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By S. P. Rivers

The stainless steel industry re1ies on nitric-hydrofluoric acid (HNO,/HF) pickling solutions to remove surface contaminants and maintain the corrosion resistance of the steel. More stringent environmental guide1ines are expected to be placed on the disposal of these solutions which could significantly increase processing costs. The U.S. Bureau of Mines has been conducting research to develop a process for recycling depleted pickling solutions, thus reducing the quantity of by product acids generated. Research has shown that F- can be liberated from the predominant iron fluoride species (FeF,') by using oxalic acid in an electrodialysis cell. Ion selective membranes allow dissolved metals in the depleted solution to be replaced with hydronium ions by metathesis, thereby regenerating the HF. The regenerated HN03/HF is then retained in the pick1ing solution. This paper reports on the research effort at the U.S. Bureau of Mines Rolla Research Center to apply electrodialytic recycling to HN03/HF pickling solutions.

Jan 1, 1993

By N. Shi, T. C. Lowe, S. J. Zhou, M. L. Lovato, Y. T. Zhu, J. A. Valdez, W. R. Blumenthal, M. G. Stout

"A major problem of short-fiber composites is that the interfaces between the fiber and matrix become a limiting factor in improving mechanical properties such as strength. For a short fiber, a strong interface is desired to effectively transfer load from matrix to fiber, thus reducing the ineffective fiber length. However, a strong interface will make it difficult to relieve fiber stress concentration in front of an approaching crack. Stress concentrations result in fiber breakage. We report in this paper an innovative approach to overcome this problem: reinforcement morphology design. Short-fibers with enlarged ends are processed and used to reinforce a polyester matrix. The initial results show that the bone-shaped short-fibers produce a composite with significantly higher strength than can be attained with conventional short, straight fibers.IntroductionThese interfaces between the fiber and the matrix in short-fiber composites play a critical role and, in many cases, become a limiting factor in improving such mechanical properties as strength and toughness of the composites (1-4). For a short fiber, a strong interface is desired to effectively transfer load from matrix to fiber. A stronger interface can reduce the ineffective length at both ends of the fiber and, therefore, can increase the effective length that carries load (5-9). However, with a strong interface it is difficult to relieve fiber stress concentration -in front of an approaching crack; and such stress concentration can result in fiber breakage (10, 11). This effect is particularly severe for ceramic matrix composites, because of their low matrix toughness and lack of plasticity. Even for a composite with a highly ductile matrix, such as plastics, too strong an interface may still cause successive adjacent fiber breakage and subsequently reduce composite toughness (1, 11). On the other hand, a weak interface significantly decreases the fiber load-carrying length due to ineffective load transfer and complete fiber interfacial debonding and pullout during loading. A compromise in the interfacial bond strength will also compromise the load-carrying potential of short fibers."

Jan 1, 1998

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 Y. W. Chung, W. I. Chia

"The interaction of water vapor with single crystal Ni3(Al,Ti) and polycrystalline Ni3Fe, with and without the presence of oxygen, has been studied with Auger electron spectroscopy, photoemission spectroscopy, thermal desorption and isotope exchange. Water dissociates to produce atomic hydrogen above 200 K on both Ni3(Al,Ti) and Ni3Fe surfaces. For Ni3(Al, Ti), the reaction is structure-sensitive. Pre-adsorbed or co-adsorbed oxygen on Ni3(Al,Ti) and Ni3Fe significantly suppresses hydrogen production due to water dissociation. This suppression process occurs more efficiently on Ni3Fe than Ni3(Al, Ti).IntroductionOrdered intermetallic compounds such as aluminides, silicides and titanides are very attractive for structural applications at high temperatures. This is because these intermetallics tend to form adherent oxides in oxidizing environments which protect the base materials from excessive oxidation and corrosion. In addition, they have low density, relatively high melting points and good high-temperature strength. However, the moisture in air severely embrittles many ordered intermetallics such as FeAl [1-3], Fe3A1 [4,5], C03Ti [6,7], (Co,Fe)) V [8], Ni3Si [9], Ni3(Si,Ti) [10], Ni3(AI,Mn) [Ill, and Ni3A1 [12-14], resulting in low 'ductility and brittle fracture at room temperature. Recent studies by Liu and coworkers (see review by George and Liu [15]) provide a qualitative description of the mechanism for this moisture-induced embrittlement. During elongation testing, cracks are formed, thus exposing fresh alloy surfaces. One or more active components of the alloy react with water vapor in the environment to produce atomic hydrogen which penetrates into crack tips and causes hydrogen embrittlement. This is similar to that proposed for moisture-induced embrittlement of aluminum alloys [16]."

