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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 Stephen W. Paff

The EPA has estimated that there are over 3,000 sites across the United States contaminated with lead. Techniques to remediate these sites include standard stabilization/disposal technologies, reclamation of lead using secondary lead smelters, soil washing, and biological removal technologies. In this paper, the current technologies used for lead remediation will be reviewed. Factors affecting the use of each technology, such as range of applicable concentrations, soil types, interferences from other contaminants, economics, and current technology status will be assessed. The paper will also focus on the results of a recent study completed by the Center for Hazardous Materials Research (CHMR), in conjunction with a major lead smelter, which demonstrates that secondary lead smelters may be used economically to reclaim lead from a wide range of lead-containing materials frequently found at Superfund sites. Such materials include battery case materials, lead dross, and debris containing between 3 and 70% lead. The results of development work completed by CHMR on the Acid Extraction Treatment System (AETS), which has been demonstrated to extract Lead from soils containing up to 30,000 mg/kg lead, will also be presented. The use of these technologies will be compared with other options for the remediation of sites.

Jan 1, 1994

By J. Méndez-Nonell

The thermodynamic and chemical properties of SrSO4 and SrS in a gaseous flow of CO and CO2 at high temperature are discussed. The thermodynamic analysis of the system was made using data from the literature. The results obtained from the thermodynamic analysis were experimentally verified using the thermogravimetric technique. The experimental results suggest the formation of a complex compound between SrO and SrSO4. It was also found a change in the chemical mechanism of the process between SrSO4 and CO-CO2 and in the chemical mechanism of the process between SrS and pure CO2.

Jan 1, 1995

By Willy Persson

A common feature of the kinds and amounts of impurities present most pyrometallurgical, processes is injection of oxygen to, remove various in the feed. The degree of success of a specific process step relies critically on control of the instantaneous oxygen potential/oxidation stage, throughout the step as well as upon termination of the step. This will, for instance, determine the distribution of impurities between metal and slag. As long as the operation is perturbation free -detailed analysis of all additions and application of advanced models often yield satisfactory control means However, a pyrometallurgical process is seldom free from disturbances, which reduces the accuracy of the static models and leads to inconsistencies in scheduled route might be uncontrollable changes in quality and quantity of feed, operator interventions and shift changes, timing of cranes, lining wear and accretions etc. The implementation of dynamic, control to correct for disturbances and, more generally for process optimization, requires continuous on-line information on, the actual status of the process. The implementation of sensors for continuous process monitoring, e.g., as regards the instantaneously prevailing oxygen potential or oxidation stage, has been hampered by the highly aggressive environment in smelters; This is. where remote-sensing techniques based on optics and spectroscopy, have proven to form invaluable, tools towards the realization of dynamic production control. Since about 15 years Semtch has developed and industrialized a remote-sensing technology, based on ,optics and spectroscopy, for continuous on-line process monitoring and production control of various pyrometallurgical processes. The presentation will discuss applicability aspects with examples and experiences from installations and tests in ferrous and non-ferrous industry. Keywords: Applied spectroscopy, Metallurgy, Process monitoring, Production. Control

