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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 Dian Adisty, Leiv Kolbeinsen, Eli Ringdalen

In Si and FeSi production, the main Si source is SiO2, in the form of quartz. Reactions with SiO2 generate SiO-gas that further reacts with SiC to Si. During heating, quartz will transform to other SiO2 modifications with cristobalite as the stable high temperature phase. Transformation to cristobalite has been investigated and shown to be a slow process where the rate varies between the investigated quartz types. The effect of quartz versus cristobalite as SiO2 source has been studied for reaction (1) 2SiO2 + SiC = 3SiO + CO, by heating of pellets with SiO2 + SiC in Ar-gas. The reaction was faster with cristobalite than with quartz. Initial experiments indicates that this is the case only in Ar and not in CO-atmosphere The higher specific surface area of cristobalite is believed to contribute to the higher rate. The industrial consequences of the observed difference between quartz types are discussed.

Jan 1, 2014

By I. C. Knight

The current levels of copper smelter by-product acid production are reviewed on a regional basis, together with the possible changes in the future. There will be increasing pressure for all smelters to achieve a sulphur capture level of at least 95% by the end of the decade.

Jan 1, 1996

By K. Tozwa

The electrical conductivity of electrolytes for copper electrorefining and electrowinning processes has been reported by many researchers since 1911. The experimental results show that the conductivity increases with an increase in sulfuric acid concentration and decreascs with an increase in copper concentration. In pure copper sulfate solution, however, the conductivity increases with an increase in the copper concentration. After confirming the conductivity of pure and acidified copper sulfate solutions experimentally, the concentrations of hydrogen ion and free (not hydrated) water in the electrolytes were estimated and it was found that the relation between the conductivity of acidified copper sulfate electrolytes and the products of concentration of hydrogen ion and free water is linear. Accordingly, the conductivity of acidified copper sulfate electrolytes increases with an increase in sulfuric acid concentration and decreases with an increase in copper concentration.

Jan 1, 2003

By Andrzej Warczok

Intensive smelting of copper concentrate in Teniente Converter (CT) leads to the production of high grade matte and highly oxidized slag. Smelting slag is processed in Teniente vascular slag cleaning furnace. The slag composition and forms of copper affect the slag cleaning process and final copper content. Converting of high grade matte in Pierce-Smith converter faces some difficulties in proper slagging of iron oxides. Overblowing in copper making stage allows for slag liquidation but leads to high content of copper oxide in converter slag. Converter slag recycling into CT results in the increase of the participation of oxidic copper. Separate treatment of converter slag and its impact on the forms of copper in CT slag has been analyzed. Thermodynamic properties of a system and kinetic limitations pointed out the negative effect of converter slag recycling on the forms of copper and copper recovery in slag cleaning stage. Experimental results of slag cleaning tests in a crucible scale as well as microscopic examination of laboratory and industrial slag samples supported the above analysis and permitted to formulate recommendations of separate processing of converter slag. Keywords: copper, losses, slag, recycling

Jan 1, 2001

By John A. Mavrogenes

Reflected light microscopy and electron microprobe techniques were used to determine the mineralogy, phase percentages, grain sizes, and textures of Co-Ni-rich mattes. The mattes were produced by submerged bath smelting at the University of Missouri-Rolla Pyrometallurgical Center of a flotation concentrate with 4.S% Co and 5.1% Ni that was prepared at the United States Bureau of Mines Rolla Research Center by flotation up-grading of the cobalt and nickel content of a copper concentrate from the Magmont mine, Viburnum Trend, Southeast Missouri. Nine distinct phases were distinguished in the matte samples, and three of these contain cobalt and nickel. The phases that were free from cobalt and nickel are bornite, chalcocite, pyrrhotite, magnetite, metallic copper, and galena. Submerged bath smelting serves to segregate the cobalt and nickel into phases that can subsequently be recovered by flotation. These phases are: shandite (Ni3PbZSZ)' cobaltpentlandite ((Co,Ni,Fe)9SS)' and Co-bearing Fe-rich sphalerite ((Zn,Fe,Co)S). Most of the cobalt occurs in cobaltpentlandite, but some is present in sphalerite. High total air conditions during smelting favor the development and segregation of cobalt into cobaltpentlandite. Nickel occurs in cobaltpentlandite and shandite. Shandite contains lead, a deleterious constituent in the smelting of cobalt and nickel.

