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By G. Diáz

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

Jan 1, 1995

By Ramana G. Reddy

Thermodynamic modeling and experimental study on impurity capacities and their distribution between mattes or metal and slags in smelting, converting and refining of non-ferrous metals was discussed. A brief review on the recent developments in copper smelting and converting is presented. The analysis showed that, copper smelting capacity increased by a factor of 10 since 60's, smelting rate increased by a factor of more than 5 and process fuel equivalent decreased by a factor of 2. A thermodynamic model for prediction of impurities capacities in slags and their distribution in mattes and slags was developed. The impurities capacities (i.e. sulfur and arsenic) of slags were calculated a priori with no adjustable parameters using the Reddy-Blander model. The capacities predictions were made in a wide range of matte and slag compositions, PSo, and temperatures in conditions pertaining to copper and lead industrial slags. The calculated results for sulfide and arsenate capacities are in good agreement with the available experimental and industrial copper and lead industrial slags data. The sulfide and arsenate capacities in copper slags (fayalite, ferrite and olivine) and lead slags are reviewed. The application of RB model predicted ratios of O2 and S2 partial pressures in industrial copper smelting processes are discussed. Application of this model for the prediction of Sb, Bi and other impurity capacities and their distribution ratios in mattes or metal and slags, in industrial smelting and refining processes is discussed.

Jan 1, 2003

By I. Gaballah

Jarosite contains up to 15 % of heavy metal compounds 'HMC'. The current waste disposal methods will not be allowed in the near future due to new environmental regulations and pollution risks. For these reasons, thermal treatments of raw or decomposed jarosite, in controlled atmospheres, were investigated. The aim of these treatments is to decontaminate the jarosite and/ or to recover the HMC for recycling. According to physico-chemical characteristics of the samples, the thermal treatments in controlled atmospheres N2, CO+N2 and C12+air lead to the extraction rate that vary from 93 to 98 %. Heavy metal compounds were separated by cooling the gaseous phase. The treatments' residue was almost free from HMC. Between 700 "C and 800 "C, the chlorinating treatment was successful of eliminating more than 97 % of HMC contained in four different samples.

Jan 1, 1999

By D. Donald Downey

Pilot Testing Ion Exchange Resin (IEX) can go from very simple beaker testing to complicated column testing. Space velocities, regenerant quantities, loading capacities, ion leakage, are all terms that get accumulated together to prove or disprove a resin’s (or resins’) ability to load a single ion (or specific set of ions). Not getting all the resin’s operating parameters correct will disqualify (or at least skew) the results. Laboratory tests for capacity, moisture content, bead size, metals fouling, etc.—what does it all mean? At last count, there were over twenty-five separate ion exchange resin tests (analyses) that were available to end users. Standard testing procedures identify the resin properties but more specific procedures can be used to identify problems with equipment operation. Then, there are the costs to consider; simple cation resin testing (moisture content, total capacity and bead integrity) is in the $200/sample range. However, add to this Chatillon, Russian Ball Mill Test, HIAC particle size, metals and % regeneration test procedures and the lab work can increase to over $1000/sample. In this paper, the author will explain the “must-do” pilot and test procedures and why they are important and the key to understanding how resin performs ion exchange.

By A. E. M. Warner

Inco Limited has long and extensive experience in converting nickel-copper primary smelting mattes over a broad range of nickel/copper weight ratios and combined nickel-copper-cobalt contents. At the Copper Cliff Smelter, the composition of the converter product matte has to meet the requirements of the matte separation process; at the Thompson Smelter, converter matte of a different composition is cast into anodes for nickel electrorefining; and in Soroako, Indonesia, a very low copper product matte is granulated for the Japanese market. Recently, Inco has conducted pilot plant testing of three possible nickel-copper matte continuous converting routes, namely flash converting, oxygen top blowing-nitrogen bottom stirring, and tuyere blowing. This test work has generated substantial new information on nickel-copper matte converting chemistry. This overview paper reviews the metallurgy of nickel-copper matte converting, in particular the behaviour of cobalt and the operating conditions required to meet the iron and sulfur specifications of the product matte. The relevant thermodynamic information is used to discuss the industrial data.