Jan 1, 1996

By Keith M. Axler

This report addresses issues specific to the generation of hydrogen fluoride via reaction of calcium fluoride with sulfuric acid. This process has been established on a commercial scale and is under consideration for treatment of calcium fluoride residues from uranium processing. Magnesium fluoride slags are also available as a product of uranium processing. The technique of using sulfuric acid for the production of hydrogen fluoride from magnesium fluoride is also under consideration as a residue processing scheme. In the current study, thermodynamic modeling was used to investigate these chemical processing systems. The results presented herein reveal information relevant to the selection of processing temperatures and conditions. Details include predicted effects in system composition based on operating temperatures for both the calcium fluoride and the magnesium fluoride systems.

Jan 1, 1996

By Eric J. Beckman

Recovery of metals from dilute solution, whether the matrix is solid, or liquid, remains a considerable technical and financial challenge. Methods currently exist whereby metals can be extracted from either type of matrix, yet these methods consume significant quantities of reagents and can also generate multiple waste ,streams in the process. Technology developed in our lab allows efficient application of environmentally-benign CO2 to a number of separation problems involving metals. For example, we have employed biphasic mixtures of C02 and water as a green acid leach medium. Metals have been extracted from a steelmaking process residue and then recovered as metal carbonates through depressurization. In this process, metals are extracted and recovered without the use of reagents other than CO2 and water, and CO2 is sequestered as a solid. In addition, through synthesis of Cal-miscible phase transfer agents, we have shown that CO2 can replace the organic solvent currently used in refining of precious metals, The sensitivity to pressure of phase behavior in a CO2-mixture may allow significant streamlining of the process as well. Finally, CO2 soluble chelating agents have been used to extract toxic metals from acidic effluent such as that found in plating facilities.

Jan 1, 1999

By Richard D. Hagni

Although the economically important uranium minerals are difficult to recognize under the ore microscope, they can be identified by a combination of qualitative and quantitative techniques. Useful quantitative techniques include indentation hardness, percent reflectance, spectral reflectance curves, and color coordinates. The latter two properties are especially distinctive for the primary urahlferous minerals uraninite, coffinite, brannerlte, and davidite. Together with the quantitative properties of indentation hardness and reflectance, the character and color of internal reflections are distinctive for many of the secondary uranium minerals. Ore microscopic techniques also provide an excellent means for determining the intergrowths of these minerals with other ore and gangue minerals. Such intergrowths are important to an understanding of the genesis of uranium deposits, and they may be important to uranium extractions.

Jan 1, 1981

By Ahmet Haxhiaj, Jaroslaw Drelich

"Both composition and porosity of pellets are the main parameters influencing the reductive melting process in water-jacket furnace during the roasting of sulfide lead concentrate. Roasting in a smelter located in Trepçë is done at about 9000C, for pellets which are composed of PbS, CaCO3, Fe2O3, and SiO2. In order to faciltiate the formation of slag in the reductive melting, the pellets must have the proper content of CaO, SiO2, and FeO, and porosity. The plant’s practice indicates that pellets with porosity of 18% do not melt adequately in the water-jacket furnace. The optimum porosity for the proper melting of pellets needs to be 32-40% and can be achieved when pellets are loaded with more than 10 wt.% CaO. Pellets with less than 10% CaO have a limited network of pores, such that reactive gases cannot reach the entire ore structure. Also, the composition of the pellets must satisfy the ratio of CaO : SiO2 : FeO = 1 : 1.2 : 1.8 to facilitate the formation of slag in the reductive melting process.IntroductionAgglomeration roasting of sulfide lead concentrate is an important phase in the production of lead by reductive melting [1-6]. The reductive melting process is a complex process with contradictory effects of several technological indexes which many times are hard to measure and determine. In this process, loading the water-jacket furnace with pellets of optimized composition and structure can reduce the consumption of coke, and achieve high level of lead recovery. Pellets (agglomerates) should be porous, but at the same time they should have necessary mechanical strength. ‘Self-melting’ ability of pellets is controlled by the types and quantities of fluxes blended into the pellet composition. Three major additives and their role are:"

Jan 1, 2011

By Charles H. Bucknam

A gold sampling optimization study was carried out in support of open pit gold mining operations for the Newmont Gold Company Bootstrap-Capstone deposits in Northeastern Nevada. Six bulk samples were tested using fire refining techniques at field particle size, to determine coarse particle heterogeneity of the ores, and by gravity .concentration methods at 10 mesh particle size, to observe any particulate gold liberation. An overall sampling model is presented for the deposit based on the pooled test information, to reconcile the results of coarse particle heterogeneity testing and the fine particle 'liberation testing. The sampling model is used to recommend procedures to control the variability of gold grade estimation due to the fundamental error (nugget effect) during sampling, sample preparation and assaying of the ores and other fundamental variances. The technique of simplified quantitative risk analysis (SQRA) is used to provide an economic justification for implementation of. recommended improvements to field sampling practices.

