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By Kimio Itagaki, Makoto Ohtsuka, Kouki Chiba, Minoru Matsumoto

"The properties of Ni-Mn-Ga films such as chemical composition, crystal structure, microstructure and transformation temperature were investigated with respect to sputtering conditions in the present study. The Ni-Mn-Ga films were deposited on a polyvinyl alcohol substrate with a radio-frequency magnetron sputtering apparatus using the NisoMn2sGa2s and Nis2Mn:«1Ga24 targets. After separating from the substrates, the films were annealed at the temperature between 873 and 1273 K for 3.6 ks. The chemical composition of the films depended on the radiofrequency generating power, however, there was no dependence on the heat treatment temperature. Each deposited film had a columnar grain structure. After heat treatment, the width of columnar grains widened and then became indistinct with increasing heat treatment temperature. The Heusler type cubic crystal structure of the fi4n with heat treatment at 1073 K changed to the tetragonal one through the martensitic structural transformation during cooling. The martensitic structural transformation temperature increased with increasing nickel content of films, while the Curie temperature decreased. The film obtained at 200 W using the Nis2Mn24Ga24 target after heat treatment at 1073 K showed one-way shape memory effect through the reverse martensitic structural transformation during heating.IntroductionThe ternary intermetallic compound NiiMnGa has a Heusler-type crystal structure and is an intelligent material, which has a shape memory effect and a ferromagnetic property. The martensitic structural transformation occurs within the ferromagnetic temperature region. The cubic crystal structure of L21 at high temperature changes to a tetragonal one through the martehsitic structural transformation during cooling. The films of this compound can be applied for an actuator of micro-machines."

Jan 1, 2000

By K. C. Liddell, B. Dou

"In producing multilayer films for magnetic data storage applications, the interfacial roughness must be controlled in order to obtain high quality materials with reproducible properties. The present understanding of the effect of roughness on multilayer properties such as magnetoresistance is sketchy, particularly for electrodeposited films. In this study, quantitative atomic force microscopy was used to characterize surface morphology before and after Ni films of varying thickness were deposited on Cu cathodes. A multinuclear multilayer growth mechanism is supported by both the deposition conditions and the AFM images, and a multinuclear multilayer model gave a satisfactory fit to measurements of the density of peaks on ultrathin Ni films between 0 and 8 nm thick.Alloys consisting of alternating ferro-and paramagnetic layers have begun to replace Permalloy in the sensing elements of magnetic hard drives. The operating principle of the new read heads is giant magnetoresistance (GMR), and they are smaller and more sensitive than previous inductive heads (1). Experimental studies on sputtered multilayers have emphasized the role of layer thickness and interlayer roughness in determining the presence and size of the GMR effect (e.g., 2,3,4,5,6). However, roughness in electrodeposited multilayers has rarely been measured, even though read heads are likely to continue to be made by this process for some time to come. Cu/Ni can be considered a model system for understanding processing-microstructure-property relationships in electrodeposited multilayers and is the most widely investigated of all such systems (e.g., 7,8,9,10,11,12). Nevertheless, the roughness of the interfaces in Cu/Ni electrodeposits has not been systematically characterized by quantitative techniques, and in all studies reported so far, the total deposit thicknesses were considerably greater than the 10 nm needed for most sensor applications (1). The thinnest such films were about 50 nm (7)."

Jan 1, 1998

By Lei Zhang, Shining Chen, Lina Wang, Pu Liu, Benquan Fu, Jiannyang Hwang

A three-dimensional (3D) electrode reactor combined with Fenton reagent was used for advanced treatment of coking wastewater from secondary biological treatment. Effects of some key factors on total organic carbon (TOC) removal rate were investigated, and the results were compared with those of the common three-dimensional electrode reactor. Experimental results showed that TOC removal rate could reach 51.7%, when optimal operating conditions were as follows: initial pH value 3.5, H2O2 dosage 17.6mmol/L, reaction time 90min and FeSO4·7H2O dosage 3.5mmol/L. Analytical results from UV absorption spectra indicated that the organic substances in the coking wastewater were well degraded by this system, which provided good experimental basis for the practical application of this process in the treatment of coking wastewater. This can be meaningful for the treatment of other kinds of wastewater.

