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By W. W. Albrecht

I. Introduction Refractory metals like tungsten, molybdenum, rhenium, tantalum and niobium and their compounds are essential ingredients of our modern technology. Especially in purified form, they are used in special alloys, electronics, optics and ceramics. The processing route from raw material to high purity refractory metals and their compounds includes, as a prime option, the following steps: - dissolution of raw materials. - liquid liquid extraction. - precipitation of high purity intermediate compounds. - calcination/reduction to high purity oxides/metals. Especially in the first three steps, major amounts of chemicals like acids or sodium hydroxide are used and, as by-products, substantial quantities of residues and effluents are generated. The impact of environmental regulations on these by-products and the attempt to reduce or minimize the amount of residues and effluents produced will be discussed in this presentation using Ta/Nb chemistry as the example. The basis of our considerations will be the way these by-products are handled at HCST, a major, and in some cases, the biggest producer of refractory metals (tungsten, molybdenum, rhenium, tantalum, and niobium).

Jan 1, 1992

By Robert W. Bartlett

Chalcopyrite in copper flotation concentrates can be hydrothermally converted to digenite with oxygen in a continuous process, with rapid kinetics when operated above 200°C. This eliminates large amounts of sulfur and iron. These "super-concentrates" have potential for debottlenecking smelters and avoiding capital intensive future smelter expansions, otherwise required in the late 1990s. The technology of producing super- concentrates is described, with cost estimates, and the use of super-concentrates as smelter feed is discussed, with examples.

Jan 1, 1992

By Renato G. Bautista

The prospect for recovery of rare earths from red mud, the bauxite tailings from the production of alumina is examined. The Jamaican red mud by far has the higher trace concentrations of lanthanum, cerium, neodymium, and yttrium. Scandium is also present. The dissolution of the rare earths is a major extraction problem because of the large volume of other materials present. The recovery processes that have been proposed include the production of co-products such as iron, alumina, and titania concentrates, with the rare earths going with the titania A critical examination of the possible chemical processes for the complete utilization of the red mud are presented Recommendations for research projects considered to be important in the development of a chemical separation process where no pig iron product is contemplated are also discussed.

Jan 1, 1992

By Donald R. Sadoway

The viability of treating certain forms of hazardous waste by direct electrolysis in molten oxides is under investigation. Secondary residue or waste mud produced in the course of chromate chemical production is the focus of attention in this study. The goal is to reduce the water soluble hexavalent chromium either to insoluble trivalent chromium or to chromium metal. Electrolysis tests have been conducted in a high temperature cell containing chromate sludge dissolved in an electrolyte composed of Al2O3, SiO2, CaO, and MgO. Oxygen production on a carbon-free anode has been confirmed.

Jan 1, 1992

By Stephen J. Hales

State-of-the-art Resistance Spot Welding (RSW) equipment has the potential to permit adaptive feedback through recent advances in computerized process control. The initial step toward achieving this goal involves assessment of the effect of specific variables and the interaction between these process inputs on spot weld characteristics. This investigation addresses this issue through the application of Taguchi methodology to understand and refine a RSW schedule developed for joining of two dissimilar aluminum-lithium (AI-Li) alloys of different nominal thickness. The experiment was designed to establish a hierarchy of inputs with respect to each 'other, and to determine the significance of these inputs with respect to experimental noise. Valuable insight was gained regarding the interaction between process variables and the effect of certain equipment-related changes. In spite of a decrease in equipment performance, an improvement in the maximum strength attainable for defect-free spot welds resulted from the application of the statistical experiment.

Jan 1, 1992

By M. Zamalloa

Slag foaming is an important phenomenon in many metallurgical processes. It creates large surface areas for multi-phase reactions to take place. In other applications, it protects electrodes and improves the energy efficiency by reducing radiation from hot surfaces. However, it may also be a source of serious disturbances. To control and optimize the use of slag foams, an extensive knowledge of the factors controlling the foam formation and stability is required. Slag foaming experiments were carried out using synthetic FeO-CaO-Si02 slags at temperatures ranging from 1200 to 1350 "C. A data acquisition system was used to continuously measure the foam height, gas flow rate, bubble frequency and temperature. The experimental results show that the gas injection rate has a strong effect on the behaviour of slag foams. At high flow rates and rapid bubbling, unstable foams with short decay times were created. The addition of P20, favours the foam formation and stability by lowering the surface tension of the slag. The average foam life increases with decreasing basicity (CaO/Si02). It is proposed that this is attributed to the increase of the surface viscosity due to surface adsorption of a thin film of silica, retarding the drainage of the liquid films.

Jan 1, 1992

By Husamuddin Ahmadzai

A survey of regulations and state of the art control technologies is presented relating to the smelting of primary aluminium, copper and recycling of residues. Some costs associated with the alternatives and trends for the coming decade in this. sector are identified.