Jan 1, 1999

By Bin Xu, Qian Li, Yong-bin Yang, Xiao-liang Liu, Tao Jiang, Yan Zhang

Some high sulfur and arsenic-bearing gold concentrate has a gold leaching rate less than 80% by oxidation roasting-pickling-cyanidation process. The characteristics and intensification of gold leaching were studied systemically. By combining chemical composition and phase analysis, the low gold leaching rate was found to lie in the capsulation of gold by iron-containing phases including iron oxides, arsenopyrite and pyrite. 96.66% of gold in the industrial leaching residue was capsulated and 95.88% of the capsulated turned out to be in the iron-containing phases. The results of laboratory pickling-cyanidation experiments on the calcine and industrial leaching residue presented further demonstration for the fact that gold capsulated in the iron-containing phases was hard to be leached. However, the gold cyanide leaching rate of calcine could be raised over 95% by a reduction roasting-pickling pretreatment which played such a significant role in exposing the capsulated gold that gold leaching was intensified remarkably.

Jan 1, 2015

By J. -S. Park, H. -S. Jeon

This study has been carried out to develop a relatively simple hydrometallurgical process for recovering nickel as nickel sulfate from the spent nickel-cadmium battery residue in which cadmium was removed by vacuum distillation. This residue is composed of 36 % nickel, 20 % iron, and other metals such as cobalt. First, crushing and selective classification were performed to separate iron to produce a nickel-rich product (over 40 % nickel). This product was dissolved in sulfuric acid to obtain a nickel sulfate solution. During the dissolution, nitric acid and air were added to the system to enhance the iron oxidation reaction rate. The free acid remaining in the dissolved solution was neutralized by adding nickel carbonate. Iron was precipitated as iron hydroxide and removed from the solution. The nickel sulfate solution was then fed to a vacuum evaporator to concentrate the solution by evaporation of water and crystallized at around 45°C to obtain nickel sulfate hexahydrate. A recrystallization process could remove other impurities such as zinc and manganese.

Jan 1, 2000

By W. L. Dalmijn

The processing of scrap and scrap cars starts with size reduction by a hammermill, or shredder. After the liberation the magnetic fraction is removed. The remaining non¬magnetic fraction mixed with other materials is screened and each fraction is processed separately. The increased use of plastic has a negative effect on the recovery of metals and waste production. At Huron Valley, Belleville Michigen, USA, the non-ferrous fraction from 5 million obsolete cars per year, containing 200,000 tons of non-ferrous metal, is processed. Aluminium Is recovered with a heavy medium separation process and concentrated with eddy current separators. The remaining heavy non-ferrous fraction is concentrated by a new combination of eddy current separation and image processing. After this separation process the zinc fraction is melted and refined and the copper, brass, stainless steel and other high-quality concentrates are sold to the secondary industries. The recycling of car scrap has become an important source of metals and materials for the secondary. materials processing industry.

Jan 1, 1995

By Ivan Imris

The iron production has generated many tonnes of very fine residues with high concentration of iron. In addition, during the recycling of galvanised steel scrap in the steel making processes the zinc and lead are largely concentrated in the dust. These kinds of dusts are usually dumped beside the metallurgical plants and cause environmental problems. Therefore the metal recovery from the metallurgical residues has become a major interest not only from the viewpoint of metals recycling but mainly from the viewpoint of environmental land protection. The thermodynamic analyses and laboratory experiments suggested that the metals could be recovered from metallurgical wastes by reduction roasting and by plasma smelting processes. The iron rich pellets with very high metallization may be obtained from metallurgical wastes by the reduction roasting and the inert slag and pig iron could be produced by plasma smelting processes. In both cases the iron rich products are suitable for the steel production. During the reduction roasting or plasma smelting the high volatile zinc and lead metals were removed and enriched as a secondary dust, Zn-Pb concentrate, which is suitable for processing in zinc and lead smelters. Suggested processes are commercially feasible and environmentally friendly without any solid or liquid waste.