Jan 1, 2003

By Yu Hu, Gabriella Tranell, Song Zhang, Eivind Johannes Øvrelid

"In the present research, recycling feedstock of silicon for Photovoltic (PV) application is investigated. Whether these recycling feedstocks are reliable in the future use is discussed in this work to assess the properties of the crystal silicon ingot, which is commercially pulled from top-cuts of casted multicrystalline ingot via one kind of Czochralski method - FerroTech. Dopant is the acceptor type Boron (B) and growth direction was <100>. Crystal diameter and the length were 190mm and about 1700mm, which were controlled by the temperature and the pulling speed, then cut to 156mm * 156mm wafers with 2000um and 200um thickness. Resistivity measurements of these wafers by Four Point Probe (FPP) are in good agreement to the calibrated profile after Rapid Thermal Process (RTP). In this work, the Minority Carrier Lifetime MCI, shown by Carrier Density Image (CDI) and Quasi Steady State Photo Conductance (QSSPC), gives the mapping results on the cross section and the relationship to the injection level, increases in an arrange from 40us to 90us along the ingot height, which is abnormal distribution compared to the standard ingot. Then Oxygen and other metal impurities distributions, measured by Flourier Transform Infra - Red (FTIR) respectively, account for the novel phenomenon of the continuously increased MCI. Various types of heat treatments were performed on these wafers (different ingot and different positions) in N 2 and 0 2 mixture atmosphere. Before and after heat treatment, micro-defects were revealed by copper decoration and etching work. Solar cells are fabricated by Energy Research Center of the Netherlands from the experimental ingot, and processed under an industrial standard line. Compared to results of the reference mono-crystalline and multi-crystalline silicon solar cells, the performances of experimental ones show excellent efficiency values up to 18.5%, and Jsc values up to 37mA/cm2.IntroductionThe PV industry has gone through rapid development, with a high growth rate resulting in an increasing demand for silicon feedstock. In addition, costs in production need to be reduced such that solar energy can compete other conventional and renewable energy. Searching low cost, reliable and efficient feedstock is one promoting way to improve and enhance the competitiveness of the PVindustry.More and more researchers start searching new raw materials for PV application [1]-[4]. The key to make full use of low cost raw materials is to control the distribution and effect of impurities, such as Carbon, Nitrogen, and other metal contamination [5]."

Jan 1, 2013

By Rainer Schmid-Fetzer

"Isothermal solidification can be used to form strong bonds at low temperature which remain solid at much higher temperatures. The exploitation of this principally known technique for new high temperature processing steps and applications in electronic assemblies is the aim of this study. Three basically different variants of this bonding process are given. A comprehensive metallurgical screening is performed and the feasibility of binary material systems is given on a quantitative scale. Very attractive systems are spotted that have never been studied before. Detailed examples for the realization of bonding with complex ternary and multilayer systems are given. A highly innovative example is the chip stack or wafer to wafer bonding of unmetallized Si or SiC at 250°C. The proposed bond remains stable above the melting point of Si and enables entirely new semiconductor manufacturing steps. An improved die bonding process was proposed and verified experimentally.1. IntroductionIsothermal solidification can be applied to form strong bonds at relatively low temperature which remain solid at higher temperatures. The general principle of this type of joining processes is illustrated in Fig. 1. An interlayer of a low melting component, Lo, is provided as a foil or a thin film coating between the high melting joint components, Hi. The assembly is heated under moderate pressure to the bonding temperature, T 8 , and a liquid filler forms, either because the melting point of Lo is exceeded or due to a eutectic reaction between Lo and Hi. This molten filler initiates a rapid interdiffusion or reaction diffusion between Lo and Hi and the subsequent approach to an equilibrium state results in isothermal solidification. The solid phases formed at T 8 in the joint region exhibit a remelt temperature above T8 •"