Jan 1, 1992

By Barry T. Kilbourn

A dominant characteristic of many derivatives of the lanthanides is stability at high- temperatures. Combine this with novel solid-state behavior under those conditions and there is the potential for new materials that can not only improve existing applications but also help create new technologies. These property themes will be traced through new uses ranging from efficient energy generation and raw material conversion to control of environmental emissions and temperature measurement. Conducting ceramics, methane conversion catalysts, sulfur oxide capture agents and phosphor hosts will be described. Some categories will account in the future for significant lanthanide consumption whereas others will remain commercially negligible but technologically vital. All uses will illustrate the versatility of those elements inappropriately termed rare.

Jan 1, 1992

By Guilian Gao

TbFeCo is a common choice for many rare-earth transition metal films currently used as the magneto-optic layer for magneto-optical: recording devices. Since the environmental stability of RE-TM alloys is typically poor compared with traditional metal oxide particle media, such devices rely on multiple functional overlayers (metallic and/or dielectric) and organic coatings for durability. This paper presents an electrochemical evaluation of the degree of protection of several candidates for the reflective layer, Al, AlCr and AIPt and for the dielectric layer, SiN, AISIN and AIN. Cyclic voltammetry In 0.2M K2SO4 solutions at room temperature revealed that AIPt film offers superior corrosion protection compared to Al and AICr films. Of the three dielectric layers examined, SIN seems to be the most corrosion resistant. Examination by optical and scanning electron microscope confirm the findings of electrochemical experiments. The corrosion resistance of single layers of Al, AICr and AIPt has also been examined and factors affecting their performance are discussed.

Jan 1, 1992

By Michael P. Meisel

Solinox is a physical scrubbing process capable of removing a number of noxious materials from off-gasses, especially SO2, hydrocarbons, halo¬gens, heavy metals such as dust, etc. As these materials are dissolved physically, (not chemically bound), the solvent is absolutely stable and no by-products are formed in the scrubbing cycle. The process has been installed in three plants up to now, treating from approximately 30 MMSCFD to approximately 100 MMSCFD. These installations are in a non ferrous metal smelting operation, in a cellulose factory, and in a roasting process.

Jan 1, 1992

By P. D. Ferro

The direct oxide reduction (DOR) of plutonium oxide generates significant amounts of contaminated waste. This waste primarily consists of calcium oxide-saturated calcium chloride salt. This investigation explores the possibility of recycling the salt, by the electroreduction of the calcium oxide. Fused salt electrolysis of a simulated salt mix (CaC12 + ~10 wt. pct. CaO) is being carried out to electrowin calcium, and the process is being optimized in terms of the calcium solubility, cell temperature, current density and cell design to maximize the current efficiency. This work identifies the major concerns in the development of a process to electrowin calcium from this simulated salt mix.

Jan 1, 1992

By Jae-Chun Lee

Di-2-ethylhexyl phosphoric acid (D2EHPA) is widely used for separating rare-earth elements. In commercial plants, rare-earths are usually stripped from loaded extractant streams using mineral acid, then precipitated as oxalates. Many rare-earth uses demand specific powder characteristics, which are obtained by secondary processing. This paper demonstrates the feasibility of combining the stripping, precipitation and powder processing stages, thereby achieving considerable savings. MEHPA solutions were loaded with yttrium, then emulsified with oxalic acid-HC1 solutions to precipitate yttrium oxalate, which was readily calcined to yttrium oxide. The precipitation kinetics and yield were sensitive to process conditions. The morphology and size of the yttrium oxalate powders varied with the concentrations of D2EHPA and oxalic acid, and the presence of SPAN 60, which affected nucleation, growth, and the emulsion characteristics.

Jan 1, 1992

By Musa Karakus

Zirconia-based refractorics arc finding increasing use for specialized applications in steelmaking technology, making optimization of their resistance to corrosion by steelmaking slags more important. Samples of calcia- and magnesia-stabilized zirconia refractories have been exposed to slags in the CaO - FeO - SiO, system at 155WC for the purposes of measuring corrosion rates. Examination by SEM/EDX and cathodoluminescence of the mineralogy of the attacked specimens reveals important clues about the mechanism of attack.

Jan 1, 1992

By C. J. Lewis

This presentation concerns calcium oxide-better known as high calcium quick lime High calcium quicklime is produced by calcining high calcium limestone, mostly in the many rotary kilns located throughout the United States and Canada. This paper presents suggestions on the handling of lime based on field experience. The subjects covered are chemical analyses, transporta¬tion, lime storage, lime slaking to form a water slurry of calcium hydroxide solids, slurry transportation, slurry viscosity, and scaling of lime slurries. It is hoped that the comments on the foregoing areas will be of use to those designing or operating lime systems.

