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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 Joachim Ulrich

The spreading and splashing behaviour of single tin, lead, copper, aluminium and steel droplets impacting on a solid surface were experimentally examined. The droplet impact was observed using a high speed video imaging technique. The onset of splashing and the mass of the secondary droplets of impacting tin and lead droplets was quantified by the weight difference of the droplets before melting and the splat after the impact. The spread factor and the mass of the secondary droplets in dependence of the impact velocity is shown for different droplet materials, initial droplet diameters, target temperatures in ambient air and inert gas atmosphere. An empirical found correlation predicting the transition from spreading to splashing is presented by means of dimensionless numbers.

Jan 1, 1999

By P. Aguirre

Recovery of zinc, copper and nickel from electroplating waste solutions was achieved 'by using a Pulsated Percolated Porous Electrode "3PE" reactor on a pilot plant scale. Intensity - potential curves were used to study the possibility of metal removal and to define the working potential range. The present study describes the use of the 3PE reactors in several electroplating industrial units for the decontamination of their effluents. These effluents were issued from different industrial solutions such as cyanide, sulfate, chloride and Watts baths. Using the stripping curves, deposition rates and electrical efficiencies were determined as function of the metal concentrations in these effluents. Their decontamination could be achieved to the level of few ppm of metals with reasonable current efficiencies. The recovery rates of zinc and copper were about 93 and 99 %, respectively. The. treated effluents contained less than 7 and 1 % of the initial contents of Zn and Cu, respec¬tively. This process allows the recycling of the recovered metals and leads to water saving.

Feb 13, 2014

By Larry M. Southwick

There is much ongoing work in research and development of new processes for the recovery and recycling of met.a.ls and other materials from various waste and scrap streams. Commercialization of such new technologies requires the bringing together and successful execution of a considerable effort involving a variety of activities. These include process conceptualization, research and development, detailed design and construction, and then plant startup and operation. Processes evolve through all of these steps by engineering due diligence, making objective and critical analyses of results, and troubleshooting processing steps to, hopefully, arrive at a sequence that has the best chance to succeed operationally and economically. After a summary review of the above steps, several processes will be described in more detail that provide mostly successful examples of the above procedures. Finally, some observations will be made on areas that will become critical in the near future to the success of new processes for wastes and residues.

Jan 1, 2000

By Shijie Wang

In pressure oxidation leaching of copper anode slimes, than 65% of the tellurium is m' cxtraoted during decopperizing. About l0- 15% of the selenium is also dissolved simultane¬ously by severe leach conditions. Current operation for the treatment of the leachate is to constantly recirculate the leach solution through a bed of copper turnings. The tellurium and sele¬nium are precipitated from the leach liquor as copper telluride and copper selenide and sepa¬rated from the solution by filtration. In order to improve the reaction efficiency and reduce the process cost, viz, minimize the copper addition, cut retention time, and reduce the energy consumption; a chemical reducing agent is studied and the cementation process tested in the laboratory. In this paper, the test results are presented and the process chemistry is discussed.

Jan 1, 2003

By Serge Lavoie

Alcan's Guillaume-Tremblay plant, located in Jonquiere, Quebec, has been in operation since 1990. This was the first plasma dross processing plant ever built. In addition to the use of the plasma heating technology, Guillaume-Tremblay has other unique features making it a modern and efficient dross processing facility. This paper presents a general overview of the practical experience at the Guillaume-Tremblay plant. In particular, the utilization of plasma heating in industrial conditions, the metallurgical performance, the unique dross handling system, the control and information management system and the reclaiming of the by-products will be discussed. Finally, the use of the plasma process for salty dross will be addressed' briefly.

Jan 1, 1995

By Dietmar Eifler, Marcus Klein, Hendrik Kramer

Conventional methods to characterize the fatigue behavior of metallic materials are very time and cost consuming. That is why the new short-time procedure PHYBALCHT was developed at the Institute of Materials Science and Engineering at the University of Kaiserslautern. This innovative method requires only a planar material surface to perform cyclic force-controlled hardness indentation tests. To characterize the cyclic elastic-plastic behavior of the test material the change of the force-indentation-depth-hysteresis is plotted versus the number of indentation cycles. In accordance to the plastic strain amplitude the indentation-depth width of the hysteresis loop is measured at half minimum force and is called plastic indentation-depth amplitude. Its change as a function of the number of cycles of indentation can be described by power-laws. One of these power-laws contains the hardening-exponentCHT eII, which correlates very well with the amount of cyclic hardening in conventional constant amplitude fatigue tests. To identify heat-treatment-parameters and SAE 52100 TRIP-alloys with high hardening rates as well as their damage tolerance the PHYBALCHT- and PHYBALLIT-method were used. One modified SAE 52100 TRIP-alloy was investigated in detail. The fatigue behavior and the cyclic hardening of the selected SAE 52100 TRIP-alloy was investigated and compared with conventional SAE 52100. Conventional stress-controlled fatigue tests were performed on a servo-hydraulic test system with a frequency of 5 Hz and a load ratio of R = -1. Different rates of cyclic hardening were identified. The size of the nonmetallic inclusions leading to crack initiation and the number of cycles to failure were used to evaluate differences in the damage tolerance capability.