Jan 1, 2015

By J. L. Holman

The Bureau of Mines is investigating recovery of Ni, Co, Cr, and other metals from mixed contaminated supera110y scrap. The scrap is melt-refined and cast into anodes for electrodeposition of recyclable Ni-Co alloy. Melt oxidation using roasted superalloy grinding sludge as oxygen source can divert the Cr to the slag but with excessive Ni-Co loss. Melt oxidation-carburization or direct melt carburization retains -95 pct of the Ni-Co in the anode alloy. With direct carburization, -90 pct or more of the Cr and other refractory metals report to the anode alloy, largely as carbide phases insoluble in electrolysis. Electrorefining data relate parameters such as controlled cathode potential, Fe and Cr impurities, pH, and compartmented cell use, to current efficiency and Ni-Co deposit quality. Recovery of -90 pct of the Ni-Co in the scrap can be achieved. Preliminary experiments to recover Cr, W, and other metals from the anode sludge and other byproducts are discussed. 347

Jan 1, 1987

By Hoda Emami

In this study, a combined pyrometallurgical and hydrometallurgical technique has been designed and used to recover rare earth mixture elements (REE) and cobalt from a NdFeB magnetic waste. while addressing the cost of reagent and process facility. This process can be adjusted to different magnetic wastes regardless of their compositions. Prior to the leaching, the magnet scrap was pretreated by two rounds of roasting (750°C in air) and a mechanical grinding in between, to convert iron metal to ferric oxide. Subsequent leaching was performed using optimized conditions (pH, temperature and retention time) where the extraction ratio of REE to Fe III is the highest. After removing iron content from the leachate (pH ≈ 3), REE was precipitated selectively and purified further. The produced REE concentrate reaches 99% purity with 85% recovery in a single run. The cobalt oxide was isolated from the PLS as a by-product with 99.8% purity.

By H. Soto, J. Jara, F. Nava

A method has been developed to recover cyanide and copper from solutions containing copper complexes and thiocyanate. Copper is precipitated as copper thiocyanate or as copper cyanide depending on pH and the concentrations of thiocyanate and cyanide in the effluent. The copper precipitate assays over 50% copper and presents good dewatering characteristics. After settling it can be separated from the effluent by filtration. The solution containing the bulk of the cyanide is then oxidized with ozone to transform the remaining thiocyanate into cyanide. This results in a regenerated solution rich in free cyanide that can be recycled to the cyanidation process. Careful control of the pH of the solution is required. First, pH of the effluent is lowered to optimize the precipitation and oxidation stages, then the pH is restored to an alkaline value to regenerate the cyanide solution. Recoveries of over 96% copper and cyanide were obtained in laboratory tests using industrial solutions. With this procedure, cyanocidic gold/copper ores could be treated economically by heap leaching, since the cyanide consumed by the copper impurities could be regenerated at very low cost (most of the cost of cyanide regeneration would be compensated by the copper credits). In order to achieve this, a bleed of the barren solution could be treated by the proposed method, and then recycled to the leaching step. The volume of solution to be treated should be large enough to keep a cyanide/copper molar ratio higher than 3:1. This would assure that copper does not cause undue interferences in the leaching or the carbon adsorption stages. If the thiocyanate content is low, the oxidation stage can be avoided, and the solution can be recycled to the leaching stage directly after the solid-liquid separation stage.

Jan 1, 1997

By J. L. Johnson

Remediation of small-arms firing ranges is being investigated by the Naval Civil Engineering Laboratory and the U.S. Bureau of Mines. Scheduled closures of military installations, as well as the management of active ranges, require the development of methodologies for heavy metals removal to prevent their entering the surrounding environment. The impact berms contain high concentrations of metals, and the soil and vegetation surrounding the berms were found to have slightly elevated levels. The heavy metals characterized are in the form of whole bullets, a wide size distribution of free fragments, smeared lead on the surface of the soil grains, and very finely attached particles. Gravity beneficiation can remove liberated metal contamination effectively. Weak acetic acid leaching shows promise in lowering the final metal contamination to allow the soil to pass the Environmental Protection Agency's (EPA) Toxicity Characteristic Leaching Procedure (TCLP) criteria.

