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By Guojun Qi

This work relates to wafer bumping technologies for flip chip packaging applications in the electronics industry. Nickel and its alloys are alternative under bump metallization (UBM) materials because of their slower reaction rates with Sn-based solder as compared to Cu-based UBMs. In this study, we compared the morphologies of the intermetallic compounds (IMC) formed between Sn-bearing solders (Sn3.5Ag and eutectic Sn-Pb) and two types of nickel- based UBMs, electroless Ni-P (EN) and sputtered nickel. Both chunky-type and needle-type of intermetallics were observed between the EN UBM and the solders. In the case of sputtered Ni UBM, there is only a layer of scallop-type intermetallics formed. The morphology change and growth kinetics of the IMC in thermal aging process were analysed. Kirkendall voids were noticed from samples of Sn3.5Ag solder vs Ni-P UBM that have undergone prolonged thermal aging at high temperature.

Jan 1, 2003

By Ralph P. Hackl

Bacterial leaching of the Doe Run Company?s cobalt/nickel-containing copper concentrate at low pH (pH 1.0-1.2) and high redox potential (>750 mV vs. SHE) enabled the cobalt and nickel to be preferentially dissolved over copper and iron due to the rapid passivation of the chalcopyrite component. Selective leaching of the cobalt and nickel was achieved with a mesophilic culture comprised mainly of Leptospirillum-like bacteria and Acidithiobacillus thiooxidans. This finding led to the conception of a novel hydrometallurgical process for passivating chalcopyrite and recovering the cobalt and nickel. The bacterial leaching process was tested extensively at the bench and pilot plant scales during 1997-1998. A pilot plant containing four leaching stages processed 30-40 kg/day of chalcopyrite concentrate continuously for 87 days. The cobalt extraction ranged from 75% to 86% during 6- and 8-day retention times respectively, whereas the copper extraction was limited to about 9%

Jan 1, 2003

By A. F. Otero

During the electrowinning (EW) of copper significant quantities of highly toxic vapors (acid mist) are produced due to the liberation of oxygen at the cathodes. Acid mist affects the health of operators, the environment and plant infrastructure. Acid mist can be decreased to acceptable levels by a combination of physical means (e.g. ventilation, plastic spheres over electrolyte) and chemical surfactants that decrease the surface tension of the electrolyte, modifying the way oxygen bubbles burst at the surface of the electrolyte. However, only few chemical surfactants are compatible with electrolytic applications, and they are not always used due to their high costs. This paper describes the application of a novel surfactant of natural origin (commercial name Mistop®) to suppress acid mist in copper EW process. Mistop® contains triterpenic saponins derived from the Chilean quillaja tree Quillaja saponaria Molina. The product is non-toxic, and poses no risks to the environment or to EW operators. Mistop® was tested at a laboratory, pilot plant and industrial scale in the world?s largest copper EW production plant at Radomiro Tomic (RT), CODELCO, Chile. At a Mistop® dosage of 8-9 ppm, acid mist decreased below the value accepted by Chilean regulations (< 0.5 mg/m3). At this dosage, Mistop® represents and economical alternative to chemical surfactants, and it is currently industrially used at RT.

Jan 1, 2003

By Huaming Yang

The vanadium-doped SnO2 nanoparticle was synthesized by the co-precipitation reaction and subsequent calcination from the vanadium(III) chloride and tin(IV) chloride. The crystal size, pore size distribution, micrograph and properties of the nanocrystalline powders were examined by differential thermal analysis (DTA). thermogravimetric analysis (TGA). X-ray diffraction (XRD), desorption isotherm (Barrett-Joyner-Halenda method) and transmission electron microscopy (TEM). Thermal treatment of the precipitate powder at 600&apos;C led to the formation of crystal0nmincrystal size. Most of the pores in the narmparticle are about 5~15nm in diameter. Effect of doped vanadium on the crystal size of the nanoparticle was discussed.

Jan 1, 2003

By J. Alberto Vázquez M.

A sensor employing yttria-stabilized zirconia (YSZ) was used to determine the oxygen activity of molten copper at laboratory scale at temperatures of 1200° and 1300 dc. The reference electrode was a Ni-NiO mixture. The amount of the deoxidizing agent (CU3P) ranged from I to 3% of the mass of copper. Thermodynamic analysis of the Cu-O-P liquid system was carried out to predict the required deoxidizing agent and the final composition of the molten copper. Both results, calculated and experimental, show that the oxygen removal is more efficient at lower temperatures. The kinetics of the deoxidizing reaction is very fast in the first minutes of the treatment. A metalography analysis of rapid cooled samples show the oxygen and phosphorus distribution

Jan 1, 2003

By Edgar E. Vidal

The deposition of ceramic materials onto substrates is of special interest in the development of surface related technologies. Research interest has been placed on using thermal plasma as the deposition method, specifically inductively coupled plasmas. Many different modifications to the same basic principle of deposition have been performed through out the materials research community. Such a technique may have many advantages over more conventional techniques, such as high deposition rates, high surface area coverage, clean energy source, no contamination from electrodes and operation near atmospheric pressures. Materials deposited vary from simple oxide systems like TiO2 to more complex structures like ternary oxides and nitrides. This paper reviews recent developments relative to the inductively coupled plasma deposition of thin films.

