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By Lassi Klemettinen

For better understanding and maximal value utilization of the WEEE smelting process, the behavior and distribution of different trace elements must be known. In this study, the behavior of nickel as a trace element was studied in an equilibrium system with metallic copper—spinel saturated iron silicate slag (with 3 wt-% K2O)—iron aluminous spinel—gas. The experiments were conducted in alumina crucibles at 1300 °C, in oxygen pressure range of 10−10–10−5 atm. A time series of 15–60 min experiments was also conducted for investigating the formation rate of the primary spinel phase in the system. The results show that the distribution coefficient of nickel between metallic copper and liquid slag changes from approximately 70 to 0.4 along the increasing oxygen pressure range. In addition, a significant part of the nickel deports into the spinel phase. The spinel formation was investigated based on composition analysis results and visual observations from SEM-images.

By J. L. Jambor

Previous crystal-structure determination of magnesian annabergite (Ni,MgMAsO4)2 8H2O indicated that ordering of Ni and Mg occurs in non-equivalent octahedral sites; such ordering supports the possibility of miscibility gaps on the Ni3(AsO4)2 8H2O -MgiAs04)2 8H2O. (annabergite-hornesite) join. In a predecessor study based on analyses of natural specimens, it was proposed that solid solution is incomplete both for annabergite-hornesite and annabergite-erythrite [Co, (AsO4)2 8H2O]. In the current study, syntheses by use of a slow-addition technique and aging of the precipitates indicated that the annabergite-erythrite solid solution is complete, and that no miscibility gap is present on the annabergite-hornesite join to at least 58 mol % Mg. Thus, interpretation of the compositions of these phases in oxidized mill-tailings impoundments can be done with the normal precautions for homogeneity, and without the added concern of the possible presence of miscibility gaps in the ternary system.

Jan 1, 1995

By P. M. Tyroler

Inco operates a hydrometallurgical plant to treat the residue from the pressure carbonylation process. The main constituent in the residue is cop¬per. The residue is leached under pressure in an acid sulphate solution in two stages and the copper is recovered via electrowinning. The electrowinning tankhouse is fully integrated into the overall plant flowsheet as spent elect¬rolyte is required in upstream leaching steps. In recent years, the amount of residue had increased and copper removal capacity became the rate limiting factor for the entire plant. Consequently, a major program was undertaken to upgrade the tankhouse with regards to capacity, efficiency, cathode quality, working environment and structual integrity and appearance. This paper will describe current facilities and operation, and detail progress in our up¬grading efforts.

Jan 1, 1987

By Kimiaki Utsunomiya, Yasumasa Hattori, Yoshiaki Mori, Toyokazu Okubo

"The effect of various operating conditions on splashing behavior in a Peirce-Smith converter has been investigated with a 1/5.7 scale cold model. Dynamic similarity between the model and a commercial converter was attained by setting the modified Froude number in the model experiments in· the range for normal converter operation. It is known that for a given modified Froude number the dimensionless penetration length of gas into the liquid phase increases as the liquid density decreases. Moreover, penetration· length has a large effect on splashing behavior. Therefore, a heavy liquid, a mixture of water and lead concentrate was used as the liquid phase. It was concluded that the amount of splash dramatically decreases with a reduction in the buoyancy energy per, unit liquid mass and an increase in the horizontal distance between the tuyere tip and the edge of the mouth.IntroductionSubmerged gas injection is widely used in practice in ferrous and nonferrous pyrometallurgical operations to achieve large gas-liquid contact areas and good agitation of liquid for rapid chemical reaction. The common application in ·nonferrous industry is the Peirce-Smith converter with multi-tuyere for copper and nickel matte converting. This process has been used for over 100 years because of its effectiveness in mixing of the molten bath, as well as its merits of the engineering simplicity. However, the mechanisms which · determine the blowing performance is poorly understood, and the design and operating conditions of the Peirce-Smith converter varies widely from plant to plant, such as by diameter, length, mouth angle, tuyere position and level of molten matte. Smelters have continuously made an effort to increase converter productivity, implying maximum tuyere blowing rate. Above a certain critical blowing rate, splash of molten matte from the converter mouth becomes unacceptable because of dangerous ejection and accretion buildup around the converter mouth, which results in interference with effective hood sealing. In fact, a 1993 converter survey[!] reported that splash was a major limiting factor for blowing rate and 54% of responding plants from around the world regard it as a limiting condition[2]. In order to increase tuyere blowing rate a study of the effect of various operating conditions on splashing behavior is expected."