Jan 1, 1996

By Eddie C. Chou

Phelps Dodge, Inc. (PD) is currently developing a lateritic nicke/Vcobalt deposit in Madagascar. Hazen Research, Inc. provides technical assistance to PD to investigate recovery processes for nickel and cobalt. Various process options were evaluated in laboratory experiments and pilot plant operations. The process selected for the feasibility study consists of feed preparation, high-pressure acid leach, countercurrent decantation wash, sulfide precipitation, sulfide dissolution, solvent extraction, ion exchange, and electrowinning. Among these unit processes, high-pressure acid leach, sulfide precipitation, and sulfide dissolution are applications of pressure technologies. Process development work and design criteria for commercial operations of these unit processes are presented in this paper. Concerns related to scaling in the high-pressure acid leach and the sulfide precipitation processes are discussed. Corrosion of various metal coupons under these environments was examined.

Jan 1, 2000

By R J. Singh, E. Z. Chacko, Devilal, S. K. Jha, Rina Sahu, Sheshank Shekhar

"Breakouts are one of the biggest problems encountered during continuous casting of steel billets. Billets get cracked locally or break completely in two parts during solidification causing the liquid part of the partially solidified billet to empty inside the cooling chamber. Proper control of important parameters is necessary to avoid break outs during continuous casting. In the present work, the nature of the break outs at a billet caster at Tata Steel was studied. Data analysis was also done for certain casting parameters and the Sulphur tracer test was conducted to understand solidification in the mould. It was found that to reduce the occurrence of break outs, it was necessary to tune the operations based on the grade being cast and the design of the mould tube being used.IntroductionA break out during the continuous casting process is a rupture of the partially solidified shell inside the secondary cooling chamber, causing the contained liquid steel to spill out. In the mid 1970s while continuous casting technology was still in early stage of development, causes of breakouts was not well understood. Today, with technological development much has been understood about breakouts but, most of the understanding has been in the slab casting process wherein due to the higher level of instrumentation, a lot of information has been gained. In billet casting however, due to the geometry of the mould housing with the tube mould, multiplied by the complexity of the multiple strands, instrumentation has not been used and obtaining data for analysis has been difficult.Breakouts at billet casters are still the main hindrances to production. A break out results in a loss in production since the strand which has had a break out is now not available to produce and thus a six strand caster would be reduced to a five strand caster, increasing the time for casting the same tonnage. Additionally extra set up time is required as more often than not a mould change is required in order to have the strand casting again."

Jan 1, 2014

By Versiane Albis Leão

This work aims at the selection of an appropriate eluant for cyanide recycling using ion exchange resins. Based on a literature review as well as on experimental results, the elution of resins loaded with copper and minor amounts of iron and nickel is discussed. The resins Imac HP 555s, Amberlite IRA 900 (Rohm&Hass) and Purolite A860S (Purolite Co) were eluted using either NaCI, zinc and nickel cyanides, hydrochloric acid, sulfuric acid or acid thiourea solutions. The results indicate that saline solutions are effective only with polyacrylic resins (Purolite A860S), failing to desorb the metals, specially the nickel cyanocomplex, loaded on polystyrene-based resins. Cyanide solutions of both zinc and nickel are capable of eluting over 90% of the loaded metals. In contact with pure acid&apos; solutions, iron precipitates onto the resin beads, as Cu(II) ferrous cyanideCu2Fe(CN)6.xH20. Thiourea is able to elute all the three metal cyanocomplexes owing to the increased solubility of copper cyanocomplexes in the presence of this complexing agent. The results demonstrate that a universal eluant is not available and the selection of the most appropriate resin-elution procedure should be based on the specific features of the system under consideration

Jan 1, 1998

By René Winand

A new process was studied at large laboratory scale at Université Libre de Bruxelles, under contract with Metallurgie Hoboken-Overpelt. A two cathodes (1m long ; 0.2 m high) channel cell was used at 2000 A/m2, with an electrolyte flow rate up to 1.8 m/sec. The main results may be summarized as follows : cathodes are electro¬refined grade in analysis ; metallographic structure and surface roughness are kept under control up to 1.3 cm (one side deposits) ; silver in cathode is controlled by CI and Br ions in solution ; organics must be used at very low concentrations (in the range of 0.1 mg/1, with a consumption of about 0.01 mg/lh).