Jan 1, 2003

By Florian Kongoli

"Lime ferrite" slag with limited silica content has proven to be a valuable choice in the modem processes of copper smelting and converting due to several advantages that this slag offers compared to classical silicate slags. Nevertheless the liquidus surface of this slag has been experimentally measured only at low oxygen potentials such as in equilibrium with iron or hear it and in air. Although most of the smelting and converting processes that use this slag occur at intermediate oxygen potentials, the liquidus surface of this slag is not known at these conditions and the effect of oxygen potential and silica has not been correctly understood. This has brought some confusion in literature as well as in the industrial practice. In this work the liquidus surface of the calcium ferrite slags has been quantified by the means of a new thermophysicochemical model and a new type of liquidus surface diagrams which are very convenient for any industrial process that uses calcium ferrite slags. These diagrams can be easily used to select the lowest liquidus temperature of calcium ferrite slags at a minimum cost and can help design several fluxing strategies in copper smelting and converting processes. The effect of the oxygen potential and silica is also quantified and important industrially related conclusions are drawn.

Jan 1, 2003

By A. V. Tarasov

The high efficiency of autoclave processes is attributed to the fact that they are suitable for processing of refractory raw materials, have low capital costs and high productivity, ensure integrated utilization of the feed materials, produce innovative saleable products, completely eliminate any air emissions, provide low-waste or waste-less technology, as well as mechanization and automation of production processes. In the immediate future, it might be expected that autoclave processes will find use on commercial scale for production of heavy non-ferrous metals in combination with other processes (hydrometallurgical, upgrading, sorption and solvent extraction, electrolytic, etc.) to ensure: -Integrated processing of refractory ores and concentrates (pyrrhotite, zinc, copper-zinc, lead-zinc, nickel-cobalt, copper, pyrite); -Production of metallic powders of base metals as commercial products (copper, cobalt, nickel, etc.), composites on their bases, final products and saleable salts. Processing technologies incorporating autoclave processes, especially, at the stage of liberation (chemical upgrading) of minerals, are characterized generally by high overall recoveries of valuable constituents significantly exceeding recoveries common for conventional pyrometallurgical processes (for some elements by several tens of percent). An example is processing of low-grade refractory pyrrhotite concentrates using autoclave liberation of feed material under pressure of a new reagent, i.e., sulfur dioxide. The use of sulfur dioxide ensures a significant improvement in the recoveries of non-ferrous metals and platinoids to sulfide concentrate and smelting of the latter increases the capacity of the smelting units employed and minimizes the yield of discard slag and loss of metals in slag; in addition, it resolves the problem of sulfur dioxide utilization.

Jan 1, 2003

By Norihiro Murayama

Syntheses of zeolitic materials were carried out from coal fly ash by alkali hydrothermal treatment as part of the reuse and recycle technologies of coal ash, For the obtained zeolites, the cation exchange capacity and acid resistance, which are very important in the practical use of cation exchanger in aqueous solution, are investigated during this stufY, The cation exchange amounts of the NaP, CaP and K-CHA zeolites are measured for various cations such as K+, Na +, NH4+ Ca2+, Mg2+, Pb2+, Cd2+ and so on. The change in crystallization degree are researched as a function of pH. The simultaneous removal ability of NH4+ and PO43- in solution is examined for an example of the water purification with CaP zeolite. From these results, the characteristic and its mechanism of cation exchange are clarified for the various zeolitic materials obtained from coal fly ash.

Jan 1, 2003

By Johannes Boonstra

High rate bacterial catalyzed processes can serve to improve hydrometallurgical operations. These solutions are not only economical but also environmental sustainable. With references around the globe, the value of this new approach is recognized by industry worldwide. For instance, metals can safely and economically be separated from process and waste streams using biotechnologically produced sulfide, recovering a valuable metal sulfide product instead of a waste gypsum stream for disposal. Both the natural biological sulfur and nitrogen cycles offer bioconversions that are applied on industrial scale. The shared advantage of these processes is that waste compounds are converted in either a reusable raw material or in a harmless product. This way, natural product cycles can be closed. Applications based upon bioconversions are for example: Sulfur based: Bioleaching, reduction of oxidized sulfur compounds to elemental sulfur, metal recovery with biogenic produced H2S, SO2removal from gas streams, etc. Nitrogen based: Ammonia removal using the anammox-process, biological removal of NOxfrom gas streams, nitrate removal from water streams, etc. Metals: Bacterial processes for the reduction of metals such as uranium, selenium and manganese have proven to offer great potential for clean-up of groundwater streams. This paper contains a description of the above applications. Further, a short introduction on engineered high rate bioreactor systems and a description of industrial biotechnological applications will be provided.