Jan 1, 1991

By Joon H. Jang

At a selected pH, hydrothermal oxidation of chalcopyrite was carried out under controlled F+,, at elevated pressures and temperatures (172-200°C) by balancing the rate of oxygen injection against the rate of consumption. Chalcopyrite was converted to covellite (CuS) and digenite (CU1.8S) with rejection of iron and sulfur to the solution. Covellite forms in the first stage, followed by nucleation and growth of digenite in the second stage. The effects of rapid and slow injection of stoichiometric quantities of oxygen are compared. Both the covellite and digenite form a porous layer occupying the same volume as the original chalcopyrite grain. An electrochemical kinetic model is presented to correlate the observed results.

Jan 1, 1993

By J. T. I. Poijärvi

Outokumpu Harjavalta Metals Oy operates copper and nickel smelters, three sulphuric acid plants and nickel refinery at Harjavalta and copper refinery and precious metal plant at Pori. The by-products of these plants are presented in this paper. The by-products of the smelters include products from slag cleaning of flash smelting furnaces and converters, flue dusts and smelter off-gases. Weak acid and sludges from cleaning of smelter off-gases and acids are the by-products of the acid plants. The by-products out of the copper refinery are crystallized metal sulphates and sludges from electrolyte purification, on which a co-production process of the copper tankhouse is based. The main by-products of the precious metals plant are products from anode slime treatment and platinum metal group concentrates in the recovery of precious metals. Sludges from nickel matte leaching and precipitates from solution purification are the by-products of the nickel refinery. The formation, treatment and processing as well as the research work done for the utilization instead of dumping of the by-products in the production of copper and nickel will also be discussed in this paper.

Jan 1, 1995

By Broggi Andrea

Condensates produced by SiO(g) and CO(g) have a crucial importance in silicon production. Condensation will follow the reactions 3 SiOðgÞ+COðgÞ→ 2 SiO2 + SiC and 2 SiO ðgÞ→Si+SiO2. Solid compounds generated during silicon production contain Si, SiO2 and SiC in different microstructures and amounts. In industrial systems, condensates limit the SiO(g) escape to the off-gas system. On the other hand, they can block the gas flowing from the high temperature zone, hence the necessity of studying an optimized condensation process. This review discusses SiO(g) condensation and its interaction with CO(g). The report gives an overview of the condensates found both at laboratory and at industrial scale. The two main compounds are the Si–SiO2 and the SiOx–SiC mixtures. The hypothesis on the mechanism of formation of SiC–SiOx condensates is presented through a wide selection of performed works. The advantages and disadvantages of the former experimental procedures are discussed.

By Mark Tsirlin

Kinetics of the initial oxidation stages of diffusive silicide coatings on 8 molybdenum and niobium at 1100 - 1700 and under the pressure of 400 and 1330 Pa has been studied using methods of gravimetry and gas phase analysis of oxygen, as well as by SEK, XRD and EDMA methods. The first oxidation stage described by asymptotic equation in case of NbSi coating changed over to the stage described by parabolic equation. The asymptotic law was shown to depend on non - stationary conditions on the oxide layer boundaries. Interconnection between silicides and quartz structures, on the one hand, and peculiarities of oxidation kinetics, on the other, is [discussed. The possibility of estimation oxygen atom jump frequency in quartz and fractions of oxygen reacting with metal and with silicon proceeding from the analysis of the kinetic data was ascertained. Conditions of oxidation kine- tics transfer from asymptotic (or parabolic) stage to a non - protective "linear" stage, associated with volatile ~roduct formation, are also discussed.

Jan 1, 1995

By A. V. Reddy, C. Beckermann

"The DC continuous casting of a grain refined AI-4.5%Cu round ingot with realistic boundary conditions is numerically simulated. Of particular interest are the effects of the transport of free solid in the form of equiaxed grains on the macro segregation patterns and the final grain size distribution. The study uses a previously developed two-phase model that incorporates descriptions of heat transfer, solute redistribution, melt convection, and solid transport on the system scale with microscopic models of solutal undercooling, microsegregation and grain impingement. The numerical results indicate that grain transport inhibits the formation of inverse segregation in the ingot shell and promotes negative centerline segregation. This is explained by the reduction in the solid coherency next to the mold and the advection of solute-lean grains towards the centerline. Comparisons with the experiments of Finn et al. [5] illustrate the need for considerable improvements in the model. IntroductionMacrosegregation continues to be one of the concerns in DC continuous casting of aluminum ingots. The variation in composition over the ingot cross section results in the need to adjust alloy composition in order to meet mechanical property specifications in finished products. The extent of macrosegregation is greatly affected by the casting conditions, such as casting speed, superheat, cooling rate, mold size, alloy composition, and grain refining practices. Thus, it is of great interest to develop a comprehensive mathematical model to simulate the casting process, enabling the selection of conditions that minimize macrosegregation while maintaining a high productivity."