Jan 1, 2003

By William Petruk, J. H. Gilles Laflamme, Jean Robitaille, Louis J. Cabri

"A quantitative mineralogical study using ore microscopy, electron microscopy, proton-microprobe, image analysis, and material balances was done on samples from the circuit of a concentrator in Quebec, with particular emphasis on the Cu concentrate. The ore contains many different minerals, of which the principal ones, in decreasing order of abundance, are pyrite, sphalerite, chalcopyrite, bornite, galena, tennantite, and pyrrhotite. Minor to trace amounts of covellite, chalcocite, stannoidite, mawsonite, colusite, wittichenite, miharaite, hessite, petzite, electrum, and an unidentified Cu-Pb-Bi-sulfide also occur.Liberation of pyrite is very high in all size fractions for all samples (ranging from 80-91 %). Liberation of chalcopyrite, bomite, sphalerite, and tennantite is relatively high, on average, in the head .sample and Cu concentrate (55-78% and 66-88%, respectively). Most of the chalcopyrite in the flotation tails is not liberated, whereas about one half of the tennantite and sphalerite are liberated in both the flotation and :final tails. Recoveries calculated for the Cu concentrate (on the basis of assays, mineralogy, and image analysis) are chalcopyrite 72. 5%, bornite 73. 7%, sphalerite 41.0%, tennantite 70.9 %, and galena (together with some trace minerals) 34.2%. It was also calculated that the Cu concentrate contains 10.0 % of the pyrrhotite and i.4 % of the pyrite.Materials balance calculations were done on the five major sulfide minerals to determine the mineralogical distribution of 13 major, minor, and trace elements (as determined by protonmicroprobe analyses). It was determined that tennantite is the principal carrier of Bi (67%), As (90%), and Te (86%) in the Cu concentrate. Therefore, removal oftennantite, which is mostly liberated in the Cu concentrate would significantly reduce these three contaminant elements, but at a loss of9% of the Cu, 2.0% of the Zn, and 0.7% of the Ag. The precious metals (Au, Ag) occur as discrete minerals (electrum, petzite, hessite). Some of the Ag also occurs in solid solution in bornite (23.1% of Ag in Cu concentrate), tennantite, and sphalerite. Four of the major sulfides (chalcopyrite, bomite, sphalerite, tennantite) in the ore also contain measurable concentrations of the following trace elements: Se, Cd, In, Sn, and Sb, occurring mostly as solid solutions. Some of these elements are also concentrated (up to about 18%) in minor and trace minerals such as colusite, stannoidite, and mawsonite."

Jan 1, 1999

By Stephen K. Pave1

Over 1,100 tons per day of Fluid Catalytic Cracking Unit (FCCU) catalyst is used worldwide. During the cracking reaction, catalyst is contaminated by deposited metals including nickel, vanadium, potassium, copper, iron, sodium, etc. To compensate for contaminants, a portion of the circulating catalyst inventory is withdrawn for disposal and fresh catalyst is added. The DEMETR process takes spent FCCU catalyst and removes a portion of the metal contaminants, enabling the refiner to recycle demetallized catalyst, thus reducing the solid waste from the refinery. Through August, 1993, the operation of one unit for one refiner has resulted in the recycling of over 7,500 tons of spent catalyst.

Jan 1, 1994

By Kafui Nyavor

Acid mine drainage (AMD) is presently the biggest single environmental problem facing the mining industry. New and expanding metal mines in most parts of the world have to demonstrate their ability to contain this problem to obtain operating permits. Conventional methods of controlling acid mine drainage have primarily been limited to collecting the drainage and neutralizing with alkaline materials which do not provide a permanent solution to the AMD problem. Since acid mine drainage results from the oxidation of sulfides in the presence of oxygen, water and iron-oxidizing bacteria, controlling any of these three factors contributing to pyrite oxidation provides a potential at-source remedy for reducing or preventing acid mine drainage formation. Physical properties such as hydrophobicity also play an important role in the attachment of bacteria, adsorption of oxygen, water, and other ions that subsequently lead to the oxidation of pyrite. In this communication, the suppression of pyrite oxidation by treatment with fatty acid amines (FAA) was investigated. The FAA treated pyrite samples were tested at various conditions of temperature and pressure. At an elevated oxygen pressure of 500 psi and a temperature of 600 C, less than 0.2% oxidation was obtained for the FAA treated pyrite samples, while over 1.2% oxidation was obtained for the untreated samples in 10 hours of oxidation time. Accelerated column oxidation tests at ambient condition showed that FAA mated samples reduced pyrite oxidation by at least 75% in 81 days.

Jan 1, 1994

By Tom Lewis

The metal finishing and electronic industries are searching for ways to recycle materials · and reduce costs. The areas of heavy metal waste and water recycling has gained new interests with the potential of impacting the operation's bottom line. Lewis Environmental Services, Inc. has completed numerous heavy metal recovery and effluent recycling projects with its ENVIRO-CLEAN PROCESS for government and private sector clients. This patented process utilizes a proprietary chemically treated granular activated carbon with enhanced heavy metal adsorption capabilities combined with electrolytic metal recovery to produce a saleable metallic product. The process generates no sludge or hazardous waste and the effluent meets EPA .limits. This paper covers several heavy metal removal projects, two fullcscale commercial installations, and one treatability case study.

