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By Serdar Aksu, Fiona M. Doyle

"CMP will be an essential process in the production of integrated circuits containing copper interconnects. This study aims to improve our mechanistic understanding of the role that organic chelating agents might play in the reactive slurries used in copper CMP. Copper dissolution behavior in EDTA arid glycine was first examined by producing potential-pH diagrams for the copper-water-EDTA and copper-water-glycine 'systems. The results of potentiodynamic polarization experiments were then considered in light of these diagrams. . In-situ polarization experiments were conducted to gain insight into the electrochemistry of copper during dynamic polishing in slurries prepared from EDT A and glycine.IntroductionCopper has recently started to replace aluminum as the interconnect metal in integrated circuits. Copper interconnection offers faster and more reliable integrated circuits due to its higher electrical conductivity and superior electromigration resistance (1). The damascene method is used to form multilevel interconnects in the manufacture of integrated circuit devices with copper metallization (2, 3). Copper is deposited by CVD or electroplating into vias and trenches etched in the interlayer dielectric (IDL), over a diffusion barrier usually made from titanium, tantalum or their nitrides. Chemical mechanical planarization (CMP) then prepares the wafer for the next deposition step, by removing excess copper and planarizing the surface. During CMP, the wafer is rotated and pressed against a rotating platen covered with a polishing pad. Chemically active slurries containing submicron size abrasive particles (Si02, Al20 3, ceria, diamond, etc.) are applied. Both the mechanical action of the abrasive particles and the chemical action of slurry constituents remove material from the wafer surface. Planarization results because material is removed faster from protruding regions on the surface than from recessed regions. Since CMP can globally planarize .the entire wafer, it has become one of the key technologies for producing integrated circuits with copper metallization."

Jan 1, 2000

By Batric Pesic

A hydrometallurgical process for recovery of Zn and Mn from Bunker Hill Water Treatment Plant sludge was developed. The process is unique because it treats an unusual combination of metals, Zn and Mn. Another non-standard feature of the process is that leaching takes place with ~S04 in the presence of a reductant (SO2). Zn and Mn are recovered simultaneously by electrowinning, Zn on a cathode and Mn on an anode, as MnO2 The major purpose of the process is to detoxify the sludge by removing toxic heavy metals. The recovered metal values could be marketed to offset the overall costs of water and sludge processing. This work is presented in two separate parts, 1. Leaching and Solution Purification, and II. Electrowinning. This paper covers only the first part of the hydrometallurgical process: Leaching and Solution Purification. Initially, the paper briefly discusses the history of the pollution problem at the Bunker Hill Superfund Site, the origin of heavy metals in the mine waters, and the development and use of the water treatment plant. The leaching of sludge was examined as a function of the following parameters: constant vs. initial pH, initial vs. delayed addition of SO2, temperature, and pulp density. It was found that leaching with H2SO4 at pH 2.0 for 15 minutes (at 60°C), followed by S02 addition for another 15 minutes, could completely dissolve Zn and Mn. Solution purifIcation was done in three stages. In the first stage iron was removed by adjustment of pH (to pH 5.0) and oxidation offerrous to ferric iron (with H2O2). In the second stage, Cu and Cd were removed by Zn dust cementation. Finally, Co and Ni were precipitated with the organic reagents 1-2 nitroso-naphthol and nitroso, respectively. Electrowinning of Zn and Mn is discussed separately in Part II of this paper.

Jan 1, 1996

By L. M. . Chia

The successful treatment of waste materials to recover metals with acceptable purity is often hampered by the presence of undesirable impurities. The problem is further complicated by the need to insure that any residues or solutions generated are environmentally acceptable. Hydrometallurgical processes involving leaching- solvent extraction-electrowinning offer some attractive features which address many of these problems. However, in certain instances trace impurities that contaminate the organics are difficult to chemically strip and interfere with the overall process efficiency. A new processing scheme has been developed which appears to provide some attractive alternatives for impurity removal from organics. It has been shown that many ionic impurities can be electrochemically removed from the organic by spontaneous direct reduction using solid metals. A variety of metal ion impurities have been removed from selected common organic extractants such as D2EHPA and TBP using different metals as the reducing agents. The results and probable mechanisms involved in the reactions are discussed.