Jan 1, 1994

By George P. Demopoulos

n this study we have sought to highlight the critical linkage between individual reaction kinetic parameters (usually determined in small bench scale experiments) and large continuous reactor performance by focusing on the industrially significant zinc pressure leach process. To this end a comprehensive mathematical model previously developed for the description of this process was employed. In this paper we have examined in particular how small variations in key kinetic parameters impact on the autoclave&apos;s performance, i.e. attainment of autogenous steady-state temperature, zinc conversion and solution chemistry. The reaction parameters studied were: (i) stoichiometry of the marmatite leaching reaction; (ii) the activation energy of the same reaction, E,; (iii) the rate constant of the ferrous to ferric oxidation reaction, k,; and (iv) the apparent equilibrium constant for ferric precipitation, K,. This parameter sensitivity analysis was done under no oxygen mass transfer control limitations. Model predictions were found to be more sensitive to the kinetic parameters under certain conditions than others. The most dramatic finding was the one related to the small amount of sulfate produced during marmatite leaching. In connection to this it was found that the small percentage (< 5 %) of sulfate produced enhances the autothermal operational stability of the autoclave. The need for accurate kinetic parameter determination under conditions similar to those encountered in industrial zinc pressure leaching was demonstrated.

Jan 1, 1999

By Xun An

Slag from an electric slag cleaning furnace was injected with methane and air mixtures to facilitate the recovery of copper and cobalt. The effects of methane-to-air ratio, gas flow rate and temperature on the reduction and metal separation were investigated. The results showed that over 90 percent copper and up to 60 percent cobalt could be recovered from the slag with a gas utilisation of around 70 percent, as calculated by thermodynamic simulation. Methane-to- air ratio was a major factor affecting the rate of reduction under the present experimental conditions. Further, injection of gaseous reductants greatly enhanced the coalescence and settling of entrained metal droplets. A reduction mechanism is proposed and the factors influencing the coalescence of copper droplets are discussed.

Jan 1, 1998

By Daojin Cao

Aiming at many controversial reports on Raman spectral pattern of octamolybdate ion in aqueous solution appearing in the literature, a new method for the establishment of corresponding relation between Raman spectral pattern and chemical components of aqueous molybdate solution was put forward using spectroscopy measure and component analyses of saturated solution of ammonium octamolybdate hydrate known structure. It was found that the main characteristic of Raman spectral pattern of the saturated solution was described as the same ?double-peaks, hereinto a weak peak at the boundary? as some literature, but chemical components of the saturated solution were affirmed to be octamolybdate ion (Mo8O264-) and double protonated heptamolybdate ion (H2Mo7O244-), which were in equilibrium in aqueous solution each other. The authors propose that the pattern of the saturated solution can be regarded as the standard pattern of primiparous octamolybdate ion during acidified molybdate solution. It is satisfying that the standard pattern is applied to the identification of primiparous octamolybdate ion during acidified molybdate solution.

Jan 1, 2006

By G. L. Hundley, D. N. Nilsen

The U.S. Department of Energy investigated the use of liquid-emulsion membranes (LEM) for the selective removal and recovery of metals such as copper and zinc from mine waste waters. This investigation included field tests of a mobile, pilot plant-scale, continuous-flow LEM system. The system was tested at copper mines with solutions containing from 100 to 1,400 ppm Cu, and at a zinc mine with a solution containing 115 ppm Zn. Typical results from the copper tests were >90% copper recovery, and zinc extraction from waste water also was typically>90%. Although all of these waste waters contained high impurity levels, pure products were produced. On several of these field tests, integrated systems were tested that resulted in recovery of metal by-products, selectiv~ precipitation of iron, and polishing to reach discharge targets for essentially all of the contained metals. In addition, some results are included from laboratory-scale tests.

