the pressure was 0.6 MPa. TiH2 powder was milled under nitrogen atmosphere at a spinning rate of 250 rpm. The results show that the stable TiN is formed after grinding for 2.5 h according to the X-ray diffraction pattern. DSC (differential scanning calorimetry) curves also indicate that milled compound powder adsorbs certain nitrogen gas. The gas adsorbed in TiH2-TiN composite can exist stably below 200 °C.

Mar 1, 2017

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