Jan 1, 1989

By S. C. Grund

In secondary copper smelting as it is performed at Hüttenwerke Kayser plant in Lünen, tin-and lead-containing flue dusts are produced as intermediate products. These flue dusts are further processed in a hearth furnace. Followed by certain refining operations a saleable tin-lead-alloy is produced. Even though the hearth furnace technology has been in use for this purpose for a long time still its performance undergoes changes in search for optimum processing conditions regarding to the increasing complexity of the raw materials and tightening economical and ecological boundaries. The use of modern statistical tools for the calculation of accurate mass balances is demonstrated for the tin-lead hearth furnace. These reliable mass balances are the basis for any further modelling of the process with the aim of optimization. Incorporating metallurgical knowledge and experience as well as different mathematical modelling techniques, further studies are planned in which the recoveries of valuable and minor elements and their dependency from various process parameters are examined. The aim of this modelling is to optimize the recoveries of the valuable elements, to minimize the energy consumption and the processing costs and thus to keep the process competitive in a harsher economical and ecological surrounding. The modelling principles are transferable to other metallurgical operations and are especially suited for ill-defined pyrometallurgical processes.

Jan 1, 1999

By Kazuki Morita

A new route to produce solar grade silicon (SOG-Si 6N) from metallurgical grade (MG-Si 98%) has been developed in Japan, which may satisfy the increasing demand for solar cells in the near future. Since some elements such as P and B have very large segregation coefficients, solidification refining is not effective for their removal and costly processes, such as electron beam vacuum melting and oxidation plasma refining, are required. According to our previous results which showed the effectiveness of leaching procedure with Ca addition for Fe and Ti removal, possibility of P and B removal by acid leaching was focused expecting that their affinities for Ca in molten silicon might be considerable. Hence, the effects of Ca addition on the thennodynamic properties of P and B in molten silicon alloys have been investigated for overall control and optimization of the SOG-Si production process in the present study. The interaction parameters between Ca and P, and Ca and B were determined by chemical equilibration techniques at 1723 K. Although the interaction parameter between Ca and B was slightly negative, that between Ca and P showed a large negative value. Also, the results for the leaching test with various amount of Ca addition revealed that the removal fractions of both elements, especially P, drastically increased with increase in the Ca content, which showed very good agreement with the prediction from the interaction parameters derived in the present work. The present results suggest that the preliminary leaching procedure can reduce the processing time and energy for SOG-Si refining. Keywords: Silicon, Solar Cell, Refining, Acid Leaching, Thennodynamics. Interaction, Phosphorus, Boron, Calcium

Jan 1, 2003

By Riqing Ye

Laser Engineered Net-shaping (LENS TM) is an emerging manufacturing technique that ensures significant reduction of process time between initial design and final components. The fabrication of fully dense parts with appropriate properties using LENS TM process requires an in-depth understanding of the entire thermal behavior of process. In this paper, the thermal behavior during LENSTM processing of 316 stainless steel was studied both numerically and experimentally. Temperature distribution and gradient in the fabricated 316 stainless steel part were obtained by Finite Element Method (FEM) simulation. The numerical results are in good agreement with the experimental observations. The numerical method may be used to optirnize process parameters and predict the thermal response of LENSTM fabricated components. Key words: Laser Engineered Net-shaping, Thermal Behavior, Finite Element Analysis

Jan 1, 2003

By A. K. Kyllo, N. B. Gray, B. N. McCurry

"Dynamic control of the formation of a solidified layer between a pipe wall and a flowing melt enables the flow rate to be adjusted in real time. This solidified layer can be generated by using a coolant on the outside of the pipe wall to remove the required heat. The coolant, and hence the solidified layer, can be controlled remotely. The dynamic behaviour of the solidified layer was investigated by both physical experiments and mathematical modelling. The mathematical model has been developed using a finite difference technique to describe conduction through the pipe wall and solidified layer. Results from the model were consistent with previous steadystate experimental results using molten lead. Experiments are currently being carried out using molten tin in a recirculating circuit with a cooling system that is instrumented for accurate computer control to validate the model. The circuit is designed for flowrates of up to 24 kg/s (86 tph) of molten tin. Steady-state and dynamic predictions were made for the current rig.Industrial SignificanceThe current method of choice for tapping slags, metals and mattes from many metallurgical furnaces is using an oxygen lance to open the taphole and using a clay plug to close it. There are, however, some significant drawbacks in this method. The heat generated by the oxygen lance erodes the refractory lining of the taphole, as well as the clay plug, and the furnace products themselves corrode the taphole. Using an oxygen lance is also a significant safety hazard to the operators as they must work in close proximity to the furnace and be subjected to a shower of sparks while opening the taphole. Also, the flowrate of material through the taphole cannot be controlled online as the diameter of the opening cannot be varied easily. This feature means that the level of product in a furnace cannot be kept constant."

