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By Taufiq Hidayat

Accurate description of complex phase equilibria provide the foundations for the improvement of non-ferrous pyrometallurgical smelting and recycling processes. Recent advances in microanalysis and experimental techniques enable accurate phase equilibria characterisation. Quantitative microanalytical techniques including Electron Probe X-ray Microanalysis and Laser Ablation ICP-MS enable the concentrations of major and minor elements present in different phases in samples to be accurately measured providing data that cannot be obtained using bulk chemical analysis techniques. High-temperature equilibration experiments coupled with the subsequent analysis of elementary reactions at micro- and macro-scales ensure the attainment of equilibrium conditions, and therefore, ensure true phase equilibria information is obtained. Examples of the application of the improved methodology on the investigation of phase equilibria of low-order and complex, multi-component gas/slag/matte/metal/solids Cu2O–PbO–ZnO–Al2O3–CaO–MgO– FeO–Fe2O3–SiO2–S systems and the distribution of minor element are provided. The experimental study is closely integrated with thermodynamic database development for the above system. Example of implementation of the research outcomes into industrial operations is demonstrated.

By Darryl Lovato, Ramiro Pereyra, Daniel S. Schwartz

"During an annual inventory of nuclear material, a plated steel container which contained plutonium oxide failed. The container had been packaged for temporary storage but had been overlooked and remained in storage for more than 23 years. Although it was determined that the failure occurred through the slip-top rim, a metallurgical evaluation was requested to help to determine the integrity of the container.Optical metallography and scanning electron microscopy were used to analyze the character and degree of corrosion in the container. The depth of corrosion, measured at approximately 10 µm, did not pose a threat to the integrity of the container. However, the corrosion morphology and chemistry did suggest that a galvanic cell had developed between the tin and steel from the condensation of water. The morphology also suggests that the attack of the steel took place over a series of cycles due to changes of the environment.IntroductionMetallographic analysis was requested as part of the investigation into the mechanism of the failure of a slip-top container (#38621) containing plutonium oxide (PuO2) powder. The container had leaked during a special nuclear material (SNM) annual inventory causing contamination and closure of the vault. A photograph of the container and interior container is shown on the right in Figure 1. An initial investigation established that the source of contamination was the consequence of the failure of multiple layers of containment. Initially by the deterioration of the interior plastic bottle and polyvinyl chloride (PVC) bagout bag, and finally through the lid and steel container interface at a location where tape had not adhered properly [1]. Although the source of the breach was established, it was determined that metallographic analysis was important to establish the extent of deterioration of the steel container."

Jan 1, 2008

By Frustino L. Prado

For more than a century, the AAC (ammonia I ammonium carbonate) process has been applied to the recovery of various metals. A variation of it, the Caron Process was first used in the early 1940's in Cuba for the extraction and recovery of nickel from laterites. The original Nicaro plant has been in continuous operation since then. Years later the Caron process was used again in Australia at the Greenvale (Yabulu) NickelICobalt plant, commissioned in 1974. Other projects (Sered, Niquelandia, Nonoc, Punta Gorda, Albania) as well as several studies have been carried out. The Caron Process is alive and still promising. Members of our organization have been working with AAC and the Caron Process since 1952. This paper will review current approaches and potential improvements (enhancement of recoveries of Ni and Co, reduced energy consumption and maintenance simplification). Keywords: Caron Process, Ammonia, Ammonium Carbonate, Laterites, Nickel, Cobalt

Jan 1, 2004

By M. El Ganaoui, P. Bontoux

"A computational model to investigate solid/liquid phase change transitions for binary alloy under directional solidification is presented. Conservation equations are developed by using an homogeneous formulation. A second order accuracy method of time and space based on finite volume approximation has been evaluated by comparing results to spectral solution for time-dependent solutal convection developping in a melted alloy. For extended model to solid/liquid interface effects time amplification of solutal perturbation injected near the interface is described before considering solutal convection is melt.IntroductionThe enthalpy method gives a front fixing approach for energy equation without introducing coordinate transformation. The interfare position is recovered a posteriori [1]. A number of authors have extended this approach so as to include the convection phenomena within the two phase 'mushy region' [2, 3, 4, 5, 6].We have developed a time-dependent enthalpy-porosity formulation for directional solidification [4, 6, 8]. The interaction between solid and liquid phases is modelised by a Darcien type force in the phase change area. The behaviour of the melt is similar with the flow of an incompressible fluid in a porous medium. This force is proportional to the relative phase velocity. It corresponds to a damping force depending on the anisotropic permeability of the 'mushy zone'. The permeability depends on the liquid fraction and on the size of·solidification microstructures. An informative discussion of a new slant on the general approach of continuum mechanics needed to analyze the formation of mushy zone is given in [12]. The method is extended to the presence of species diffusion: the solutal Stefan condition which expresses the solute incorporation or rejection across the interface is accounted implicitly in a species equation valid in all the domain [14, 15]."