Jan 1, 2003

By Z. Zhang, R. G. Reddy

The viscosities of industrial lead slags with various compositions were measured as a function of temperature. It was found that viscosities of lead slags decreased with increasing temperature, and the plots of ln(11) vs. 104tr followed a linear relation over the reported ranges of temperature. Using the data of this study and available other related data from the literature, a viscosity expression was developed as a function of composition and temperature. The calculated results using this viscosity expression are in good agreement with the measured data. The composition dependency of viscosity of lead slags is discussed.

Jan 1, 2000

By Chan. C. L., Zehr. R., M. M. Chen, J. Mazumder

"Two three-dimensional models of a surface tension gradient driven flow during laser surface heating are developed. The first model is based on a perturbation solution. The basic solution corresponds to the stationary axisynwnetric case and perturbation is based on a small scanning velocity. The advantage of seeking a perturbation solution, as it turns out, is that the three-dimensional flow is modeled by two sets of two-dimensional equations which are presumably much more tractable than the original three-dimensional equations. Numerical solutions are obtained and discussed. The second model is a full three-dimensional numerical solution of the Navier-Stokes equations, using a point-by-point partially vectorized iteration scheme. Surface shape is also determined in a self-consistent manner. The effect of the presence of convection on pool geometry, cooling rate and solute redistribution is presented and discussed.IntroductionThe existence of fluid flow and convection and their effects were first reported in the fifties (1,2). The role of convection in controlling pool geometry such as pool shape, undercut and ripples, and defects such as variable penetration, porosity and lack of fusion and weld properties such as weld homogeneity and bead formation is studied by a number of researchers and is reviewed by the authors in a recent paper (3).Recently, surface tension gradient driven flow has been identified as one of the forces responsible for convection within the molten pool (4,5). It is postulated that surface tension gradient driven flow is responsible for the surface ripple formation in the weld pool (6-8). Oreper, et al. (9) developed a two-dimensional convection model. Buoyancy, electromagnetic and surface tension gradient forces were considered. The formulation was based on a specified pool profile. It was found that the surface tension gradient is the dominant force in most cases. However, the solid-liquid interface is not known a priori. In fact, the solid-liquid interface, i.e. the pool shape, is a piece of information that the model should be able to predict. A two-dimensional transient self-consistent (i.e. the solid-liquid interface is solved as part of the solution] model for laser surface melted pool was first developed by Chan, Mazumder, and Chen (3)). This model predicted a non-uniform cooling rate, hence non-uniform microstructure. Depending on the Prandtl number (i.e. material) and surface tension number, the shape of the molten region as well as the cooling rate changes. It was also predicted that the recirculating velocity is of one or two order of magnitude higher than that of the scanning velocity. This model provides the detail of the flow field and heat transfer on a plane perpendicular to the scanning direction. However, the front-to-back motion and its effect on heat transfer also play important roles in the physical process, especially for the fact that the recirculating velocity is so much higher than the scanning velocity. Such a motion cannot be obtained from two-dimensional models."

Jan 1, 1986

By R. Padilla

The reaction of chalcopyrite with gaseous sulfur has been investigated in the range 350-450 °C in order to transform this mineral into a more acid soluble copper sulfide and insoluble iron sulfide. The results of thermodynamic analysis of this system as well as the X-ray diffraction analysis of the reaction products showed that in the temperature range 350 400°C the sulfidation reaction proceeded without formation of intermediate copper-iron sulfides according to: The effects of temperature and time on the conversion of chalcopyrite were studied. Conversion of chalcopyrite reached about 80% very rapidly with increase in temperature up to about 400°C. The recovery of copper from the sulfidized samples was determined by leaching in oxygenated 1.2M H2S04, 2M NaCI solution. Copper recoveries over 90 % were obtained from samples sulfidized for 30 min at temperatures lower than 400°C.

Jan 1, 2001

By J. M. Skeaff

As much as 100% of the gold and 67% of the silver in a sulphur-bearing hydrometallurgical leach residue have been transferred to copper metal at copper smelting temperatures by dissolving the partially calcined residue in an iron-bearing slag maintained in equilibrium with the liquid copper metal and matte phases. The precious metals can then be recovered by conventional refining techniques. Copper can be recycled at least four times without any detrimental effects on gold and silver transfers and recoveries. Apparent copper recovery in the .process can be over 100% because of the copper content of the residue. Based on slag analys.es, the overal1 recovery of gold in the copper metal and matte phases varies from 94% to 100% under all conditions investigated. On the? same basis, silver recovery varies .from 9S% ?to 99% under optimum conditions, but is only 4S% to 73% under other, less attractive conditions. Unaccounted for silver losses of' about 30% make it difficult to determine the major factors affecting ?silver transfer and recovery. A method for implementing the technology on a commercial scale at a Canadian copper/zinc smelter has been proposed. A preliminary economic assessment and comparison of the proposed pyrometallurgical process with conventional cyanidation indicates that either process is economically attractive for recovering gold and silver from leach residues. Although the capital costs are higher, the pyrometallurgical process is simpler, has higher recoveries, lower operating costs and no .potential environmental problems related to cyanide disposal.