Jan 1, 1999

By James W. Evans, Dong Xu, Jr. Jones

A physical (water) model based on particle image velocimetry (PIV) has been constructed at UC Berkeley. The PIV technique enables the use of water modeling to quantitatively characterize the fluid flow behavior in the mold during the continuous casting of steel, in a whole field sense, i.e., section by section. A method to obtain e\e time-averagevelocity (TA V) vector maps was developed by averaging 40 instant aneous vectc -r plots revealing the time average features of the flow. Another benefit of TAV vector maps is the ability to compare with present mathematical models, which are mostly based on the time-average technique. Bifurcated submerged entry nozzles (SEN) with ports inclined at various angles to the horizontal were used in the modeling to study their effects on the flow inside the caster. Argon was also introduced into the model to simulate the influence of argon injection on the metal delivery from the tundish into the caster. The bubble sizes and distribution (in specific sections) of argon were characterized, at the same time, by the imaging system of the PIV. This will allow for validation of current mathematical models that were developed to simulate argon injection in casters. Comparison with results calculated by the commercial finite element package FIDAP is also presented.

Jan 1, 1998

By J. F. White

An experimental study was undertaken to evaluate the feasibility of a selective chloridizing roasting pre?treatment process for the elimination of impurities from zinc feed?stocks prior to recovering zinc by conventional unit operations. In this investigation, a number of chemistries that might serve as a basis for such a pre? treatment process were examined. A variety of chloridizing agents were admixed with EAF dust to promote the selective removal of lead and cadmium by the formation of volatile metal chlorides, he results of the experimentation firmly establish that selective chloridizing roasting is a technically feasible means of eliminating lead and cadmium from EAF dust. Excellent extraction efficiencies were accomplished with a number of chloride additives; as high as 98 percent lead extraction and 88 percent cadmium extraction were attained with minimal zinc losses, Continuous pilot?scale tests reinforced the trends established by laboratory?scale experimentation, Attempts of chlorine elimination using pyrohydrolysis were less successful. The extent of chlorine elimination was found to be highly dependent upon EAF dust sample type and treatment temperature.

Jan 1, 1996

By G. Archer

ASARCO, a large and diverse producer of nonferrous metals, is involved primarily in the smelting and refining of lead and copper. Lead-antimony alloys, antimony trioxide, bismuth, cadmium oxide, selenium, tellurium, silver and gold are among products which result from processing by-products of smelting and refining. The complex mixture of concentrates at some smelters and the high impurity loads at some refineries result in various drosses, sludges, dusts and slags. In this paper, the complex interplant and intraplant transfer of by-products is addressed. These by-products result in an exchange of metals between the lead circuit and the copper circuit. Examples of the transfer of by-products and the prospects for the recycle of valuable products from wastes generated by customers and unrelated processors are also discussed.