Jan 1, 2001

By R. F. Hammen

Heavy metal contamination of water is a problem of immense national and international proportions. However, effective cleanup is complicated both by the toxicity and the low concentrations of metals in wastewater streams. Using high performance chelation chromatography, the solid phase extraction and purification of extremely dilute metals from water was highly effective. The process is based on selective displacement of metals from a chromatographic column containing a chelating resin. The resin is characterized by extremely efficient adsorption kinetics which allow rapid and complete removal of the metals.

Jan 1, 1993

By O. Ryosuke Suzuki

A new metallurgical process via sulfide is proposed: a sulfide is produced at a high temperature from its metallic oxide using gaseous CS2, and this sulfide is electrochemically reduced to its metallic state using molten salt. This combined process via sulfide is effective to obtain high purity of metallic powder, even if the metal in its oxide is strongly combined with oxygen. For example, it is not easy to reduce stable oxide TiO2, and only Ca can remove oxygen to form α-Ti. However, a fairly large amount of oxygen remains as Ti–O solid solution. Because the solubility of S in Ti is very small, this proposal was examined experimentally both on the conversion of TiO2 to TiS2 and on the successive reduction of TiS2 to Ti. TiO2 powder was exposed to CS2 gas flow at 1073 K, and the conversion to TiS2 was confirmed. TiS2 could be reduced to Ti powder either by calciothermic reduction or electrolysis in a CaCl2 melt. By Ca reduction at 1133 K in CaCl2 melt, sulfur concentration decreased to 0.03 mass%S when the amount greater than twice the stoichiometric calcium amount is added. By electrochemical reduction at 1173 K in CaCl2–CaS melt, S concentration significantly decreased to 0.01 mass% S when four times larger amount of electric charge was supplied.

By Jorge Alberto Soares Tenório, Flávia Paulucci Cianga Silvas, Bianca Medeiros, Denise Crocce Romano Espinosa, Ivo André Homrich Schneider, Daniella Cardoso Buzzi, José Roberto de Oliveira

"AMD is one of the main problems associated with mining activities and the techniques used in their treatment may be the biosorption. The aim of this work was to study the rice husk as a biosorbent for the AMD treatment keeping constant: pH (2.6), biomass concentration (1g.L-1), temperature (25°C) and agitation (175rpm). And varying the contact time of 5, 20, 60 and 240 minutes. Rice husk samples will be characterized before and after the biosorptives tests through analysis of SEM and IR. The micrographs indicate the occurrence of micro-precipitation and changes in biomass physical structure. Since the infrared spectra indicate changes in functional groups present in the biomass before and after the biosorptives tests. AMD synthetic solutions will be analyzed by ICP in order to quantify the metals concentration captured by biomassIntroductionThe preoccupation for the environment has led the industry in general, to treat their waste. As the only industrial activity is increasing, the pollutants generated must undergo treatment processes aimed at reducing pollution, and therefore, less aggression ecosystems.In mining there is waste water with accumulation of heavy metals, and these are harmful to health of living beings, thus being one of those industries responsible for some pollution of the environment. These wastewater in contact with oxygen to generate an acidic water is called acid mine drainage (AMD). This aqueous solution has a pH below 3 and varieties of dissolved metals. When this solution comes in contact with water, generates a series of environmental problems, so there is a need to recover the metals present in the DAM."

Jan 1, 2012

By Mahesh C. Meyer Jha

AMAX has developed a chloride refining process to produce pure nickel and cobalt metals from mixed sulfide .precipitates, Metal chloride solutions, generated in a hydrochloric acid leaching step and purified in a solvent extraction circuit, are converted to metal oxides .and HCI gas by pyrohydrolysis. A pilot plant consisting of a 30-inch diameter fluidized bed reactor and other ancillary units was designed, constructed, and operated for over one year. Process design was aimed at minimizing energy consumption, maximizing conversion efficiency, and achieving simplicity of operation and control. The operation provided valuable information on process scale up parameters, process control strategies, and materials of construction., Several process variables such as bed temperature, solution composition, solution feeding system, bed particle size distribution, and fines recycle system were investigated to determine their effects on process efficiency and the physical and chemical characteristics of the product.