Jan 1, 1994

By E. Kuzeci, R. Kammel

"Lately various voltametric methods have gained increased attention as an analytic tool in hydrometallurgy. Voltammograms with mercury drop electrodes or glassy carbon electrodes provide information about the electrocrystallization of cathodic deposits and allow calculation of kinetic data by means of characteristic parameters like the peak potential and peak current and their variation with the voltage scanning rate.Cyclic voltammograms are also suitable for identification of reaction sequences. Voltammograms with carbon paste electroactive electrodes containing metal sulphide additions reveal information about the dissolution behavior. The stripping voltammetry can be applied to analyze metal ions and organic additives (e. g., thiourea) in extreme low concentration. Typical application of the various methods studied with microcomputer controlled measurement system are explained by examples selected from copper hydrometallurgy.IntroductionThe use of electroanalytical methods in metallurgical process control can be dated back to the starting period of industrial copper refining, when the deposition of the metal ions was followed electro-gravimetrically by weighing the electrode with deposits (1). The principles of metal deposition and dissolution have not changed but the methods to follow these phenomena were subjected to noticeable developments and especially the introduction of polarographic investigations by Heyrowsky (2) has greatly contributed to the progress in electro-analysis. A review about the fundamental work on the electrochemical kinetics in earlier time is compiled in a monograph of Vetter (2). With the steady improvements in the instrumental techniques, it is nowadays possible to apply several current and potential modulations for measurements with improved selectivity and sensibility. There is however, still a lack in theoretical interpretation of the data obtained. More theoretical information are already available for linear voltametric methods for systems where reduced as well as oxidized species are dissolved in the electrolyte (4, 5). Some recent investigations have also shown the reliability of these techniques to study electro-crystallization (6, 7). Main fields of the application in the hydro - and electro-metallurgy are:"

Jan 1, 1989

By K. S. Raja, M. Misra, S. K. Mohapatra

"Ordered arrays of TiO2 nanotubular photocatalysts were prepared by a simple anodization process. Band gap states of the TiO2 were altered by controlling the anodization electrolyte composition and thermal annealing conditions that resulted in enhanced photo activity. These nanotubes were used for reducing CO2 to methanol either by photochemical or photo electrochemical routes. Pd nano-particle loaded TiO2 nanotubes were employed for photochemical reduction of CO2 to methanol that showed a conversion rate of 12 x 10-3 mol m- 2h-1. Carbon modified TiO2-xCx type nanotubes were used as photo anode and Ti as cathode for photo electrochemical reduction of CO2. The potential of Ti cathode was maintained at -0.5 V SCE. The formation rate of methanol was determined as 13 x 10-3 mol.m-2h-1.1. IntroductionGlobal warming due to emission of carbon dioxide is a serious environmental concern. The atmospheric concentration of CO2 is about 384 ppm by volume and about 3 x 1012 tonnes by weight. Burning of fossil fuels and deforestation are the leading causes for increase in the anthropogenic CO2. More than 32 x 109 tonnes of CO2 are released per year (based on 2006 data) worldwide from the fossil fuel. Pumping CO2 from the fossil fuel power plants into deep ocean basin is one of the most discussed disposal options. The other potential option is converting this green house gas into valuable fuels.Carbon dioxide feed stock can be converted into fuels of solid, liquid or gas phase by chemical, electrolytic, photocatalytic and photo-electrocatalytic methods. Reduction of CO2 to fuel form of any phase requires energy. The reduction process should be energy efficient so that we do not spend more energy and emit more (indirect) CO2 in the process of converting CO2. From this point of view, conversion processes occurring at room temperature look attractive.Electrolytic conversion of CO2 into various forms such as methane1, ethane2, ethylene3, methanol4,5, ethanol6, n-propanol, formic acid7, and formaldehyde has been widely reported. The standard equilibrium potential (at pH: 0) for reduction of CO2 to methanol is 0.14 VSHE and to methane is 0.2 VSHE which is thermodynamically more favorable than hydrogen reduction. However, the gas phase reduction is kinetically complex requiring effective electrocatalyst. The major issues with electrolytic conversion of CO2 to useful products are:"

Jan 1, 2010

By Tam Tran

Most new gold mines in Australia are required to treat tailings to reduce cyanide levels before they are discharged to storage ponds to meet the stringent environmental management guidelines set by government statutory authorities. In New South Wales, the average level of weak acid dissociable cyanide allowed in open tailings dams is now limited to 20 ppm, As stringent environmental guidelines continue to be enforced in Australia as well as in other parts of the world, the management of cyanide wastes has emerged as a key issue for the gold mining industry. This paper provides a critical evaluation on technical aspects related to the use of ion exchange resins and affiliated processes in cyanide management and tailing treatment. Particular attention is given to the use of ion exchange resin technologies in the processing of mixed gold-copper ores, where cyanide usage is the highest. Information presented in this paper is heavily drawn from the experience on the application of ion exchange resin processes at May Day mine, in New South Wales, Australia and associated pilot plant test programs. Issues related to the management of thiocyanate, especially with respect to the recovery of cyanide from thiocyanate are also discussed.