Jan 1, 1992

By Vadym Drozd, Yongzhou Sun, Shah Najiba, Jiuhua Chen, Andriy Durygin

"Phase transitions of the potential hydrogen storage compound, ammonia borane (NH3.BH3), was investigated using Raman spectroscopy and a diamond anvil cell at high pressures up to 9.5 GPa and low temperatures down to 90K. At room temperature, ammonia borane has three phase transitions in this pressure range. Upon cooling, four new phases were discovered through changes in characteristic Raman spectra. This result provides information about the stability of new bonding characteristics of this potential hydrogen storage material at low temperature and high pressure region.IntroductionDevelopment of hydrogen technology requires the safe, efficient and environmental friendly materials for hydrogen storage and hydrides have attracted much attention as hydrogen storage media. Among chemical hydrides, ammonia borane (BH3NH3) stands out due to its high gravimetric and volumetric hydrogen density ' "". Despite high hydrogen content, this compound is very stable. It releases hydrogen in several steps by thermal decomposition in the temperature range of 100°C to 500°C. Direct thermal decomposition also causes toxic borazine emission. Recent research interests on ammonia borane include destabilizing this compound to lower the dehydrogenation temperature with an enhanced hydrogen release rate using different techniques, e.g. the nanoscaffolds'', ionic liquids"" and acid'"" or transition metal catalysts' ""'. As a molecule of ammonia borane consists of protonic (NH) and hydritic (BH) hydrogens bonded by the polarized dative bond, thermal or catalyzed decomposition requires breaking of N-H and B-H bonding. Still now, the detailed information about the bonding characteristics of ammonia borane is not sufficient to understand details about its phases and structures. The development of methods to enhance hydrogen discharge rate from ammonia borane requires a detailed study about the structural and dynamical properties that control the stability and the intermolecular interactions of this material. This study is motivated to investigate the stability of the existing phases and also to explore the existence of any new phases at different temperatures and pressures which may have enhanced hydrogen release and uptake properties."

Jan 1, 2012

By Ray Y. Lin, Randall A. Blue

"Joining of silicon carbide with infrared using a mixture of Si-30wt.%C as the brazing material has been investigated. Joining was performed at a temperature of 1500 °C in a flowing argon atmosphere for processing times ranging from 5 to 60 seconds. The joining filler materials include thin film silicon obtained by thinning down silicon wafers to about 70 /!m and graphite powder of a 15 /!m average particle size. Joint strengths were determined with a specially designed shear-in-compression jig for testing shear strengths of brittle materials. Cross section examinations of the joined specimens with optical microscopy, scanning electron microscopy and transmission electron microscopy have shown that all joints are essentially void free with excellent wetting between the base SiC and the brazing material. Silicon carbide in the B form has been identified as the reaction product in the joining zone with a transmission electron microscope (TEM) and selected area diffiaction (SAD) analysis. At 1500 °C with a joining time of 60 seconds, the joint has consisted of primarily SiC. With such a high SiC content in the joint, the joint strength is comparable to those by other joining techniques, such as diffusion bonding, as reported in the literature. A kinetic model for the formation of SiC from liquid silicon and carbon is proposed to explain the observed joint microstructural evolution.IntroductionSilicon carbide is of great interest for high temperature structural applications because of its excellent high temperature strength, wear resistance and anticorrosive characteristics [1]. Even though the interest in SiC is high, the use of the material has been limited by the high cost and difficulties involved in forming components of complicated shapes [2]. It is these limitations that necessitate the development of effective joining techniques that are cost effective and able to provide strong joints."

Jan 1, 1996

By I. H. Gundiler

Sandia National Laboratories (SNL) is tasked to support The Department of Energy in the dismantlement and disposal of SNL designed weapon components. These components are sealed in a potting compound, and contain heavy metals, explosive, radioactive, and toxic materials. SNL developed a process to identify and remove the hazardous sub-components utilizing real-time radiography and abrasive water-jet cutting. The components were then crushed, granulated, screened, and separated into an aluminum and a precious-and-base-metals fraction using air-tables. Plastics were further cleaned for disposal as non-hazardous waste. New Mexico Bureau of Mines & Mineral Resources assisted SNL in investigation of size- reduction and separation technologies.

Jan 1, 1995

By William Petruk

A mineralogical and image analysis study was conducted on samples of U tailings from pilot-plant runs on Midwest ore in Northern Saskatchewan. The tailings had been subjected to simulated weathering for the equivalent of 10 years in a tailings facility (lysimeter). The pH varied from 7.0 at the beginning of the test to 5.9 at the end. The results show that during the simulated weathering sane of the gersdorffite, uraninite, galena and pyrite had oxidized, with gersdorffite being the most reactive and pyrite the least. Reaction was evident at the top of the lysilleter , but was most intense at the seepage discharge. sane of the released ions precipitated as Ni, Pb, and U arsenates, sulfarsenates, sulfates and oxides on particles of all minerals. Green crystals of Ni sulfate and white crystals of ca sulfate had precipitated at the surface of the lysilleter. Clay minerals and chlorite had washed from the top of the lysirneter towards the seepage discharge.