Jan 1, 2000

By Li Kaihua, Li Liang, Miao Qingdong, Wang Cong

The current process of production of titanium sponge involves the use of TiCl4 as a feed material and a huge amount of heat is generated during the magnesiothermic reduction process. For this reason, it is possible to agglomerate into a titanium lump with the partial high temperature. And, it is difficult to obtain soft titanium sponge with low content of impurities. In order to solve the current problems in the titanium sponge production process, process optimization experiments study of TiCl4 feeding speed, vacuum distillation temperature, system pressure and time control had been conducted for obtain high quality titanium sponge. Experimental results show that lower feeding speed can improve the output capacity of titanium sponge and softer products can be obtained. The product grade rate of titanium sponge improved significantly.

Jan 1, 2015

By Wilhelm Wendt

About five years ago we showed that it is possible to use the spectral in- formation in the light emitted by the off-gas flame of a PS converter for on-line production control. Very recently measurements have been performed using improved optical equipment and data evaluation software, resulting in both improved accuracy and the establishment of new optical process parameters. Using the optical signals the slag heats could be stopped at a predetermined Cu content of the white metal with an accuracy of +0.2% Cu m the range 74-78% Cu. A good correlation was found between the slag composition and optical data, providing a possibility for on-line monitoring of the SiO2 content of the slag. The measurements indicate the possibility of predicting the optimum end-point of the copper-making stage and having real time information on the impurity removal. Factors influencing the optical parameters, such as blowrate, Pb content, temperature etc. will be discussed.

Jan 1, 1993

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 Petrus Christiaan Pistorius, Farzin Fatollahi-Fard

The production of synthetic rutile—a common starting material for most titanium production processes—from iron-rich titanium minerals such as pseudorutile and ilmenite is described. The process for “upgrading” the mineral to synthetic rutile is by carbothermal reduction of the mineral while immersed in a molten salt at high temperature, followed by magnetic separation of the reduced iron. A variety of factors are also investigated, such as particle size of the mineral, the type of mineral, and the molten salt used. The solubility of iron(III) oxide in different molten salts is also experimentally determined.

Jan 1, 2016

By Xiao Y. Yan

A fused salt electrochemical process was investigated for the synthesis of non-oxide ceramic powders directly from metal oxides, boric oxide, and carbon powders by electro-deoxidation. Sintered pellets of the mixed powders were designed to act as a composite cathode in the electrolytic cell. Electrolysis was carried out in molten CaCl2-NaCl eutectic at 3.1 V and at 600-900 ºC under argon. The favoured cathodic reaction was the removal of the oxygen from the oxides to produce metal atoms that reacted with either the reduced boron atoms, forming a metal boride, or the carbon initially present in the sintered pellets to produce a metal carbide. The technical viability of the process was demonstrated by the electro-deoxidation of sintered pellets of TiO2/B2O3 and TiO2/C to produce TiB2 and TiC, respectively. Compared to existing carbothermic reduction process, this new electrochemical process may be less energy intensive and may lead to lower production costs. I

Jan 1, 2008

By J. W. Lyman

The U.S. Department of the Interior, Bureau of Mines, investigated methods to recover valuable rare-earth materials from NdFeB magnet scrap. Although several processing techniques were evaluated" the best separation of rare earths from the NdFeB magnet ,scrap was obtained by sulfuric acid dissolution followed by precipitation of recyclable rare-earth salts. Both sodium and ammonium intermediate double-salt precipitates' that can be converted to a variety of useful neodymium products were investigated. The sodium system showed a neodymium recovery of 98 pct, while the ammonium system yielded 70 pct during double-salt precipitation. The iron-rich effluent following the rare-earth recovery was treated to produce sodium and ammonium iron jarosites that can be disposed of or converted to hematite. By following this new procedure, many materials handling and economic disadvantages found with fluoride or oxalate direct precipitation were avoided.