Jan 1, 1989

By D. E. Karvelas

Argonne National Laboratory is conducting research to develop a cost-effective and environmentally acceptable process for the separation of high-value plastics from discarded household appliances. The process under development has separated individual high purity (greater than 99.5%) acrylonitrile-butadiene-styrene (ABS) and high-impact polystyrene (HIPS) from corruningled plastics generated by appliance-shredding and metal-recovery operations. The process consists of size-reduction steps for the commingled plastics, followed by a series of gravity- separation techniques to separate plastic materials of different densities. Individual plastics of similar densities, such as ABS and HIPS, are further separated by using a chemical solution. By controlling the surface tension, the density, and the temperature of the chemical solution, we are able to selectively float/separate plastics that have different surface energies. This separation technique has proven to be highly effective in recovering high-purity plastics materials from discarded household appliances. A conceptual design of a continuous process to recover high-value plastics from discarded appliances is also discussed. In addition to plastics separation research, Argonne National Laboratory is conducting research to develop cost-effective techniques for improving the mechanical properties of plastics recovered from appliances.

Jan 1, 1996

By Xiaodi Huang, Matthew Andriese, Zheng Zhang, Jiann-Yang Hwang, Zhiwei Peng

"The thermal decomposition and regeneration behaviors of wüstite were investigated by in situ high temperature X-ray diffraction (HT-XRD) under non-isothermal condition at heating rate of 4 K min-1 in vacuum ranging from 294 K to 973 K. Wüstite on heating decomposes to magnetite and iron up to 823 K, above which it exhibits marked tendency to regenerate. Investigation of thermal stability of the reaction system shows that the decomposition proceeds under kinetic reaction control while the regeneration is under thermodynamic control. Kinetics study based on the Coats-Redfern integral approximation method indicates that the decomposition reaction follows a Komatsu-Uemura model-based diffusion-controlled kinetics with activation energy of 32.860 kJ mol-1. The thermodynamics analysis of regeneration reaction demonstrates that wüstite regenerates at lower temperature than stoichiometric ferrous oxide.IntroductionOwing to its importance in preparing various magnetic ceramic/metal nanocompostites or nanocrystals with high values of coercivity for the application as recording media, wüstite (non-stoichiometric ferrous oxide) has been attracting the attention of scientists over a long period [1-6]. The thermal behavior of wüstite was investigated by several researchers and phase transformations due to thermal decomposition and regeneration of wüstite during the heating in a specific temperature range was observed [7-9]. In spite of wüstite being found to dissociate to magnetite and iron at temperatures lower than 848 K and then regenerates at higher temperature, a clear understanding of the reaction mechanisms is clearly lacking [9]."

Jan 1, 2012

By G. Glinski, K. A. Pericleous

"Recent advances in new computational modelling techniques such as Lattice-Boltzmann and Dissipative Particle methods offer the prospect of simulating complex fluids such as colloidal and dense suspensions in industrial processes. They are referred to as mesoscopic methods since they lie between molecular dynamics at a microscopic atomistic scale «lO-9m) and traditional macroscopic CFD methods (> 1O-2m). The models behave like a 'coarse-grained' gas consisting of fictitious interacting particles, which are much larger than the real molecules of the actual fluid they represent. Inter-particle forces are set so that the collisions collectively mimic the phenomenological transport properties and flow of the underlying fluid at a macroscopic scale.Much of the developmental work to date has focused on laying theoretical foundations based on thermodynamic and kinetic theory. Successful applications include predictions of macroscopic transport properties of complex fluids and flows in porous media and filters. With the constant increase in computational power, these mesoscopic methods are now sufficiently developed to determine their suitability to simulate complex fluid flows in real industrial processes. This work describes the application of meso scopic methods to the stencil printing of solder pastes in the assembly of electronic components. The aim of this work is to assess the ability of these methods to study the transport mechanisms of individual solder particles suspended in the flux solvent as they enter and fill the micro-apertures of a stencil. This paper demonstrates the coupling of such mesoscopic methods to continuum CFD methods to predict the flow of dense suspensions (i.e. solder paste) in industrial processes."

Jan 1, 2001