Jan 1, 1989

By Kazuhiro Nisizono, Takashi Kuroki, Nobuyuki Mori, Keisaku Ogi

"The improvement of critical current density and mechanical property is essential to the practical application of the superconductive oxides. A solidification technique is developed in this study for the growth of columnar or single Y123 crystal with finely dispersed Y211 and Ag particles through a monotecto-peritectic reaction of Li.(Ba-Cu-Ag-0 rich liquid)+ Y211-+ Y123+Lz(Ag rich liquid). The large solidification rate and temperature gradient can refine the Ag and Y211 particles. But Ag-free region is widely formed along the crystal growth direction in the central part of the Y123 cell. Since this phenomenon occurs because of the cellular growth, it is necessary to narrow Y123 cell width or to grow Y123 crystal with flat freezing interface. By controlling crystal growth direction using a seed crystal, Y123 columnar or single crystal with uniformly dispersed fine Ag particles are obtained. The· behavior of Ag and Y211 particles during the solidification of Y123 crystal is simulated by the peritectic growth model of faceted Y123 crystals.IntroductionY-Ba-Cu-0 superconducting oxide (YBCO) with high critical temperature also has excellent superconducting characteristic under the high magnetic field. The critical current density (Jc) has been enhanced by ·using unidirectional-solidification technique, which can overcome the weak-link problem at grain boundaries and control the crystal orientation and the distribution of Y211 particles which give effective magnetic flux pinning centers in the Yl23 matrix [1-4].In addition to improving superconducting properties, it is necessary to improve mechanical property for the practical application. The silver addition to the melt-textured YBCO superconducting oxide has been reported as the effective method to improve mechanical properties without degrading superconducting properties. Since the material properties are considered to be largely affected by silver particle size, form, dispersion state etc. in the Y123 phase, it is important to control Ag distribution in YBCO/Ag composites. Besides, it is also reported that the silver addition improve the corrosion resistance to the water and CO2 [5,6]. Nishizono et al. [7-9] have reported that the silver distribution in the YBCO/Ag composites is largely affected by the solidification condition, but yet some unclear points are also remained. YBCO has been also fabricated by the zone melting method [10-12], and Furuya et al. [5] and Hirano et al. [13] have reported the fabrication of silver added YBCO composites, but the distribution and behavior of Ag are not investigated in detail"

Jan 1, 2000

By Nourreddine Menad

Plastic materials have been associated with electric and electronic applications since the early days of the electrical industry. Plastics can amount to 30 percents of the scrap mass. Generally, they are treated with flame retardants such as halogenated ones and they can result in different toxic chemical compounds. These plastics can be used as combustibles in the recovery of copper and precious metals. However, during their combustion, halogenated flame retardants can produce dibenzo-p-dioxins and dibenzo-furans. The estimated thermodynamic data of several organic compounds resulting from combustion of electric and electronic scrap, have been used in conjunction with the program HSC to calculate the conditions for dioxin and furan formation. The results show that the formation of the dioxins is dependent on the quantities of carbon, hydrogen, chlorine and oxygen reacting in a given system, as well as on parameters such as temperature and pressure.

Jan 1, 1998

By John L. Watson

Many metals-based industrial processes experience limitations in their operations due to an inability to effectively separate solids and liquids where partidesizes are less than 25 microns. Steel plant sludges ,generated, from the cleaning of furnace off-gases represent a typical example of processing difficulties attributable to material characteristics, and recycling or even efficient disposal of these materials is often a major problem. The use of a magnetic field to augment the traditional mechanisms of vacuum dewatering has, been demonstrated in previous work to have significant value in separating solids and 'liquids, where the solids exhibit some magnetic character. Magnetic vacuum dewatering has been used with magnetite ores and with blast furnace sludges and magnetic fields have been incorporated successfully in drum and disk vacuum filters. The research described in this paper investigates the use of magnetic seed material and flocculants to extend the application of magnetic, vacuum filtration to non-magnetic pulps. It is shown that the addition of a flocculant can enhance the capacity of drum and disk magnetic fIlters when treating materials, such as steelmaking sludges, which are only partially magnetic. In addition, the use of seed magnetite with a flocculant is shown to improve the dewatering of fine hematite pulps in a drum magnetic filter. However the use of a flocculant and seed magnetite had only limited success in improving filtration in a disk magnetic filter with a fine quartz pulp. A disadvantage of magnetic vacuum filtration with seeding appears to bean increase in cake moisture due to water entrapment in the floes resulting from agglomeration and magnetic attraction.

Jan 1, 1999