Jan 1, 1998

By Manfred K. Walther

"Tests were conducted on instrumented plates cast in the Abex Experimental Foundry to compare recorded solidification histories with results computed for corresponding models simulated with the C.A.S.T. program. The first plate was cast of low alloy steel and the second of carbon steel with a graphite chill at one end. Both were cast in molds of bonded silica sand. Temperature histories were recorded in the castings, molds and chill. Exceptionally good agreement was achieved between computed and experimental data. Other investigators will find the results useful as a benchmark against which they can compare the results of their own calculations.IntroductionSince the early 1970's our foundry engineers have used both two- and three-dimensional versions of the G.A.S.T. program to gain knowledge of the solidification process [1,2,3]. Study of the computed data gave insight as to how the rigging and risering of specific castings might be changed or adjusted to improve quality and yield. New schemes based on such analyses were then recommended for implementation on the foundry floor. The degree of success of the new practice was subsequently evaluated after the part had been poured, shaken out and examined. Similar conditions were noted in the sectioned castings whenever porosity and voids had been predicted by the computations. Appropriate modifications, when found successful in the model, were applied to the process. This led to a reduction, if not complete elimination, of the defects. Such results gave credence to the use of these programs as an aid in the production of better castings.Earlier investigations on simple shapes revealed excellent correlation between output derived with the G.A.S.T. program and exact solutions. Results also compared favorably with data calculated using other codes as reported in the literature [4] and summarized in the Appendix. However, since the computer program had not been verified by direct experiment, it was decided to run instrumented tests to check the theoretical predictions with actual measurements."

Jan 1, 1986

By M. P. Bohrer

A closed-loop hydrometallurgical process has been developed for treatment of smelter flue dust generated by copper recycling. The process is a semi-continuous operation in which zinc, iron, and copper are first extracted from the dust with a sulfuric acid solution. The lead and precious metals, initially present in the dust, remain as solids and can be recycled to the copper smelting furnace. Cementation with iron and zinc metal purifies the zinc and iron-rich liquid stream prior to spray drying. The spray-dried product, consisting of a mixture of zinc sulfate monohydrate and iron sulfate monohydrate, is a desirable micronutrient additive for use in animal feeds. Treatment of the smelter flue dust in this manner will generate a positive return on investment, as well as mitigate a potential environmental liability.

Jan 1, 1992

By Kimio Ilagaki

The distribution ratios of Ag, Pb, As, Sb and Bi for the Cu2S-FeS or Ni3S2-FeS matte I FeOx-SiOl, FeOx-Si02-CaO or FeOx-CaO slag equilibration in a MgO crucible were determined experimentally at 1523 ~1573K under controlled partial pressures of S2 and 02 at given PS02 of 10.1,50.7 and 101.3 kPa(O.I, 0.5 and I atm), and the observed dependency of distribution ratio on the matte grade, S02 pressure and slag basicity were analyzed on the basis of thermodynamics.

Jan 1, 2003

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 Glenn C. Miller

Cyanide is the most common lixiviant for extraction of precious metals, and its efficient use in open pit mines has contributed to the increase in world production of gold during the previous two decades. With this expansion of precious metals mining using cyanide, public concerns have developed in response to the inherent public perception of cyanide as a tox-in as well as a series of environmental problems that are directly or indirectly related to cyanide use in open pit mining. Some of these have technical or regulatory solutions, while others will require additional investigation before they can be resolved. The following discussion will summarize some of the public concerns regarding the use of cyanide in precious metals mining. The issue of cyanide use in large scale precious mining is controversial, and recent banning of cyanide use in open pit mines in Montana, or complete banning of cyanide in Hungary has reflected those international concerns. The underlying basis for some of the bans (e.g. Montana) reflect a general concern of the environmental impacts of mining, rather than specific issues related to risk of cyanide use. The human safety record for cyanide use, particularly in the developed countries is good, and cyanide is clearly the most efficient lixiviant for precious metals. Indeed, the relatively short lifetime for cyanide in the environment renders it one of the less problematic chemicals used for extraction of gold from ore. Mercury amalgamation or use of bromide as a lixiviant are certainly much more problematic. What, then, is the basis f~r the international concern about precious metals mines that use cyanide. Ifuse of cyanide for gold recovery is to continue, what additional infom1ation needs to be developed that will allow a better management of the risks of cyanide? Which of the concerns are directly related to cyanide, and which are indirect concerns that more related to effects of open pit mining. Under what conditions should use of cyanide be discouraged? DUl::ing June of 2000 the United Nations Environmental Program conducted a two-day workshop on cyanide use in mining that was attended by persons from the mining industry, regulators and environmental community. Support and attendance at this workshop reflected concerns by all three groups on further restrictions for cyanide use and the emerging potential for guidelines for better management of the catastrophic release of cyanide-containing mining waste. The following discussion is meant to focus-on those risks and explore the basis for an often negative reaction to precious metals mining using cyanide. It is presented in the format of a statement, followed by a discussion. While admittedly provocative, the statements are meant to express the concerns? of the public regarding cyanide and the mining industry.