Jan 1, 2015

By Srinath Viswanathan, Adrian Sabau

"In general, the occurrence of microporosity during metal casting is due to the combined effects of solidification shrinkage and gas precipitation. The governing equations for fluid flow and hydrogen evolution indicate that porosity formation and fluid flow are strongly coupled. However, in most studies on microporosity, it is considered that the porosity formation does not influence the fluid flow in the mushy zone. In this study, a computational methodology is presented for the numerical simulation of interdendritic fluid flow and microporosity evolution. The solution algorithm presented includes a fully coupled, implicit treatment of microporosity and local pressure in the mushy zone. The effects of microporosity evolution due to the local pressure drop in the mushy zone, and pore expansion in casting regions where liquid feeding alone cannot compensate for the solidification shrinkage are also considered. It is shown that neglecting the effect of porosity formation on the pressure in the mushy zone yields higher pressure drops. By its growth, microporosity partially compensates for the solidification shrinkage, reducing the feeding demand. A reduced feeding demand requires less fluid flow to compensate for solidification shrinkage, and results in smaller pressure drops in the mushy zone. Therefore, in order to accurately describe casting defects, comprehensive models of fluid flow, heat transfer, and solidification must include the effect of microporosity as well.IntroductionIn the terminology commonly used by foundrymen, porosity is usually considered to be either ""hydrogen"" or ""shrinkage"" porosity. Hydrogen porosity is the term given to porosity that is generally rounded, isolated, and well distributed. Porosity that is interconnected or clustered, and of an irregular shape corresponding to the shape of the interdendritic region, is usually termed shrinkage. In general, the occurrence of microporosity in aluminum alloys is due to the combined effects of solidification shrinkage and gas precipitation [1]. Continuum models [1, 2- 7] have been used to predict the level of porosity in castings. A number of other studies have also attempted to understand the phenomena of porosity formation and pore growth [8-10] and pore morphology [11].The governing equations for fluid flow and hydrogen evolution indicate that porosity formation and fluid flow are strongly coupled. However, in most studies [4, 9, 10], it is considered that the porosity formation does not influence the fluid flow in the mushy zone. Kubo and Pehlke [3] presented a methodology for the prediction of microporosity distribution in shaped castings by considering the effects of both the hydrogen precipitation during solidification and the pressure drop in the mushy zone. In their approach, the local pressure and porosity were computed in an uncoupled manner based on a ""flux of interdendritic liquid"" criterion, i.e., either pressure or porosity was first computed using the other variable at the previous time step. Their approach has been used with little change in numerous studies [6, 12, 13]. Recently, Kuznetsov and Vafai [14] presented a fully coupled, one-dimensional model for the computation of pressure and porosity. They showed that neglecting the effect of porosity formation on the pressure in the mushy zone yields higher pressure drops and an over-prediction of final porosity. They also showed that the influence of porosity formation on the pressure is larger at lower pressures in the mushy zone."

Jan 1, 2001

By Gil Bourcier

A process has been developed for detoxifying spent potliner (SPL) in which the SPL is blended with limestone and an anti-agglomeration agent and thermally treated in a rotary kiln. The process has been proven and a commercial plant is in operation at Gum Springs, Arkansas. The treated by-product material has been delisted by the U.S. EPA and is now a potential raw material for many commercial applications. Finding uses for a non-hazardous material has many advantages over finding uses for a hazardous material like SPL. Complete usage of the by-product will complete the life cycle and eliminate any landfilling of non-hazardous SPL by-products or residues. Being non-hazardous and containing compounds used in the ceramic and numerous other industries assures many potential uses for the spent potliner by-product.