Jan 1, 1992

By A. A. el-Geassy

High-grade iron ore fines rejected from the DRl plants (>96%Fe20) were isothermally reduced in 30-60%COIH2 gas mixtures at 973-1273K. The freshly reduced reaction products were then subsequently carburised in either H2/CO or H2/CO/S mixtures at 823-1073K for 30-120 min. The thermogarvimetric technique was used to follow up both of reduction and carburisation reactions as a function of time. The carburised samples were characterized by X-ray and Mossbauer techniques. Chemical and carbon analyses were also applied. The influence of temperature and gas composition on the reduction behavior was investigated. The calculated values of apparent activation energy, application of gas-solid mathematical formulations were correlated with the microstructures to predict the reduction mechanism, The influence of carburization time, temperature, CO contents in H2/CO or H2/CO/S were investigated. A conversion extent of Fe to Fe3C was taken as a measurable index for the efficiency of carburization reaction under the different experimental conditions.

Jan 1, 2003

By Kumar P. Dharmasena, Haydn N. G. Wadley, Bill W. Choi

"Non-contact eddy current sensing methods have been developed and applied to Cd0.955Zn0.045Te crystal growth to obtain a better understanding of the melt, solid nucleation, and the growth process. The application of this sensor approach relies on a large difference in liquid and solid electrical conductivities near the melting point and requires knowledge of the relationships between the electrical conductivity, melt composition, and temperature. Using a multifrequency encircling eddy current sensor, the electrical conductivities of three different Cd1-xZnxTe (x=0.00, 0.045, and 0.08) alloys were measured as a function of temperature in a laboratory-scale vertical Bridgman furnace. The measured solid and liquid electrical conductivities were then used in electromagnetic finite element models to analyze the multifrequency responses of eddy current sensor designs during the simulated growth of a crystal. These eddy current sensors were fabricated and installed in a vertical Bridgman furnace and used to monitor many Cd0.955Zn0.045 Te growth runs. One sensor was placed in the vicinity of the ampoule tip to detect undercooling/spontaneous nucleation and two other sensors (""absolute"" and ""differential"" designs) placed to monitor the movement/curvature of the liquid-solid interface during crystal growth. The sensor data was used to characterize the initial melt state, detect the onset of nucle-ation, determine the growth velocity, and identify the shape of the interface.IntroductionSingle crystal CdTe and its solid solution Cd1-xZnxTe alloys (0.03<x<0.05) are used as infrared transparent substrates for infrared focal plane array (IRFPA) detectors [1-6] and as solid state y- ray detectors [7-9j. Cd1-xZnxTe substrates are normally ""mined"" from large polycrystalline boules grown by the unseeded directional solidification of Cd1-xZnxTe melts using either a vertical or horizontal Bridgman process [10-14]. The vertical Bridgman method is particularly popular for growing CdTe and its related compounds. In this process, a Cd1-xZnxTe ingot is produced by first melting a charge in the hot zone of the furnace and then vertically translating the furnace (with its associated axial temperature profile) relative to the stationary crucible to cause directional solidification. In spite of many experimental efforts to investigate the relationships between material purity, stoichiometry, the controllable growth parameters (furnace temperature profiles, ampoule geometries/materials, furnace translation rates and starting position) and the resulting material characteristics (grain structure, dislocation densities, IR transmission, macro-segregation etc.), the yield of Cd1-xZnxTe of a quality suitable for large area (e.g. 4 cm x 6 cm) substrates remains low (<10%). Since much of this poor yield is directly associated with the crystal growth process (e.g. melt stoichiometry, solidification velocity, interface shape, temperature gradients, cooling rate, etc.) intensive efforts are under way to improve this technology."