Jan 1, 1987

By J. C. Yannopoulos

The quest for a continuous copper smelting and converting process, which has been going on for a long time, has not as yet reached its objective. The most recent efforts for the development of a continuous copper?making process started about two decades ago. Among the contending proposed processes, four have been piloted and three of them are currently in operation: the WORCRA process., the NORANDA process, the MITSUBISHI process, the OUTOKUMPU process. The WORCRA process, after some long pilot plant tests, failed to develop as an industrial process: The NORANDA process, as currently operating, is a smelting process and not a continuous copper?making reactor as initially conceived. The MITSUBISHI, although the only continuous process, has not been widely accepted. The OUTOKUMPU process can be applied only to a low iron concentrate feed and co?produces blister and high in copper slag. The thermodynamics of these "continuous" systems and the practical problems of their industrial application are reviewed and discussed. The achievement of efficient and inexpensive environmental control should&apos; be the primary objective of any new process development. A review of the environmental problems of the copper industry indicates that the quest for a continuous smelting and converting furnace should be intensified.

Jan 1, 1983

By E. Dendy Sloan

An overview of hydrate properties is given, with emphasis on unusual deviations from ice, the most common solid water form. Reliable sample preparation and reproduction of in situ hydrates provide the foundation for all hydrate science and engineering. Relations are given to connect the three domains in the title: (1) micro-scopic properties measured with Raman, NMR, and diffraction spectroscopy, (2) meso-scopic properties measured with single crystals, and (3) macro-scopic properties measured with pressures, temperatures, volumes, etc. A principal illustration relates micro-scopic and macro-scopic domains. Experiments provides the basis for improving statistical thermodynamics model for these compounds. To date, this model is one of the most commonly used industrial statistical thermodynamics applications, based upon the classical model of van der Waals and Platteeuw (1959). Microscopic measurements and simulations indicate model assumption improvements, resulting in the next generation of the statistical thermodynamics for improved macroscopic property prediction.

Jan 1, 2002

By Kerri-Ann Hue, Kerry Hasapidis, Ken Babcock, Patrick O'Hagan

"Metallic nanoparticles exhibit properties that are significantly different from individual atoms or bulk materials. Their applications are diverse and have varying uses in areas such as cancer treatment, biochemical sensors, nanoelectronics, and drug delivery. For each application extensive characterization must be performed in order to probe the unique properties of these nanoparticles. In this study, ultra-high resolution mass sensors consisting of MEMs-fabricated, suspended microchannel resonators (SMRs) were used to determine the size and concentration of metallic nanoparticles. With femtogram (10- 15 g) mass resolution, ultra-high resolution mass sensors can weigh individual particles suspended in fluid, and so measure their mass, density, and size. Particle size analysis with these sensors provides excellent accuracy and resolution compared to mature technologies such as light scattering. This technique also provides quantitative information via the ability count particles.IntroductionThe unique electronic, chemical, and optical properties associated with nanoparticles vary with their size, shape, and composition[ 1-4]. These properties are attributed to increased surface area and nanosized mean free path of electrons to the particle surface. Nanoparticle colloidal solutions have been prepared and are commercially available. In recent years, noble metals such as gold, copper, and silver have been extensively researched[5-7]. In order to tailor the optical, electronic, and electrical properties of nanoparticles, size and shape must be controlled. For many applications a monodisperse colloidal solution is ideal. Methods of size characterization include Transmission Electron Microscopy (TEM), Dynamic Light Scattering (DLS), and Electrophoretic Mobility Measurements to name a few[6, 8]. Although TEM can provide shape and size distributions, sample preparation requires that samples be dried on a metal grid and cannot be analyzed in solution. DLS uses curve fitting algorithms that while useful for determining mean particle diameters are not ideal for polydisperse colloidal solutions. New technologies are therefore needed to accurately determine the particle size distributions of metallic nanoparticles."