Jan 1, 1998

By Martin J. Hansel, Jan Bäckström

Starting from historic perspectives on converting at the Rönnskär Smelter, the continuous developments of refractory practice is described. In the development the joint efforts of operators and suppliers of refractory have lead to significant achievements. This paper comprises the development of the converting process and the refractory lining as well as future prospects regarding operation and refractory lining design, especially in the face of equipment and raw material availability. 81

Jan 1, 2009

By Jared Ball, Benjamin Hogg

There are over 100 process parameters that can be monitored during a single Peirce-Smith (PS) converter batch operation. To support a consistent operation it is important to select the correct Key Performance Indicators (KPI’s) to monitor. They should be strategically chosen to drive the desired behaviour with enough flexibility to endure process variations. At the Xstrata Copper Smelter in Mount Isa most of the PS converter operators have very little experience and are often lacking in the appropriate education or training to properly understand the process. For this reason 10 simple KPI’s were chosen that could be easily comprehended and monitored by all smelter personnel. KPI compliance has been supported by relevant project work in the converter area. Charge sequence trials have been performed in an effort to reduce splash and optimise activity time. The online measurement of full and empty ladle weights has enabled an immediate indication of skull size, skim/slag carryover, and metal loss.

Jan 1, 2009

By Elders. Wilfred A.

Petrological and geochemical methods, the utility of which has long been established in the mining industry, are proving useful and cost-effective in elucidating the thermal evolution of active geothermal fields. In return, they yield insights into sulfide-silicate equilibria, mass and energy transfer in convecting hydrothermal systems, and the genesis of hydrothermal ore bodies. Within the Plio-Pleistocene sediments of the delta of the Colorado River, in the Salton Trough, several active geothermal systems are known. Temperatures vary from 100-365°C, at less than 2 km depth, and salinities vary from 3,000 to 280,000 ppm, total dissolved solids. The hydrothermal alteration causes marked induration of the sediments, producing greenschist facies metamorphic minerals, including hydrothermal ore minerals. Subsurface authigenic minerals show strong correlation with increasing temperature. A typical sequence in sandstones is (below 150°=C) montmoril-lonite-kaolinite, (above 180°C) chlorite + illite, (above 225°C) calc-alumino-silicates, (above 325°C) biotite. There is a transition from porosity-dominated\to fracture-dominated permeability in the hottest and deepest geothermal reservoirs. This regular series of minerals provides a practical tool during exploration drilling. From drill cuttings, we can make predictions on reservoir temperatures, useful in making decisions on well completion. Other types of geothermometry we have employed include light stable isotopes, fluid inclusions and vitrinite reflectance measurements. A combination of these techniques not only improves our temperature predictions, but together with fission tack annealing studies, permits us to model the dynamics of temperature change and fluid flow in these geothermal reservoirs.

Jan 1, 1981

By M. F. El-Demerdash

The activity distribution diagrams for different species in aqueous systems are developed. Computational method may be considered as an extension of the Activity-Term method introduced by the authors to construct EH-pH diagrams. In the Activity-Term method, all activities of different species are evaluated before deciding the most stable one. In the present study, a factor is assumed to allow for the conservation of the element. At any point, the total concentration of all species should contain only the input m moles of the element (elements) considered. This approach is applied to Zn-, 5-, and Zn-S-H2O and activity distribution diagrams are plotted as a function of pH, at different potential levels and at different temperatures.