Jan 1, 1992

By Philip E. J. Green

Two of the cornerstones of total quality management, the use of statistical and problem solving tools, and the involvement of employees, are directly applicable to environmental protection. The reduction in variation decreases the chances of violations and mishaps. Involving employees in minimizing environmental impacts is critical. One mistake, even with the best technology, and your plant can be shut down, customers lost and fines and penalties imposed - your reputation and the environment damaged. Proven strategies for involving employees in environmental protection, and over-coming the frequently strong differences of opinions about what constitutes environmental protection, will be discussed.

Jan 1, 1992

By Fernando Castro

Electric furnace steelmaking dust is a polluting residue that needs to be treated in order to recover metals contained and to produce an environmentally acceptable residue. Some hydrometallurgical approaches for its treatment have been evaluated, namely: caustic soda leaching followed by electrolytic recovery of zinc, ammonia leaching followed by zinc compounds precipitation and acetic acid leaching followed by lead, zinc hydroxide and gypsum precipitation.

Jan 1, 1992

By B. J. Beaudry

The preparation of alloys containing one to two percent of the volatile lanthanide metals Sm, Eu, Tm and Yb in the high melting point (HMP) rare earth metals Sc, Y and Lu was accomplished by a vapor deposition, diffusion method without crucible contamination. The method avoids the melting of the HMP metals which would introduce impurities from the crucible, generally Ta or W. Plates of the HMP metals were hung from the lid in the upper part of the Ta crucible. The volatile metals were placed on the bottom and the lid welded in place under an atmosphere of helium. By proper selection of thee alloying temperature, the effusion of the metal vapors, through the helium atmosphere was slow enough to permit diffusion to occur and prevent refluxing of the newly formed alloy. Very volatile metals such as Mg required a Knudsen cell with a suitably sized hole to prevent too rapid transfer of the low melting metal. Electron microprobe analysis of a cross-section of the HMP metals showed a homogeneous distribution of the volatile metals. The time and temperature required to obtain a homogeneous rare earth alloy without contamination are given. The use of a Knudsen cell to form magnesium-rare earth alloys is reviewed.

Jan 1, 1992

By J. S. Kirkaldy

A theoretical procedure is demonstrated for calculating two-dimensional binary cellular single-valued interfaces and extended to triple-valued (remelt) shapes. The numerical calculations for the single-valued local equilibrium problem which yield unique shapes as functions of the supersaturation parameter a and the partition coefficient k are reviewed. The cell amplitude L and wavelength A scale identically as the inverse velocity to the 112 power and the aspect ratio r is a constant equal to 312, independently of a and k for a < 0.5.. For 0.5 < a < m, L, A and r decrease asymptotically to zero indicating the finite amplitude nature of the instability at a = 1 and the existence of sub-marginal states which converge to a flat interface at a- m (Glv- m). Scaling comparisons between equilibrium single-valued and triple-valued and deep-rooted non- equilibrium cells are made.

Jan 1, 1992

By J. Boitano

This paper discusses the study, design and implementation of the new gas handling system for the Caletones Smelter of Cbdelco..Chile. A discussion on design conditions for a Mure Sulphuric Acid Plant using Teniente Converter.gases.is also included. The old system which started to be modified in 1985 and relied on natural draft and used balloon flues, resulted in a limited .gas handling capacity for operation under Mure process conditions. This system also caused excessive fugitive gases in the smelter working areas. The new system permits handling of process gases from the higher capacity Teniente converters installed in 1987-1989 Improving the gas handling of the reverberatory furnaces and Peirce-Smith converters as well as the environmental conditions of the smelter. This system utilises improved converter gas hoods, evaporative cooling and electrostatic precipitators gas cleaning, and is based on natural draft.

Jan 1, 1992

By Uday B. Pal

In the electrochemical vapor deposition (EVD) process, gaseous cation precursors are passed over one side of a porous substrate, and oxygen is passed on the other side of the substrate. The gases diffuse and react within the porous substrate, and the pores get filled with the desired solid oxide. Subsequent solid state electrochemical transport through the solid oxide in the pores continues the reaction, and the film grows over the porous substrate. The EVD process has been used to deposit lanthanum chromite interconnection films and yttria stabilized zirconia electrolyte films over porous air electrodes. The EVD growth of these solid oxide films is found to be parabolic in nature, which indicates that the solid state transport (diffusion) of ions through the film controls the growth. This solid state transport can be analyzed using Wagner&apos;s treatment of the electrochemical transport. Conductivity measurements and the information on the defect structure of the oxide can be combined with the EVD growth rate measurements to calculate the solid state transport properties (transport numbers and partial conductivities) of the rate-controlling minority species in the oxide. Using this approach, the EVD growth of other electronic, mixed conducting and ionic solid oxide films can also be analyzed.

Jan 1, 1992