Jan 1, 2000

By Ikuhiro Sumi

A new steelmaking process, in which manganese ore was intentionally reduced, was developed to achieve a higher manganese Yield using a combined blowing converter. In this study, manganese behavior was discussed through the introduction of a model. Apparent reduction rates of manganese were calculated by the two terms that were determined experimentally, with SOkg and 2S0ton combined blowing converters. The model calculated manganese changes during the operation. We applied the model to the actual operation and found that manganese behavior was predicted fairly well by this model.

Jan 1, 1996

By E. vanHuyssteen

A method of establishing the relationship between the mineralogy of a sinter and its subsequent processing behaviour in a lead blast furnace is demonstrated. It involves: 1) analyzing the Zn-spinels, hardystonite, larsenite, Pb-silicates, Pb-arsenates, Pb-(Ca)-sulphates and other femtes with an electron microprobe; 2) determining the extent of elemental substitutions in various mineral structures; 3) establishing a sequence in which the various phases formed during sintering. In this manner the relationship between the bulk chemistry of a sinter formulation and the speciation of elements into various phases in the sinter can be established. Specifically, the-substitution of Mg for Zn in hardystonite significantly influences sinter production. Mg substitution releases Zn into the surrounding matrix. This Zn reacts with the Pb-silicate to form larsenite thereby reducing the amount of Pb-silicate available for anhydrite digestion. Excessive amounts of residual anhydrite thus result if the sinter formulation is based solely on the CaO/Si& ratio.

Jan 1, 1993

By F. F. Lins

There is a large use of mercury in Brazil by the gold miners in the so called "garimpos" (non registered mining operations), where it is usual to recover the gold contained in the gravity concentrates by amalgamation, which is highly deleterious to environment if not conducted properly. Unfortunately, this is a common practice there. After presenting in brief the modus operandi generally practiced in the garimpos and the environmental problems, this work reviews some of the research conducted in CETEM according to two approaches: (i) replace amalgamation by other processes and (ii) develop technology to treat mercury-contaminated soils and effluents. Conventional processes like froth flotation, to recover gold from gravity concentrates, and centrifuges were considered. Also as alternatives to amalgamation, innovative process like the recovery of gold by coal-oil agglomerates and a technology that is currently under development in our laboratory, called gold-paraffin process, are described in brief, some results presented and their potential use assessed. To reclaim sites already polluted a technology was developed to float mercury selectively from contaminated soils. The potential use of centrifuges to pre-concentrate the mercury is also discussed. The scope for applying the last techniques is to concentrate the pollutants in a small volume of mass which would be suitable for recycling or isolation from the environment. A prospective technology to treat contaminated soils, or mercury concentrates, is the immobilization of mercury by adding inorganics. Concerning the ionic mercury which may be present in effluents, precipitation of the ions and flotation of the precipitates are being studied.

Jan 1, 1994

By Zuhair A. Munir

"The use of self-propagating combustion reactions to synthesize metallic, ceramic, and composite materials is described. The limitation of this process because of the porous nature of its products is discussed. The formation of dense bodies through the simultaneous application of pressure is shown for a metal-matrix composite. The effect of an external electric field on the synthesis of ceramic and composites is described. The nature of the effect of the field on the mechanism of synthesis is analyzed theoretically and experimentally. The use of the self-propagating combustion to synthesize intermetallic thin films is presented for the Ni-Al and Ti-Al cases. The formation of functionally gradient materials (FGM) by centrifugally-assisted self-propagating high-temperature synthesis is described.IntroductionThe use of self-propagating combustion reactions for the synthesis of a large number of simple and complex materials has been described in numerous publications. These have been amply discussed in several review articles [1-4]. The many benefits of this method of materials synthesis are commonly examined in light of its most significant limitation: the porous nature of its products. The porosity in the products of self-propagating high-temperature synthesis (SHS) is an intrinsic characteristic of the process and its elimination has been the focus of numerous attempts. Various experimental methods have been used to accomplish this goal."