Jan 1, 1997

By Ronald Klepper

In hydrometallurgy, pure gases like oxygen and hydrogen are used for oxidation and reduction. The gases are expensive and therefore should be used efficiently. Non reacted gas can be recycled into the liquid. Historically vortex gassing has been used; Le. a mixing impeller close to the liquid surface entrains gas from the headspace into the liquid through a gas vortex. Novel and more efficient methods are surface gassing with up pumping impellers and self- inducing gassing impellers. These alternative impeller systems are well established and common in the chemical industry, but have not been used until recently in hydrometallurgy. Gassing impellers act as internal compressors and increase the interfacial surface for a much higher mass transfer compared to alternate methods mentioned. In the paper results from lab and pilot tests and data from operated plants will be presented. The reactions with gases normally take place under moderate to high pressure, therefore a safe enclosure with mechanical seals and the safety "philosophy" is important. Experienced life and replacement cycles will be reported.

Jan 1, 2000

By Frederic Pineau

Semisolid metal alloys have a special microstructure of globular grains suspended in a liquid metal matrix. This particular physical state of the matter can be exploited to produce near-net- shape parts with improved mechanical properties. However, the behavior of the slurry is strongly influenced by the local solid fraction and state of agglomeration. Different flow instabilities ·associated with the combined flow and solidification process result, which make difficult the application of semi-solid processing in the casting industry. Moreover, the rheology of semisolid materials is not well understood. Most of the theory has been derived from experimental data, which are somewhat difficult to measure. A model that accounts for the multiphase nature of semisolid slurries is required to get more insight into such complex flows. This paper describes a mixture model for semisolid slurries. It assumes that the mixture of liquid-solid components behaves as a single fluid as far as overall mass and momentum balances are concerned. The coupling force between the phases is derived on the assumption that the slurry is a fluid saturated isotropic media. The proposed methodology is implemented in a finite element code. The model is then applied to the the filling of an industrial-scale capillary flow viscometer. Segregation patterns are obtained and discussed.

Jan 1, 2001

By Toshihiko Emi

The quest for cleaner steel is driven by increasingly stringent requirements from the manufacturing and construction industries. Key issues are the occurrence and removal of inclusions; These are discussed in the context of the unit processes of deoxidation, refining, transfer and casting of molten steel. Process thermodynamics and kinetics are also discussed. Recent progresses achieved and problems yet to be solved are elaborated, and an integration of the unit processes into a system to produce extra clean, steels with better performance is presented.

Jan 1, 1999

By Zbigniew Zurecki

The selection of atmosphere composition is critical for controlling surface quality of reactive aluminum alloys during solution treatments. An improper selection of annealing atmosphere can result in surface blistering in AI-Mg and sub-surface depletion of lithium in AI-U ingots. To determine optimum atmosphere compositions for homogenizing A1-Mg and Al-Li alloys, Ii number of exploratory experiments were carried out in air, nitrogen, and carbon dioxide based atmospheres including reactive impurities or additive such as moisture and sulfur hexafluoride. This paper describes the influence of these atmospheres on high-temperature oxidation and sub-surface defects. The results are discussed in terms of the change in Pilling-Bedworth ratio.

Jan 1, 1996

By Y. A. Chang, J. Woodford, C. R. Kao

Reactive diffusion studies between NbC and Si were carried out at 1300 °C under a vacuum of 10-5 torr and a uniaxial pressure of 1 MPa. The annealing time ranged from 8 to 100 hours. The Si used was single crystal silicon; the NbC was hot-pressed powder compact. A NbSi2+SiC two-phase reaction layer formed with NbSi2 as the matrix and SiC as discontinuous particles. The microstructure of the reaction product is homogeneous, dense, and fine. The NbSi2 grain size and SiC particle size are in the micron range. The growth of the reaction products follows parabolic kinetics. Extrapolation of the data to zero thickness suggests an apparent incubation time of 3.5 hours. However, for short annealing time «60 hours), the thickness data can be approximated by linear kinetics with an initial growth rate of about 2 11m/hr. Based on these experimental observations, a growth mechanism for the reactive diffusion between Si single crystal and NbC powder compact is proposed. We propose that the nucleation sites for the SiC particles are at the voids of the NbC powder compact. This proposed nucleation mechanism offers a potential way of controlling the SiC particle size by changing the void size and void density of the NbC powder compact. This hypothesis, if proven to be true, will allow us to control mechanical properties of the composites by tailoring the SiC particles formed. It is also pointed out that the microstructure requires Si to be the dominant diffusing species and to diffuse through the reaction layer, while Nb and Conly have to undergo local rearrangement.