Jan 1, 1994

By S. V. Ketov, V. P. Menushenkov, V. S. Shubakov

"The glass samples were obtained by melting of the oxides mixture SrO-Fe2O3-B2O3(Al2O3) at 1200-1250°C with subsequent quenching of the melt on quickly rotating steel roller. Submicronsized Sr(Fe,Al)12O19 particles were formed in glass-ceramic matrix during the crystallization aging of glass. The aging temperature Tag varied in the range 650-950°C. The submicron-sized hexaferrite powder was obtained by removing of the matrix phases using etching. The samples were characterized by X-ray diffraction, scamiing electron microscopy and magnetization measurements. The glass-ceramic material exhibits very high coercivity value up to 10 kOe. The samples of magnets were obtained by pressing of the hexaferrite powder at RT and subsequent aging in the range 900-1200°C. The aged samples exhibit coercivity value up to 8 kOe.IntroductionStrontium M-type hexaferrites have been widely used in technology and industry mainly for production of permanent magnets owing to their appropriate magnetic properties, chemical stability and low cost [1,2]. The SrFe12019-based compounds are characterized by high magnetocrystalline anisotropy and single easy magnetization axis. The highest coercivity is received for monodomain, defect-free single crystal particles with size D - 100 mn. Finely grained strontium hexaferrite prepared by chemical methods such as sol-gel pyrolysis and oxide glass crystallization exhibits high coercivity up to 6-8 kOe [3-5]. Owing to the partial substitution of Al for Fe in the strontium hexaferrite leading to the increase in the magnetic anisotropy field Ha=2Ki/M,, the increase in the coercivity may be received [6]. The notable results were achieved using the SrO-Fe2O3-AlzO3-B2O3 glass crystallization and formation of perfect submicron crystals of alumina-doped hexaferrite [ 6, 7]. The coercive force of glassceramics reached values of up to 10 kOe. Hexaferrite particles are well faceted and have the shape ofhexagonal bipyramids with truncated vertexes [7].In the present paper, we report results of our investigation into the SrO-Fe2O3-B2O3(Al2O3) glass crystallization, hexaferrite powders and permanent magnets, which were prepared by pressing submicron-sized hexaferrite powders at RT and subsequent sintering at 900-1200°C."

Jan 1, 2012

By Yoshisada Michiura, Junko Umeda, Katsuyoshi Kondoh

Rice husks or straws, one of the main agricultural wastes in South-east Asia, have a large possibility to be employed as usefully renewable resources to produce energy and high-purity silica (SiO2), because they consist of about 70% organics such as cellulose or hemi-cellulose, and 20% amorphous SiO2. The former is utilized as bio-mass energy; for example, thermal or electric energy, and bio-mass ethanol. High-purity silica can be used as raw materials in the industrial uses. It would be possible to extract silica elements from rice husks and straws by burning them in air because their main contents are organics. In the previous studies, a strong acid leaching treatment on rice husks before burning was carried out by using H2SO4, HCl and HNO3 to prepare high-purity silica materials. This was available to accelerate the hydrolysis of celluloses and hemicelluloses contained in rice husks, and remove the above metallic impurities. A strong acid leaching treatment, however, is significantly hazardous to environment and human life, and causes an increase of the process cost. In this study, the environmentally benign, harmless to human and economically effective process to produce high-purity amorphous SiO2 materials from rice husks has been established without using strong acids. From a viewpoint of the harmless influence on human body, the carboxylic acids were used in the leaching treatment on rice husks. TG-DTA measurement and GCMS analysis indicated that the leaching was effective for the hydrolysis of celluloses and hemicelluloses contained in rice husks at 473K~873K, which produced the same results in using the conventional sulfuric acid. The metallic impurities could be also removed from the husks via a chelate reaction between carboxyl groups (-COOH) and the metal elements. In particular, it was clarified that cadmium (Cd) were completely removed from rice straws by this reaction. Concerning the burning conditions of rice husks after the acid leaching, it was necessary to supply a suitable amount of air to completely combust organics; for example it required air supplement of 50 ml/min. or more. The burning temperature should be less than 1273K to obtain amorphous structured silica. High-purity amorphous silica materials with 99% or more were prepared from rich husks by applying the citric acid leaching treatment and burning process at 1073K in air.