Jan 1, 1985

By R. Y. Wan, S. L. Chryssoulis

"Gold associations were established in a·biooxidized, chlorinated CIL residue assaying 0.02 oz Ault and in a biooxidized thiosulfate leach residue assaying 0.01 oz Au/t. A detailed mineralogical study involved: assays of screened fractions; light microscopy; ion probe microanalysis to quantify 'invisible' gold in sulfide minerals; proton probe microanalysis to detect and quantify preg-robbed gold. In the CIL residue, most of the gold is preg-robbed (71 %). In the thiosulfate leach residue, gold occurs mainly as submicroscopic disseminations in microcrystalline quartz (chert). In both residues, the 'invisible' gold in pyrite accounts for a minor fraction of the gold assay. Quantitative determination of the gold occurrence in the two residue samples established conclusively that gold adsorption on carbonaceous matter in the thiosulfate leach is of minor importance.Acknowledgement: published with permission of Newmont Gold Company."

Jan 1, 1997

By Terry Gerritsen

Electrode control systems regulate power by physically positioning electrodes. Due to the size and weight of the electrodes, this is a slow process where power fluctuations of less than a few seconds are not fully corrected. Nickel laterite AC furnaces operating in high voltage, shielded arc mode typically incur frequent power variations of approximately +I- 20% around the power set point. To provide enhanced power control, Hatch has recently supplied, at commercial scale, a thyristor-switched reactance system called an SPLC. The SPLC incorporates predictive control software to operate furnaces at the maximum transformer rating by reducing the large power swings experienced without the SPLC. The resulting higher average power enables higher production, without increasing transformer or power plant capacity. A 60 MW production version of the SPLC has been commissioned on Falconbridge Dominicans's laterite nickel furnace, yielding excellent results with a 3 to I reduction in power fluctuations. Keywords: SPLC, AC Power Supply, Electric Furnace

Jan 1, 2004

By Brian Patrick, Norman Bell, Mark Schoenfield, Thomas Weber, Dietrich Gross

"The reduction of carbon dioxide emissions and the resultant greenhouse gas affect is hampered by the fact that all fossil fuels contain copious quantities of carbon. Process tweaking can keep the amount of carbon dioxide to a minimum but cannot significantly reduce the amount of carbon dioxide generated. The very nature of utilizing fuels requires that they be burned to release the heat required for the various processes. Reduction of metal oxides to manufacture or modify pure metals, generation of power, transportation and many other forms of fuel usage result in much of the generation of man made carbon dioxide. Oxyfuel is a unique contributor to carbon dioxide emissions. While creating higher concentrations of carbon dioxide the total volume of carbon dioxide generated is reduced. This paper will examine the unique characteristics and potential of oxyfuel that make the generation of lower volumes of carbon dioxide possible.Nearly ten years ago a commercial application of oxy-fuel was installed at Jupiter Aluminum Company in Hammond, Indiana. This process was funded and developed by Dietrich Gross CEO. This aluminum remelt facility now runs completely on oxy-fuel and has continuously for over ten years. This has reduced the melt rates to as low as 750 BTU per pound in continuous melting periods."

Jan 1, 2009

By B. M. Fisher

A process for making electrolytic copper of high quality from copper flotation concentrates is described. The concentrates are first slurried and then subjected to a high-temperature, high-pressure, oxidation-leaching operation under controlled conditions. The resulting slurry from the oxidation-leaching operation is cooled or flashed to atmospheric pressure and then subjected to a solids-liquid separation. The separated liquor, containing the recovered copper values, is cooled and then fed to an electrolytic deposition operation where metallic copper cathodes of high purity are produced. The spent electrolyte is then subjected to a sulfide treatment to precipitate the residual amounts of copper not deposited in the electrolytic cells. The precipitated copper sulfide is recovered and recycled in the form of a slurry to the initial stages of the process.