Jan 1, 1996

By John E. Litz

The Denver Process is a chemical/metallurgical process for treating radioactive or mixed wastes by extraction and concentration of the radioactive and/or hazardous component(s). The process was developed at bench scale, evaluated at pilot scale, and will be implemented at full scale to remediate a low-level radioactive sludge. Six unit operations comprise the process: feed handling, leaching, solvent extraction, electrodeposition, precipitation, and tailing preparation. Unit operation design may be modified to tailor the process for varying feed stock composition. Radioactive or mixed waste is reacted with aggressive reagents in an aqueous phase, solubilizing targeted components. These components are then selectively extracted and concentrated in subsequent steps. Waste solids and solution exit the process as non-hazardous non¬radioactive waste. Dehydration of aqueous waste by submerged combustion eliminates aqueous discharge.

Jan 1, 1994

By Dong Liang, Qijie Zhai, Zhichen Zhang, Qixin Li, Zhishuai Xu

"The formation, distribution and survival of pure Al nuclei under surface pulsed magneto oscillation (SPMO) treatment were investigated with thecombination of experiments and numerical simulation. The results indicated that the nuclei originated from the whole top surface of melt owing to the oscillation of top surface induced by SPMO. The temperature field significantly affected the survival of the nuclei The electromagnetic force and flow field of the melt with SPMO treatment were simulated by finite element software ANSYS. The electromagnetic force mainly distributed below the top surface near the mould wall. The electromagnetic farce not only made the melt oscillate but also increased the convection of meh below the top surface vigorously. The oscillation near the top surface of the melt promoted the nucleation largely, and the convection increased the uniform of the temperature distribution in the whole meh which favored the survival of nucleiIntroductionAs we all know, fine equiaxed grains are beneficial fur the improvement of the mechanical property, process ability and the uniformity of metallic materials [1-2]. With the researches of recent decades, people discovered that the electromagnetic field is an efficient method to refine the solidified structure of metals [3-7]. Pulsed magnetic field technology obtains more and more attentions in recent years due to its smaller power consumption, bigger instantaneous magnetic field intensity, non-contacting with the meh and simple convenient equipment manufacturing [8-9]. However, the melts would splash fiercely when pulsed magnetic field is applied with a slightly higher power. Thus, based on the understanding of the solidification refinement mechanism of electric current pulse (ECP) [10], Gong et al [11] developed a novel technology called pulse magneto-oscillation (PMO) to refine the solidification structure. The technology can be easily applied in the solidification structure refinement of continuous casting slab. But fur aluminum continuous casting, the sump is very shallow, which greatly limits the application of pulse magneto-oscillation technology."

Jan 1, 2014

By Frank A. Stephens

The process of converting iron ore (principally Fe,03 or Fe30,) into iron carbide (Fe,C) to be used as feedstock for steel-making yields complex mixtures of several Fe-containing compounds as a function of processing conditions. In addition to the above compounds (hematite, magnetite and cementite), the mixtures typically contain wustite (FeO) and metallic iron(Fe). Mossbauer spectroscopy has been developed into aquantitative analytical method for monitoring the degree of conversion to carbide from samples periodically extracted from a fluidized bed reactor type of pilot plant. Calibration of absolute quantities of the above five compounds is based on standards prepared from known mixtures of the high purity individual phases. The PC-based spectrometer allows fitting of the well-known spectral components of each of the five phases, the resulting spectral areas then being compared with the calibration curves via PC software to yield the weight fraction of each. Emphasis has been placed on standardizing and simplifying the analysis procedure for routine use in an industrial environment.

Jan 1, 1993