Jan 1, 2008

By Christina V. White

An experimental study was undertaken to investigate the feasibility of utilizing vapor transport for the treatment of heavy metal contaminated smelter soils. The focus of this project was to develop process chemistries that would make incineration a viable process for the treatment these soils. The experimentation concentrated on the elimination of arsenic, cadmium, and lead, and was performed in a laboramry scale rotary kiln setup. Three soil samples from non¬ferrous smelter sites, which contained various concentrations of contaminants, were utilized in the experimentation. Three chemistries were investigated for the volatilization of the heavy metals: Chloridizing volatilization, ferric chloride vapor complex formation, and the use of oxygen potential control. The samples were analyzed for residual heavy metals so that the extractions could be determined. However, the ultimate test was the leachability of the residual arsenic, cadmium, and lead, as determined by the TCLP test. The results firmly establish that incineration is a feasible process for the treatment of metal contaminated soils. It was found that no one process chemistry is suitable for all different soil samples. A two-step process consisting of a reducing step followed by a hydro-chlorination step was required to make Soil Sample-B pass the TCLP tests for all three heavy metals. Soil Sample-A passed the TCLP tests for arsenic, cadmium, and lead using a hydro-chlorination process at a minimum temperature of 700°C. In addition to passing the TCLP mm for Soil Sample-A and Soil Sample-B, 70 to 80 percent removal of the impurities was accomplished. This demonstrates that the leachability of the impurities was decreased primarily due to the removal of a large fraction of the contaminants, Soil Sample-C possessed very high levels of cadmium and lead and only moderate extractions of the impurities were generated from this soil. The arsenic TCLP test was passed at 500'C using a process gas containing ferric chloride and at temperatures of 700°C and above using chlorination of hydro-chlorination.

Jan 1, 1996

By Yoshihiko Maeda

"Although Japanese mining industry once had been a polluter of toxic heavy metals and gasses, it has been struggling for improvement of environment at mining and smelting facilities under the strict Japanese regulations. Through these efforts, the industry has developed various environmental technologies to be applied in other industries and society.Recycling of metal scraps, for example, has been conducted at smelting facilities. Treatment of hazardous waste, cleanup of contaminated soil and management of landfill are other examples of application of mining and smelting technologies and facilities. In accordance with the worldwide environmental concerns, the industry has become one of the leading industries to promote ""Sustainable Development"", and it is expected further contribution in reducing various environmental burdens to earth by utilizing its mining and smelting technologies and facilities. Some of the examples of these applications are presented in this paper.IntroductionDowa Mining Co., Ltd., established in 1984, is known as one of the ~op Japanese producer of nonferrous metals. Base on its special expertise in the mining and smelting of complex ores, it has expanded its business areas to downstream activities ranging from highly purified metals and alloys, electronics materials, chemicals and related various businesses. Dowa Mining now is becoming more active in the field of waste treatment and recycling.Dowa Mining had operated some mines until 1980th, located at the western part and northern part of Honshuu Island in Japan; the former is pyrite mine while the later is ""Black Ore"" mine,· a complex sulfide ore composed of high grade of copper,· silver, lead and zinc. However, due to the strong yen began in1985; Dowa Mining closed its mining operation in 1994, and has sifted to mining operations in Mexico."

Jan 1, 2000

By Ryokichi Shimpo

Much amount of sludge is produced from the wastewater treatments in surface finishing industry. There are many problems for the abandonment of the sludge because of the high water content and heavy metals included. It is often observed that hexavalent chromium, which is toxic, is generated in the course of heat treatments of the sludge for reducing its amount by dispersing water. In this study, conditions of the sludge calcinations for reducing water contents have been examined. Maximum hexavalent chromium generation was observed in the temperature range around 773 K, at which most of the crystallization water decomposed from the sludge. When the heating temperature became higher than 1173 K, the amount of the hexavalent chromium extracted from the calcined sludge became as low as 10 mg/kg sludge. When the sludge was heated with iron oxides, FeO or Fe203, iron ferrite has been synthesized which may be used as a magnetic material. The amounts of hexavalent chromium generated in the heat treatment with iron oxides were not much different from those without iron oxides.

Jan 1, 2003

By D. H. Rubisov

The neural networks modelling approach is one of the most elegant black-box type methods to model industrial processes. In this paper, this approach is applied to model the performance of the CEZ zinc electrowinning plant. The model that was built was found to exhibit an excellent predictive ability for voltage and current density. The model was also used to investigate the sensitivity of the process to various key variables such as temperature, current density, zinc and sulphuric acid concentration, etc. Optimal regimes for zinc production were identified from the power consumption standpoint.

Jan 1, 1996

By V. V. Satya Prasad, A. Sambasiva Rao

Electroslag melting technologies have recently been developed for recycling light scrap of valuable metals and alloys such as superalloys and oxygen free high conductivity (OFHC) copper at Defence Metallurgical Research Laboratory (DMRL), Hyderabad. Conventionally, electroslag melting processes use consumable electrodes. Because of the difficulty in compaction of scrap into a consumable electrode of satisfactory quality, non-consumable electrodes such as graphite and water-cooled copper have been designed. Electroslag remelting using a water-cooled non-consumable electrode was developed to melt scrap of a nickel base superalloy. Sound ingots with smooth surface finish and properties comparable to vacuum melted superalloys could. be obtained from scrap using this process. A modified electroslag crucible melting process using graphite crucible and graphite electrode was developed for recycling OFHC copper scrap. Copper ingots with less than 10 ppm oxygen and electrical conductivity"" 100% IACS could be produced. The same process was also utilized to produce copper-based alloys such as copper-chromium and copper-titanium starting from copper scrap.