Jan 1, 1994

By William Petruk

The Kidd Creek base metal deposit near Timmins, Ontario contains around 0.15 wt% Sn, mainly as cassiterite. The cassiterite occurs largely as inclusions in sphalerite, with 85% being in grains smaller than 18.5 micrometres in diameter. Concentrates and tails from the company's Cu, Pb and Zn circuits were studied to determine the liberations and recoveries of cassiterite in the products. The ore had been ground to about 65.% minus 44 micranetres in diameter (-325 mesh); 55% of the cassiterite was liberated. About 92% of the liberated cassiterite and 70% of the unliberated cassiterite were in the concentrator tails, and 20% of the unliberated cassiterite in the zinc concentrate. The company had attempted to recover the cassiterite from the concentrator tails by gravitational methods but recoveries were low. The grain size of the cassiterite in the gravity Sn concentrate was similar to the grain size of the liberated cassiterite in the concentrator tails. Research on flotation of the fine grained cassiterite from Kidd Creek ore has been conducted,

Jan 1, 1990

By M. C. Furerstenau

Adsorption behavior of various surfactants on sulfide minerals is very much affected by the nature of the surface of the mineral. Since sulfides are naturally meta-stable, oxidation occurs when they are exposed to air, especially in aqueous environments. As a result. oxygen assumes a major role in sulfide flotation. Mechanisms of adsorption of various thiol collectors on sulfide minerals have been reviewed. The electrochemical behavior of various sulfide minerals has also been reviewed. Flotation behavior of galena, chalcocite, sphalerite, pyrite, chalcopyrite and pentlandite has been presented together with the. flotation of copper sulfide- nickel sulfide ore.

Jan 1, 1993

By M. Friák, L. G. Wang, M. Šob, V. Vitek

"The paper gives an account of applications of quantum-mechanical (first-principles) electronic structure calculations to the problem of theoretical tensile strength in metals and intermetallics. First, we briefly describe the way of simulating the tensile test and the electronic structure calculational method. Our approach is then illustrated on calculations of theoretical tensile strength in W, NiAl and transition metal disilicides MoSi2 and WSi2 with C11b structure. In Wand NiAl, we consider uniaxial tension along [001] and [111] directions. Although tungsten is elastically nearly isotropic (C44 = C”), theoretical tensile strength exhibits a marked anisotropy (oth/001 = 29 GPa, o'th/111 = 40 GPa). Calculated results compare favorably with experimental value of 24.7±3.6 GPa obtained for tungsten whiskers grown along the [110] direction. Similarly, in NiAl, the 'hard' orientation [001] differs very significantly from the [ill] orientation (oth/001 = 46 GPa, oth/111 = 25 GPa). This anisotropy is explained in terms of higher-symmetry structures present or absent on the calculated deformation paths. In disilicides, the theoretical strength is calculated for [001] loading (oth/001 = 37 GPa and 38 GPa for MoSi2 and WSi2 , respectively). The role of relaxation of internal structure parameter is discussed and changes in bonding conditions during the tensile test are analyzed.IntroductionIn most engineering applications, the strength of materials is limited by the presence of internal defects. If there were no defects, then, for example, the tensile strength could be several orders of magnitude higher and its value would be comparable with that of shear modulus. Therefore, the strength of ideal (defect-free) crystal represents an upper limit of attainable stresses, which is called the ideal strength. While it may not be possible to achieve the ideal strength in practice, it is not possible to exceed it. However, the ideal strength is already approached in situations which are technologically relevant. These include the low-temperature deformation of inherently strong materials, such as diamond, Si, Ge and some of the transition-metal carbonitrides, deformation of whiskers, nanoindentation of materials with low defect densities, hardened thin films and coatings etc. The ideal strength sets the limits of elastic stability of a solid. Its knowledge is useful for estimation of the ideal work of fracture stresses needed for homogeneous nucleation of dislocations and for modelling of crack propagation."

Jan 1, 2001

By R. D. Irwin, W. M. Mullins, E. A. Medina

"Various stability criteria are introduced and thermo-kinetic models for metallurgical processes are used as concrete examples for evaluation. Kinetic criteria for the process of dynamic recrystallization are proposed. These criteria are compared to the non-equilibrium thermodynamic approaches discussed in the literature. The application of macroscopic stability criteria to materials processing is then discussed.IntroductionThe mechanical behavior of metals at elevated temperature is very well predicted by any of several empirical constitutive relations. Typical is the power-law (or Swift's) form,Equationwhere r-is the stress, y is the strain and m, n , t0, y0 and Q are material constants. This form has been used with some success in the metals processing area [1]. In general, though, all of the empirical constitutive equations are static, failing to account for any dynamical properties of the system they seek to describe.The physics of warm deformation is qualitatively well understood. An example is power-law creep, where the dominant mechanism is assumed to be lattice diffusion limited climb of dislocations, which allows the strain-rate to be determined by the applied stress through"