Jan 1, 1990

By Magnus Ek, Peter Olsson

The Rönnskär Smelter has been faithful to Peirce Smith Converting during its 79 years of existence. Though a visitor to our smelter museum will easily find out that a lot has happened since the beginning – and development continues. In this paper an up-date on Converting and Casting at the Rönnskär Smelter is presented. Recent developments include an investment into converter process gas handling, but also day-to-day operational aspects such as converter aisle productivity and flexibility, but also minimal EH&S impact. 127

Jan 1, 2009

By M. J. Adam

As part of its research programs, the Bureau of Mines is investigating the partitioning of complex sulfide minerals to simpler sulfide phases by sulfidation reactions. Partitioning in this manner can afford opportunity to improve selective extraction of mineral constituents of value. This report describes research involving the sulfidation partitioning of the mineral pentlandite, which is an important source of Ni in primary production. For the laboratory studies, the pentlandite was synthesized in nominally equiatomic proportions of Ni and Fe. Elemental Ni, Fe, and S powders were blended, compacted, and sealed under reduced He pressure in vitreous silica tubes. The tubes were heated under controlled conditions at SOD? C for 24 h. The product was verified by X-ray diffraction and chemical analysis to consist essentially of (Ni,Fe)9S8. Small samples of the (Ni,Fe) S were encapsulated with sulfur in silica tubes at reduced He pressures and heated for 1 to 24 h at specific temperatures between 400? and 600? C, both below and above the boiling point of sulfur (_445° Cl. Reaction rate increased with temperature. Within this temperature range, partitioning to individual Ni and Fe disu1fides proceeded to essential completion according to the reaction

Jan 1, 1988

By Robert E. (Bob) Brown

Magnesium was discovered by Davy in 1808. The production processes as they exist are not economically competitive with aluminum The electrolytic magnesium process is divided into two steps; one to make the MgCh feed and the other to apply large amounts of electric current to dissociate the feed into magnesium (450 g) and chlorine (1200 g). The production of fuJIy anhydrous, pure cell feed is a major problem Recently, there has been a growth of thermal processes, mainly the Pidgeon silicothermic production process using FeSi to reduce dolomite in horizontal retorts. Pechiney has a large vertical electrical furnace process that also uses FeSi to reduce calcined dolomite in a molten bath containing alumina. Work is proceeding to develop new or modified processes that will greatly improve magnesium production. The present methods and the research and R&D will be reviewed in this paper.

Jan 1, 2001

By Katerina Kryst

Antimony and bismuth are two of the elements that need to be removed from copper electrolyte to ensure a trouble free operation as well as to maintain copper cathode purity. One method to control these impurities is the use of aminophosphonic ion exchange resins. Antimony is present as both Sb(III) and Sb (V). Sb(V) is very difficult to remove from these resins, requiring excess amounts of highly concentrated hydrochloric acid. In industry this affinity of Sb(V) for the resin causes a buildup of Sb(V) and degrading resin performance due to continual reduction of resin capacity. A new method for regeneration of aminophosphonic resins loaded with Sb(V) has been developed, which utilizes catalytic regeneration of the resin. Ion exchange can then be utilized for continual control of Sb and Bi in copper electrolyte.

By Anjan Kumari, B. K. Soni, Manis Kumar Jha, A. Vidyadhar, Vinod Kumar

"In the present paper, recovery of valuable metals from the poly-cracked ash obtained by pyrolysis of discarded PCBs has been studied following physical beneficiation and a hydrometallurgical process alternate to smelting. The ash is subjected to comminution for the separation of metallic components from non-metallic fractions by scrubbing, tabling and froth flotation which enriched the metal in the concentrate -97% which was further screened to separate high and low metal concentrate. The finer fraction containing -12% metallic value was leached in acidic solution. Almost all (Cu, Pb, Fe, etc) were leached in 4M HN03 at 90°C in 75 min at a pulp density 100 g/L. The characterization of both ash and residues were made by XRD, EPMA, EDS, etc. to validate the experimental results. The metals from the leach liquor could be recovered/separated using solvent extraction techniques which can further be processed to get pure metal salts/ sheets.IntroductionPrinted circuit boards (PCBs) are an essential component of electrical and electronic equipments (EEEs) as it plays an important role during operation of these devices. The world market of PCBs has reached nearly $60 billion in 2012, with 1.7 percent real growth over 2011 [1]. The diverse technology-driven global market is expected to grow at an average annual rate of 5% by 2014 [2]. The waste EEEs are generated due to replacement of obsolete equipments with modem ones and thus their demand is also increasing rapidly [3]. The discarded e-wastes are being piled up as landfills which affect the environment and cause health threats to living organisms, if not disposed of properly. These e-wastes contain metals some of which are precious, few are hazardous and others as valuable."

Jan 1, 2014