Jan 1, 2000

By J. D. Ecuyer, L&apos

he microstructure of galvanneal coatings formed on extra low carbon and interstitial free steel substrates has been characterized using electron microscopy (TEM and SEM) and x-ray diffraction. The coatings are found to consist of a mixture of gamma, delta and zeta phases, of which delta is the main constituent. The amounts of each phase influences the powdering resistance of the coating which was evaluated using reverse Olsen testing and 60" bending. For the three heat input conditions considered, IF coatings were always found to contain a significant amount of gamma and only those which retained zeta phase on the surface exhibited a satisfactory powdering resistance. In much the same way, ELC coatings with relatively thick gamma layers performed satisfactorily only when some zeta was retained. It was also found, however, that coatings with minimal zeta and gamma had an excellent powdering resistance. The latter coatings were produced under galvannealing conditions of lower relative heat input. These results indicate that in addition to the zinc bath composition, coating weight and galvanneal thermal cycle, the base steel chemistry also has an effect on the coating microstructure. Knowledge and control of all aspects of galvannealing is therefore essential to consistently produce acceptable coatings.

Jan 1, 1992

By Sandra M. Stash

An integrated copper production complex includes mining, milling and smelting facilities which are usually at or near a common site, and sized to complement one another in capacity. There may also be an electrolytic retlnery serving the complex, but not always totally dedicated to its production. Mines and mills without co-owned smelters are not usually considered integrated. The first marketable product of an integrated complex is blister, or in some cases electrolytically refined copper. The nature of integrated operation brings together all of the environmental issues associated with copper production, but currently operating and newly planned facilities are required to anticipate these issues and meet stringent regulations. Older complexes, however, may have legacies of 50 or more years of operation unencumbered by current levels of environmental strictures: nevertheless, they must be remediated. Using examples from closure and remediation of the mining and mineral processing facilities in the Upper Clark Fork River Basin of Montana, the authors review some of the problems encountered since CERCLA's1 enactment in 1980, and the solutions to those problems, bearing in mind that not all of the problems and solutions were technical. Much has been written about the mines of Butte -the "Richest Hill on Earth" as it was known in its day and the mills, smelters and refineries they spawned. These facilities comprised an archetype of the integrated copper complex: from ore to metal in facilities serving and depending on one another. Many great stories of technological innovations and business triumphs have been told about Butte and Anaconda's mining history and the place The Anaconda Company occupies in that history. However, relatively little has been written about the final days: 25 years during which the once-great complex was closed, and the remnants of past glories were remediated after nearly a century of operation. This paper offers some insights from the real world affecting similar complexes still operating, and, hopefully, lessons for others just starting down the path to final closure.

Jan 1, 2003

By Batric Pesic

Reactions of metallic iron were studied in several different aqueous solution systems: water, medium salt solution used for the growth of T ferrooxidans, ferric iron solution and solution containing T ferrooxidans. Each system was studied under abiotic and biotic conditions in the presence of T ferrooxidans and as a function of pH, particle size of iron powder, temperature, ferrous and ferric iron concentrations. It was found that metallic iron reacts with water differently than does with ferric iron in water. Surprisingly, T ferrooxidans were non-functional in the dissolution of metallic iron. Also, the reactions of metallic iron with pure water were indistinguishable from the reactions with water containing medium salts for bacterial growth. The reactions with ferric iron were also independent of medium culture compounds. The mechanisms of metallic iron reactions with ferric ions are different from the mechanisms of metallic iron reactions with water.

Jan 1, 2001

By Dennis J. Kemp

Laterite projects are found in the tropical and sub-tropical regions of the world. As a result severe meteorological situations accompany such projects, often in regions of high seismic activity and political uncertainty. Frequently, socio-economic development supported by political interest is a major driver for development, while environmental protection imposes numerous stresses on the project. This paper will review and examine the many social, environmental, technical and financial issues that a mining and extraction process is subject to during development. The options that must be evaluated will be discussed in the context of sustainable development. Issues of project standards and cultural impact through to long-term issues such as greenhouse gasses and climate change will be assessed in redirecting project environmental norms. Although a rationale for sustainable project can be developed many long- term uncertainties around issues remain. Keywords: sustainable development, communities, social issues, standards, energy, waste management, consultation, agreements

Jan 1, 2004