Jan 1, 1976

By W. G. Davenport

Flash smelting is used. mainly for making molten Cu-rich matte* from fine Cu-Fe-S** flotation concentrates. It blows dried concentrate particles into a hot fumace, surrounds them with 01-rich gas and allows them to react. The results are: (a) partial oxidation of Fe and S from the concentrate (b) generation of heat (c) melting of the oxidized particles to form molten Cu-rich matte, ~65% Cu and Cu-barren slag, ~1 % Cu. The melted particles fall to the hearth of the flash furnace where they fonn matte and slag layers, The matte is tapped from the furnace and oxidation-converted to metallic copper. The slag is skimmed, treated for Cu recovery then stockpiled or sold. Figures 1.1 and 1.2 show industrial flash furnaces and the position of flash smelting in the coppermaking flowsheet. ,Fig. 1.3 shows the locations of flash furnaces around the world.

Jan 1, 2001

By Milorad Cirkovic

Kinetics of copper concentrate oxidation in roasting processes in a fluidized bed reactor has been studied at temperatures between 600°C and 720°C using particles of 0.038 to 2.5 mm in average size. The analysis of composition of samples has been done by chemical methods. Phase composition has been determined by Siemens X-ray equipment with Cu anticathode and Ni filters at a voltage of 40 kV and a current of 18 mA. The content of sulphur has decreased from 33.23 to 19.02 mass percent with the increase of temperature, but the content of Fe304 has increased from 0.15 to 17.14 mass percent. The new mechanism of copper concentrate oxidation in a fluidized bed reactor is proposed in this study. It has been shown from the mathematical model that the velocity of oxidation of copper concentrate between 600°C and 720°C is virtually controlled by the rate of diffusion of 02 through the layer of reaction product.

Jan 1, 1999

By P. Ret, E. Üstiindag, R. Dieckmann, R. Subramanian, S. L. Sass

"Partial reduction reactions in the Ni-AI-O system, starting with the spinel compound NiAI20 4, are used to form metal-ceramic microstructures. By suitable choice of processing parameters, such as reduction temperature, oxygen partial pressure and time, two different morphologies of nearly pure Ni particles, equiaxed and rod-like, form within a ceramic matrix, which is either a-A12O3 or a metastable ""defect spinel"". Electron microscopy studies were performed for microstructural characterization, phase identification and chemical analysis. The fracture toughness of the Ni-AI2O 3 mixture was significantly improved with respect to that of the original spinel phase. The important issues that must be addressed to form useful metal-ceramic microstructures by partial reduction reactions rue discussed. It is shown that cracking at the original spinel grain boundaries, likely due to the large volume changes associated with the reduction reaction, can be avoided by the addition of small amounts of ZrO2• Initial results illustrating effect of ZrO2 on the microsuuctures are presented.IntroductionEngineering materials used in load bearing circumstances, particularly under extreme conditions (e.g. high temperatures or stresses), generally are formulated with complex microsuuctures. Such composite-like materials can possess properties unobtainable by either of the individual constituents. With metal-ceramic composites, for example, a material can be obtained with an optimum combination of the low density and high strength of the ceramic, and the toughness of the metal. For high temperature service, where demanding conditions are often present, for example, inside jet turbine engines, a successful new material must have low density, high Young's modulus as well as good oxidation resistance, strength, fracture toughness, creep and fatigue resistance. The candidates include intermetallic compounds, and metal-ceramic, intermetallic-ceramic and ceramic-ceramic composites."

Jan 1, 1994

By Rodney J. Ishak

The reduction of Mn3O4 to MnO has been investigated in a thermobalance apparatus, The charge was composed of manganese ore (decomposed by heating/calcination or pre-reduction to mainly Mn3O4) and coke. The material was charged to a crucible, which was suspended in the balance. CO-gas was distributed through a grid in the bottom of the crucible. Two sizes of ores were used; 2.4-4.8 mm and 6,7-9.5 mm. Coke particles were in the size range 4.8-6.7 mm. Experiments were conducted in the 900-1100°C temperature range. The composition of the product gas was monitored continuously. External mass transport between bulk gas and particle surface does not seem to limit the rate of reduction. Assuming that both diffusion through product layer and chemical reaction at the interface between MnO and Mn)04 are rate controlling, the data was tried both in a shrinking core model and in a grain model using regression. The grain model gives the best physical description of the process, because the reactant is in fact a porous medium. With this model the effective diffusivity was calculated to be in the 1.5-6.10.5 m2/s range. The pore size was mainly between 0.1 and 10 um,