Jan 1, 2003

By D. G. C. Robertson

The thermodynamics and kinetics of the reactions involved in fuming zinc from oxide slags using coal or coke were first studied in 1955 and have been the subject of many investigations since that time. The key reaction is ZnO(in slag) + CO Zn(g) + COl. This paper will review the some of the recent work, and will add new insights obtained in experiments carried out by the authors. In the first series of experiments it was shown that the reaction 2Fe2+ + ZnO = 2Fe3+ + Zn(g) or 2FeO + ZnO = Fe2O3 + Zn(g) does not occur at an appreciable rate, as is expected from thermodynamic considerations. In the second series of experiments it was shown that zinc does not fume from the slag at a significant rate unless a reductant has been added. This again is in accord with thermodynamic considerations, but is in contradiction to some of the experimental results reported in the literature. A third series of experiments was carried out with excess coke being present, so that the rate of supply of reductant was not in any way controlling the rate. The kinetics of zinc oxide reaction were then found to be independent of the zinc oxide concentration, but increased with increasing basicity, and temperature. The presence of high concentrations of FeO in the slag also improves the kinetics. At low zinc oxide concentrations iron oxide reduction occurred in parallel with zinc oxide reduction. We propose that (under the conditions of this work) the kinetics were controlled by a chemical step, namely the rate of desorption of an adsorbed CO2 species. This is the same mechanism as reported by Belton and co-workers for the kinetics of the reduction of FeO. This explains why the reduction of metal oxides in slags by hydrogen is often faster than by CO.

Jan 1, 2003

By James P. Bennett

EAF slag chemistry and its control have been recognized as important in producing quality steel at a low price for a number of decades_ EAF steel producers make lime and dolomite additions to furnaces, controlling the CIS ratios and sulfur pickup from the steel. Existing phase diagram data at 1600°C for CaO, MgO, FeO, SiO2, and Al2O3 was used to write a computer model optimizing slag chemistry for slag foaming and reduced refractory wear. The model, its development, and its use in an industrial steelmaking environment will be discussed along with how the model can improve energy efficiency. The importance of EAF mass balance to account for critical materials like Si in scrap and refractory wear using the model will also be emphasized_

Jan 1, 2003

By Toru H. Okabe

As part of a systematic study on the thermodynamic properties of complex nitrides, phase equilibria of the system Li-M-N (M Mg, AI, Ga) at 900 K were investigated. An attempt to determine the thermodynamic properties of complex nitrides was made by using the galvanic cell method, which utilizes LiMgN as an electrolyte under nitrogen atmosphere. The electromotive force (Emf) of the cell at temperatures between 800 and 1100 K was measured. While the Emf of the cell at 900 K was measured to be 0.137 V, data discrepancies of ±0.03 V were found. It was difficult to determine temperature dependence of the Emf. The Gibbs energy change for the reaction, 113 Li3N (s) + 1/3 Mg3N2 (s) = LiMgN (s), at 900 K was determined to be !&apos;J.Go, (LiMgN) = -13.2 (±2.9) kJ/mol. Using thermodynamic information on the binary nitride from literature, the standard Gibbs energy of LiMgN was derived to be !&apos;J.Go f (LiMgN)= - 121 kJ at 900 K. The thermodynamic stability range of nitride was discussed by constructing isothermal chemical potential diagrams that provide a better understanding of the stability region of the LiMgN phase. The diagram was found to be in good agreement with the isothermal phase diagram determined by the alloy equilibration method. Although the obtained data includes large uncertainties, the results provide a better understanding of the thermodynamic stability of nitrides. The potential application of this complex nitride to nitrogen chemical sensors or a medium for controlling nitrogen potential is also shown.

Jan 1, 2003

By Alex Mezei

Experimental rheology data are needed to produce design criteria for mass and energy transfer processes. Large throughput plants operate under continuous flow mode. The capital cost is determined by the accuracy of the rheology data used for design. The operating cost is dictated by the energy required to sustain the flowing conditions of various process slurries. Typically, rheology investigations are carried out during the final stages of metallurgical testwork, which is too late to set the design criteria for the pilot plant. This leads to increased testwork cost, and sometimes lowers confidence in the quality of the data produced. In addition, the engineering and feasibility studies are often delayed because of the lack of pertinent rheology data. One of the objectives of this paper is to emphasize the importance of timely planning and execution of the rheology study, which is shown to be a critical component of the overall testwork program. Various applications are discussed, including elaboration of process and equipment design criteria. In this paper, the emphasis is placed on gold and nickel laterite hydrometallurgy applications.