Jan 1, 2000

By Jerold L. Johnson

Remediation of small-arms firing ranges is being investigated by the Naval Civil Engineering Laboratory and the U.S. Bureau of Mines. Scheduled closures of military installations, as well as the management of active ranges, require the development of methodologies for heavy metals removal to prevent their entering the surrounding environment. The impact berms contain high concentrations of metals, and the soil and vegetation surrounding the berms were found to have slightly elevated levels. The heavy metals characterized are in the form of whole bullets, a wide size distribution of free fragments, smeared lead on the surface of the soil grains, and very finely attached particles. Gravity beneficiation can remove liberated metal contamination effectively. Weak acetic acid leaching shows promise in lowering the final metal contamination to allow the ,soil to pass the Environmental Protection Agency&apos;s (EPA) Toxicity Characteristic Leaching Procedure (TCLP) criteria.

Jan 1, 1993

By J. E. Clemson

The Black Pine sediment-hosted, disseminated gold deposit is located in Cassia County, Idaho. Gold mineralization occurs in flat-lying zones 50 to 100 feet thick. Total geological ore reserves are 5.6 million tons grading 0.049 oz/t. Ore types include: non-carbonaceous, oxidized ore; carbonaceous, sulfide ore; and carbonaceous, partly oxidized ore. In the oxidized ores, native gold grains commonly occur in porous hematite pseudomorphs that have replaced disseminated framboidal and euhedral pyrite, and this gold should be readily leached by cyanide solutions. Approximately 4 % of the native gold observed in the oxidized ores is locked within gangue and may be refractory to cyanide solutions. Native gold has not been observed in the unoxidized samples, all of which are characterized by primary sulfides. It is suspected that the bulk of the gold mineralization in the sulfide ore occurs as submicroscopic particles within pyrite and will be refractory to cyanidation. It is believed that much or all of the gold observed in the oxidized samples was originally in pyrite but was released and re-precipitated during oxidation. The degree of oxidation of the pyrite and the presence/absence of preg-robbing carbonaceous material is used as a guide in delimiting zones of mineralization amenable to heap leaching.

Jan 1, 1988

By G. Diáz

The PLACID process applied to the recycling of spent lead-acid batteries is being developed by an European Consortium within the Brite-Euram II programme. The status of the project entitled "Lead Recovery from Lead Oxide Secondaries" is described in this paper. The main laboratory and batch experimental results and the preliminary feasibility study are summarised. The description of the demonstration pilot plant and continuous campaigns programme for 1995 are also included. An interesting global approach is proposed, integrating the Placid process in the existing spent battery recycling pyrometallurgical facilities. This yields important improvements in the overall process. Grids would be easily treated by the conventional pyrometallurgical route, obtaining lead alloys,, while battery pastes, slags and fumes would be fed to the Placid process, obtaining pure electrolytic lead (>99.99 %), ideal for battery paste manufacturing. The implementation of the Placid process into the existing battery recycling pyrometallurgical facilities is analyzed from technical, environmental and economical viewpoints. Greater overall lead recovery, lower operating costs, reduced waste production, environmentally safer residues and much better lead product quality are the key advantages. The authors draw the following final conclusion : Integration of the Placid process with conventional pyrometallurgical treatment is a feasible and very attractive alternative route for spent lead-acid battery recycling.

Jan 1, 1995

By A. Cullaj

During a period of 15 years the metallurgical and chemical complex of Elbasan containing more than 15 principal plants, producing cast-iron, steel, coke, nickel carbonate, nickel, cobalt, chromium and other products, discharged into air, river water and soil an extensive amount of hazardous wastes containing high toxic substances. A monitoring study for the levels of heavy metals in soils nearby the former plant is carried out for the first time. Very high levels (total and extractable) of contaminants such as nickel, cobalt and chromium are found in samples taken from a relatively vast territory including the city of Elbasan, situated 8 kilometres far from the plant. The most polluted samples present a total content of 1211.8 ? 2949.6 mg/kg Ni, 97.0 ? 181.2 mg/kg Co and 1358.7 ? 4130 mg/kg Cr. These levels exceed several times the phytotoxic thresholds and present a potential hazard for the inhabitants. This study, as part of a bigger multinational project on solid decontamination, will also serve to the possible application of the new phytoremediation and phytoextraction technologies, being developed in parallel in this project.

Jan 1, 2006