Jan 1, 2011

By T. L. Baum

External oxidation during in-line heat treatment of TRIP steels can cause problems for the subsequent coating process. This research aims to elucidate the kinetic rates of internal oxidation, external oxidation and decarburization and their interdependence under different gas atmospheres and temperatures. A rolled steel sample chemistry of 0.14 wt.% C, 1.8 wt% Mn, 0.6 wt.% Si and 1 wt.% Al is used as a case study. Thermogravimetric techniques are used to examine the net mass change in a sample during heat treatment and the results show an initial mass decrease and later an increase for particular partial pressures of H2O. SEM-EDS, optical microscopy and glancing-angle x-ray are used to quantify the microstructure. The cross-section of the samples have 4 distinct zones: (i) an external scale, rich in fayalite, (ii) an internally oxidized region with Al, Si and Mn oxides in an Fe matrix, (iii) a decarburized steel region, characterized by large ferrite grains and low carbon content, and (iv) a relatively unaffected steel core with a structure similar to the starting material.

Jan 1, 2006

By Kuniaki Murase, Tetsuji Hirato, Koji Nitta, Yasuhiro Awakura

"The redox behavior of copper species in an ""ammonium imide"" room temperature molten salt was examined in order to clarify the applicability of the salt to the electroplating media of various metals. Trimethyl-n-hexylammonium bis(trifluoromethanesulfonyl)- amide (TMHA-Tf2N), having an electrochemical window of 5.6 V (50 °C), and corresponding copper(II) salt were synthesized. In TMHA-Tf2N media monovalent copper ion, Cu(I), was stable and Cu metal was oxidized, or corroded, in the presence of Cu(II) species. Cathodic electrodeposition of copper metal and anodic dissolution of it were, thus, one-electron reaction and their current efficiencies were almost 100%.IntroductionElectrodeposition of metals from aqueous solutions is an important soft process for manufacturing thin-film materials, surface finishing, and extractive metallurgy. However, the electrodeposition of base metals, such as zinc, chromium, and nickel, from aqueous media inevitably accompanies hydrogen evolution, which lowers the cathodic current efficiency of metal deposition. Since the electrodeposition of aluminium, titanium, and rare earths from aqueous media is actually impossible due to their largely negative redox potentials, nonaqueous media such as aprotic organic solvent and high-temperature molten salts have been employed for the electrodeposition of these metals. Room temperature molten salts (RTMS),1, 2) or room temperature ionic liquids, have also been developed as a promising electrolytes for the electrodeposition of base metals. In this field, chloroaluminates of alkylpyridinium or alkylimidazolium cation have been well investigated for aluminium3) or alluminium-alloy4-5) electroplating media. On the other hand, in order to avoid high hygroscopicity arising from the use of aluminium chloride, attempts have been made to combine the alkylimidazolium cations with fluorine-containing hydrophobic anions, e.g. BF4-,6) CF3SO3- (TfO-),7) (CF3SO2)2N- (Tf2N-),8) and H(HF)n-ions,9) and investigated for electrodeposition media.'°) Recently, a new series of RTMS consisting of tetraalkylammonium cations and Tf2N- anion, sometimes abbreviated as TFSI- anion, was found independently by MacFarlane et al.11, 12) and Matsumoto et al. 13) This type of RTMS, which is commonly named ""ammoniumimide"" salt, has a wide electrochemical window of ca. 5 V and, thus, the RTMS seems to be suited for practical application as a solvent for the electrodeposition process. In this paper, we report the electrochemical behavior of copper species in an ammoniumimide RTMS, trimethyl-n-hexylammonium bis(trifluoromethanesulfonyl)amide (TMHA-Tf2N)."