Jan 1, 2003

By Carlos Antonio da Silva

Steel refining reactors based on chemical heating are being used as an alternative to ladle furnaces. They show a high degree of flexibility in respect to heating rate in addition to carrying out refining reactions such as de-S, inclusion removal, alloying etc. IR-UT and CAS-DB are examples of such reactors. Their performance is dependent upon geometrical characteristics as well as operational conditions which determine the flow field inside the vessel. A physical model of the IR-UT process of the Companhia Siderurgica de Tubarao, steel plant located in Serra, Espirito Santo, Brazil, was developed to assess the features of the flow field and its influence on the metallurgical behavior. Results of the physical model were used to optimize the process parameters in the industrial unit.

Jan 1, 2003

By Toshiyuki Kozuka

CdTe metal composite semi-conducting material has high potential in good performance of energy conversion efficiency for solar cell and there is much room for improvement of the performance by developing a process of making a thin CdTe film. In this paper, the imposition of intense magnetic field on CdTe electro-depositing surface is proposed, which is one of the possibilities for improving the energy conversion efficiency. In the experiment, cryogen-free super-conducting magnet up to 5T was used and CdTe film was deposited electrically in -o.nv vs. SHE The electrolyte was Cd and Te ammonia alkali solution with controlled temperature in the acrylic cell of 70mm diameter. Electro-deposition behavior of CdTe has affected by the imposition of the intense magnetic field due to microscopic convection in the vicinity of the depositing surface. Electro-deposited surface of CdTe becomes smooth due to microscopic convection around the surface, and the crystallization behavior is also affected, where crystallization temperature and the grain size is changed by the imposition of intense magnetic field.

Jan 1, 2003

By Doug Halbe

?Many are called, but few are chosen.? The biblical adage applies not only to life, but also to hydrometallurgical processes. There have been, in the past, many outstanding successes with new processes ? and also some dismal failures. What are the odds of success for a new process? When there have been problems, why? What can you do to make sure these problems don?t occur with your process? What effect will a slow startup have on project economics? How do financial institutions ? the people who loan your company money for the project ? feel about new processes and why? Is it possible to predict or estimate the time required to reach design parameters?and if so, how do you sell this estimate to management ? and financial institutions? Probably most important ? when do you start thinking about the answers to these questions?

Jan 1, 2003

By Torn H. Okabe

A fundamental study was conducted with the purpose of establishing an environmentally sound recovery process for recycling of valuable metals, by combining scraps containing such metals. As an example, direct extraction and recovery of neodymium (Nd) in magnet scraps was investigated by utilizing liquid metal as an extraction medium. It was found that liquid magnesium (Mg) is a suitable extraction medium and can extract Nd from iron alloys with high efficiency at around I 100 K. The newly developed extraction apparatus for Nd is a mechanically simple and static device without moving parts, where the Mg extraction medium circulates due to differences in the temperature inside the reaction vessel. This developed device can simultaneously accomplish continuous extraction of metal Nd from scraps, re-extraction of Mg from Mg-Nd alloy and the eventual recovery of pure Mg. As a result, metal Nd with 98 % purity was directly recovered from magnet scraps under certain conditions. It was also shown that the extraction agent Mg could be reused. The results of this investigation show the possibility of establishing a new process for the direct extraction of Nd in pure metal form without oxidization.

Jan 1, 2003

By Jiann-Yang Hwang

A study on microwave assisted chalcocite leaching was carried out with a microwave hydrothermal reactor. The leaching was conducted with thick mineral slurries (50-100 g/l). The leaching media is a mixed solution of CuCL2 and NaCL The investigation included the effect of leaching temperature, quantities of the minerals per unit slurry volume as well as the initial concentration of cupric ions were investigated. The results were discussed and compared with that using conventional leaching method.

Jan 1, 2003

By Zhang Chuanfu

The fibrous nickel oxide powder was prepared by the method of chemical precipitation and pyrolysis, that is, the NiO precursor was firstly precipitated from nickel ions solution with addition of oxalate salt and then the final NiO powder was obtained by pyrolysis of the prucursor. The effects of the pH, reaction temperature, reactant concentration, addition of surfactant on the morphology of the precursor particles were investigated. The influences of the various conditions, including the temperature and time, the air flow and the speed of the temperature increase on the morphology, average size and specific surface area of the NiO particles were also addressed. The fibrous NiO particles with IOO~ 120 in axis/diameter ratio and 5.5 m2/g of the specific surface area may be produced under certain operation conditions by this process.

Jan 1, 2003