Jan 1, 2003

By Hector Henao

To provide thermodynamic data for converting the nickel matte to liquid nickel, an experimental study was conducted in the phase equilibrium between the Ni-S alloy and the CaO-Ah03 based slag melted in a MgO crucible at 1873 K under controlled Pso2 of 10.1 kPa and pO;, in a range between 2.5x,IO,2 and 10.1 Pa by using CO-C02-S0Z gas mixtures. The content of nickel in the slag at POz of 10.1 Pa, above which solid NiO is expected to precipitate in the equilibrium state, was found to be 4.1 mass% and the contents of sulfur and oxygen in the nickel melt were 0.4 and 0.2 mass%, respectively. It was clarified that increase in the temperature reduces the solubility of nickel in the slag and the contents of sulfur and oxygen in the alloy. The distribution of minor elements such as gold, silver, copper, cobalt, iron, arsenic and antimony between the Ni-S alloy and the CaO-AI20) based slag was also studied. The distribution ratios of iron and cobalt, defined by (%X in slag)/[%X in alloy] where X is the minor element, are larger values than that of nickel, while those of copper, silver and antimony are similar to that of nickel. The distribution ratios of arsenic and gold are lower than that of nickel in the higher range of oxygen partial' pressure.

Jan 1, 2003

By S. Z. El-Tawil, K. A. El-Barawy, M. B. Morsi, M. M. Nasr, Z. I. Zaki

"Tue sulphatization of zinc concentrate produced from heated zinc concentrate of Um Ghieg area, eastern desert by ammonium sulphate as sulphatizing agent is carried out at different conditions to achieve the appreciable formation of soluble sulphates. The maximum zinc recovery as soluble sulphate equfils to 95% upon using 1.5 stoichiometry ammonium sulphate at 600 °C for one hour. Tue obtained leached zinc sulphate solution is subjected· to purification process to prepare high pure zinc metal and zmc compounds such as pure zinc sulphate, zinc caibonate and zinc oxide. The products obtained are analyzed chemically and identified by X-ray analysisTue mechanism and kinetics of the sulphatization process of zinc concentrate are considered where the activation energy is calculated and equals to 33.3 K.J.mol""1 A process flowsheet for the overall sulphatization process of zinc concentrate by ammonium sulphate is proposed.IntroductionConsiderable reserves of zinc ores are present in Um Ghieg area eastern desert, Egypt. The possibility of extraction zinc from these ores and preparing its valuable compounds by choosing a more feasible technology become of vital importance. An attention is focused on the sulphatizing roasting processes (1-9) to achieve the appreciable formation of soluble sulphates. Previous publications are reported in our division by El. Tawil and others (10-16) using ammonium sulphate as sulphatizing agent for the successful treatment of nonferrous bearing materials.Therefore, the present work aims to study the different factors affecting the sulphatizing roasting process of local zinc coocentrate by anunonium sulphate to extract completely zinc and preparing its main compounds. Tue mechanism and kinetics of the different chemical reactloos that 1ake place in the process are considered."

Jan 1, 2000

By Hector Henao

To provide thermodynamic data for converting the nickel matte to liquid nickel, an experimental study was conducted in the phase equilibrium between the Ni-S alloy and the CaO-Al2O3 based slag melted in a MgO crucible at 1873 K under controlled Pso2 of 10.1 kPa and Po2 in a range between 2.5x 10-and 10.1 Pa by using CO-CO2-SO2 gas mixtures. The content of nickel in the slag at Po, of 10.1 Pa, above which solid NiO is expected to precipitate in the equilibrium state, was found to be 4, I mass% and the contents of sulfur and oxygen in the nickel melt were 0.4 and 02 mass%, respectively. ft was clarified that increase in the temperature reduces the solubility of nickel in the slag and the contents of sulfur and oxygen in the alloy, The distribution of minor elements such as gold, silver, copper, cobalt, iron, arsenic and antimony between the Ni-S alloy and the CaO-Al2O3 based slag was also studied. The distribution ratios of iron and cobalt, defined by (%X in slag)/[%X in alloy] where X is the minor element, are larger values than that of nickel, while those of copper, silver and antimony are similar to that of nickel. The distribution ratios of arsenic and gold are lower than that of nickel in the higher range of oxygen partial pressure.

Jan 1, 2003

By A. J. Davidson

A novel sensor is described for the measurement of the copper content of copper matte. Due to the high copper concentrations found in matte, potentiometric sensors are not sufficiently sensitive. A highly sensitive sensor has been developed based on a modification of the amperometric technique using a copper ion conductor, Cusicon. The results correlate closely with the theoretical predictions.

Jan 1, 1998