Jan 1, 2000

By Jeffrey W. Fergus, Shiqiang Hui

"Aluminum is an important alloying addition to the zinc used in the hot-dip galvanization of sheet steel to control the properties and appearance of the resulting coating. Optimization of the galvanization process requires control of the alloy concentration which can be improved through the use of chemical sensors. Aluminum sensors based on molten electrolytes are commercially available but are not widely used because of their high cost. One approach to reducing the cost is to use a solid electrolyte which can simplify the sensor design and thus reduce the cost of fabrication. In this paper, the development of an aluminum sensor based on a solid fluoride electrolyte, specifically magnesium fluoride, will be described.IntroductionThe concentration of the zinc bath used in hot-dip galvanization affects the galvanization process as well as the properties of the resulting coating. Thus, accurate in situ measurement of the alloy composition can be used to improve process control. This paper describes a solid-electrolyte-based aluminum sensor for monitoring the bath composition during hot-dip galvanization."

Jan 1, 1997

By Eun Duck Park

The gold catalyst supported on iron oxide was prepared from gold dissolved in aqua regia by a deposition-precipitation method and applied to CO oxidation in the absence and presence of hydrogen. Some characterization methods such as X-ray diffraction (XRD), nitrogen adsorption, transmission electron microscopy (TEM), temperature programmed reduction (TPR), temperature programmed oxidation (TPO), and the pulsed CO chemisorption with temperature programmed desorption (TPD) were conducted to explain different catalytic activities of Au/Fe2O3 catalyst pretreated at different conditions. The particle size of gold was about 10 nm for Au/Fe2O3 calcined in air at 373 and 573 K. For complete CO oxidation, the decreasing CO conversion with a reaction time was observed at low temperatures but its initial catalytic activity can be restored by a heat treatment at high temperatures. This catalyst was quite active for the selective CO oxidation in the presence of hydrogen especially at low temperatures. In the presence of hydrogen, the deactivation was significantly diminished.

Jan 1, 2006

By B. Madelin

Over the last ten years, Minemet Recherche and Metaleurop have used an approach in order to investigate and improve the operation of its Smelting furnace and its lead blast furnaces. This approach gives importance- to three complementary means of investigation : - Probing campains in the industrial furnace (temperature and gas analysis profiles), - Chemical and physical modeling (coke combustion, sinter reduction modes, flows patterns, ?.) , - Staged mass and heat balances or kinetic model. This allows to define the limits of operation of each blast furnace and to predict the influence of operating parameters on the furnace performances. For the zinc Imperial smelting furnace, the probing results show the existence- of both an Isothermal reserve zone at 1015ºc and a chemical equilibrium between ZnO and gas which makes possible the use of a practical model for heat and material balances. In particular, very good prediction on the influences of operating parameters can be made. On the contrary, for lead blast furnaces, the probing results show that the thermal and chemical equilibria are not reached. Consequently, classical models for staged heat and mass balances are not sufficient. The use of the other means allows then to characterize the specific influences of operating parameters on the thermal instabilities of these furnaces and their allowed limits.

Jan 1, 1990

By Y. Z. Zhang

Cyanide has generated environmental concerns because of its toxicity, and it may not respond to the treatment of complex and refractory gold ores. Gold leaching by thiourea is one of the most promising substitutes of cyanide. However, the high reagent consumption has hindered thiourea from its commercial application in gold extraction. The process chemistry and mechanism of thiourea degradation has been discussed on the basis of chemical bonding theory, thermodynamics and electrochemistry in this paper. Progresses on the decreasing of thiourea consumption have been summarised. The potential application of thiourea in gold extraction has been evaluated.

Jan 1, 1996