Jan 1, 1997

By J. Wong

We report a successful use of x-ray absorption spectroscopy to probe the chemical and structural environment of trace elements in coal. When applied to vanadium in coal, it was found that vanadium exists in at least two environments: a trivalent site 6-fold coordinated by oxygens at ca. 2.0~ and a tetravalent site 5-or 6-fold coordinated also by oxygens, one of which forms a short V=O bond at ca. 1.6a. No evidence of nitrogen (porphyrin)1'or sulfide environment was found. It was also found that the vanadium environ-ments in the raw coal did not survive unchanged in a liquefaction process. These findings have implications for coal cleaning processes and for trace element release into liquefaction process streams.

Jan 1, 1982

By Shengqi Chen

The reduction smelting of nickel laterites produces slag, consisting principally of the chemical components MgO, "FeO", SiO2, and A12O3, and ferro-nickel alloy. Despite the fact that the phase equilibria for the ternary MgO-"FeO"-SiO2 up to 1500°C is well established limited experimental data are available in the MgO-"FeO"-SiO2-Al2O3 system, which is relevant to commercial operation of the process. A methodology has been developed for the experimental investigation of the liquidus temperatures for the multi-component system MgO-"FeO"-SiO2-Al2O3-Cr2O3 in equilibrium with metallic iron. Experiments have been carried out using high temperature equilibration, quenching, followed by electron probe X-ray microanalysis (EPMA). Liquidus temperatures have been determined in the silica primary phase field in the composition ranges directly relevant to the Cerro Matoso S.A. ferro-nickel smelting slag. Liquidus isotherms have been determined for temperatures between 1450 to 1600°C. The study enables the liquidus to be described for a range of MgO/FeO ratios. It was found that liquidus temperatures in the silica primary phase field decrease significantly with the addition of AI2O3. Keywords: Liquidus temperature, ferro-nickel, pyrometallurgy, smelting

Jan 1, 2004

By J. K. Brimacombe

Plant trials have been conducted at the Tacoma Smelter of ASARCO to assess the effect on tuyere blockage and refractory erosion at the tuyere line, of increasing the injection pressure of air into a Peirce-Smith con¬verter. Four tuyeres each having an ID of 19.1 mm (3/4 in) were installed toward one end of the tuyere line of the No. 4 Converter. Air and oxygen-enriched air were injected at 414 kPag (60 psig) through these tuyeres and at the usual 83 kPag (12 psig) through the remainder of the tuyeres in an otherwise normal converter campaign. The test campaign consisted of 88 charges and lasted for 89 days. During this period, punching of the high-pressure tuyeres was found to-be unnecessary; and when, as a precaution, the tuyeres were cleaned by hand at the end of a charge, they were always open. Also it was observed that the flow of high-pressure air remained constant. Accretion formation around the tip of the high-pressure tuyeres varied from charge to charge and was influenced by the matte grade and the level of oxygen enrichment.

Jan 1, 1983

By Faustino G. Prado

In the, quest for an economical and environmentally friendly reclamation of metallurgical dusts generated during pyrometallurgical operations, our goal has been the separation and recovery of most of the components, as well as the complete recycle of all the reagents. Effluents have been avoided, within acceptable economic parameters. This presentation, which can be applied to a large spectrum of dusts and other residual-materials-, has focused on the dusts generated by the operation of Secondary Copper Smelters. Those dusts show a wide range of components, including zinc, lead-, copper, cadmium, tin, chlorine and-alkalies. Our present work deals with the use of ammonium salts in the separation and recovery of-the above mentioned elements in a marketable form. Most of the chemistry and techniques involved have teen already confirmed in commercial scale operations. Others have gone through pilot scale tests or bench scale tests. The recycle of reagents has also been- confirmed at the same operating levels. A preliminary evaluation indicates that the chosen route, in addition to a viable economy, offers a complete and safe reclamation within the most strict environmental regulations.

Jan 1, 1995