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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 N. Choi

The distribution behavior of selenium and tellurium in nickel sulfide smelting was investigated in the temperature range of 1250-1300 °C under an inert gas atmosphere and various oxygen partial pressures. The distribution coefficients of selenium and tellurium between nickel-copper-iron matte and silica-saturated iron silicate slag were detennined in terms of matte and slag compositions, temperature, and oxygen partial pressure. The effect of slag additives such as CaO, MgO, and Ah03 on the distribution coefficients of those elements was also investigated. It was observed that the distribution coefficients of selenium and tellurium increased with increasing matte grade and temperature. The solubility of selenium and tellurium in the slag decreased with increasing the partial pressure of oxygen within the range investigated in this study. The distribution coefficients of selenium and tellurium increased with the amount of CaO and MgO. Tellurium distribution coefficients also increased by the addition of Ah03. Meanwhile, the addition of Alz03 decreased the distribution coefficients of selenium at high matte grade.

Jan 1, 1996

By Kimio Itagaki, Makoto Ohtsuka, Kouki Chiba, Minoru Matsumoto

"The properties of Ni-Mn-Ga films such as chemical composition, crystal structure, microstructure and transformation temperature were investigated with respect to sputtering conditions in the present study. The Ni-Mn-Ga films were deposited on a polyvinyl alcohol substrate with a radio-frequency magnetron sputtering apparatus using the NisoMn2sGa2s and Nis2Mn:«1Ga24 targets. After separating from the substrates, the films were annealed at the temperature between 873 and 1273 K for 3.6 ks. The chemical composition of the films depended on the radiofrequency generating power, however, there was no dependence on the heat treatment temperature. Each deposited film had a columnar grain structure. After heat treatment, the width of columnar grains widened and then became indistinct with increasing heat treatment temperature. The Heusler type cubic crystal structure of the fi4n with heat treatment at 1073 K changed to the tetragonal one through the martensitic structural transformation during cooling. The martensitic structural transformation temperature increased with increasing nickel content of films, while the Curie temperature decreased. The film obtained at 200 W using the Nis2Mn24Ga24 target after heat treatment at 1073 K showed one-way shape memory effect through the reverse martensitic structural transformation during heating.IntroductionThe ternary intermetallic compound NiiMnGa has a Heusler-type crystal structure and is an intelligent material, which has a shape memory effect and a ferromagnetic property. The martensitic structural transformation occurs within the ferromagnetic temperature region. The cubic crystal structure of L21 at high temperature changes to a tetragonal one through the martehsitic structural transformation during cooling. The films of this compound can be applied for an actuator of micro-machines."

Jan 1, 2000

By Marc Verhaege

The effluent under investigation results from a catalic oxidation unit in which paraxylene is oxydised to terephtalic acid. The solution contains cobalt and manganese as their acetates in a concentration range of 0,4 - 1,2 g/I of cobalt and 0,8 - 2,4 g/l of manganese. Before being fed into the main waste stream treatment unit of the plant it is advisable to apply a petreatment step in which both metals are eliminated to a great extent from this effluent. Conventional treatment is done by precipitation of both metals either through pH increment with a base or by adding a suitable reagent producing insoluble species. The aim of this study was to look for a treatment (elimination of both metal species) in which no sludge or precipitate is formed.

Jan 1, 1995

By Duan Xin-hui, Wang Xin, Peng Jin-hui, C. Srinivasakannan, Zhang Li-bo

The work attempts to optimize the process of preparation of modified semi-coke from semi-coke using phosphoric acid (H3P04) as the activating agent using the response surface methodology (RSM). The influences of three major dependent variables, the impregnation ratio, activation time, and activation temperature were assessed on the independent variables yield and the iodine number. The empirical relationship between the dependent and the independent variables were established using the quadratic response surface models, which were utilized to optimize the process parameters. The significance of each of the parameters and interaction among the parameters on the independent variable was assessed based on analysis of variance (ANOVA). The process variables were varied within the range of impregnation ratio (IR) from 1.5 to 4, activation time from 30 to 90 min and activation temperature from 550 'C to 650 'C. The optimized process conditions were estimated to be an IR of 2.29, activation time of 32 min, and an activation temperature of 605°C respectively using the process optimization tool. The BET surface area of modified semi-coke of the optimized sample was estimated to be 915m2/g, with the pore volume of0.71cm3/g, with an average pore diameter of 3.09 nm, with micropore volume fraction being 52.36%. The scanning electron microscope (SEM) images were utilized to visualize the surface pore structure.

Jan 1, 2013

By Dean Ilievski

Mathematical modelling of the precipitation process requires that the kinetics of crystal growth, nucleation and agglomeration be known: This paper reviews the current state of knowledge on these precipitation sub-processes (ie. growth, nucleation and agglomeration) and describes a number of experimental techniques for estimating their kinetics. The experimental methods used to generate the precipitation data and the data analysis techniques used to extract the kinetics information from the data are discussed separately. There is no universal "best" technique for determining the kinetics. However, studies on multi-crystal systems are more reliable for modelling purposes than are single crystal studies. The selection of a technique will depend on which sub-processes are present. A problem with all kinetics studies is that there is generally a large uncertainty in the estimated kinetic parameters. This stems from the scatter in the experimental data being further propagated by the mathematical techniques used to extract the kinetic parameters.

Jan 1, 1996

By Musa Karakus

Reflected light microscopic (RLM) examination of dust particles from lead and copper smelters can effectively characterize their mineralogy, texture, and origin. Scanning electron microscopic-energy dispersive spectroscopic (SEM-EDS) analysis provides confirmation of the optical identifications and chemical data on the phases. Studied lead smelter dust samples were from the: I) blast furnace, 2) sinter plant scrubber, 3) sinter plant crusher, 4) dross furnace, and 5) refinery. Phases identified included galena fragments, melted PbS, metallic Pb and Cu, Cu-Ni, Cu-Zn, Zn-Ag, Zn-Cu-Ag, Ni-Cu-Sb, and Ni-Cu-Zn-Ag metal alloys, Ni-sulfide, Cu-sulfide, and Cu-Pb-sulfide dross .phases; slag and sinter particles, coke fragments, unreacted original feed phases: pyrite, chalcopyrite, sphalerite, siegenite, bravoite; and oxidized particles: iss, bornite, chalcocite, covellite, magnetite, hematite, and goethite. Dust from a secondary copper refinery were found by RLM and SEM to consist of tenorite, cuprite, cassiterite, two silicate phases. Magnetite, hematite, Fe-Al-Cr-Mg spinel, periclase, forsterite, and wollastonite were derived from the furnace linings during initial cleaning.

Jan 1, 1992

By G. L. Hundley, D. N. Nilsen

The U.S. Department of Energy investigated the use of liquid-emulsion membranes (LEM) for the selective removal and recovery of metals such as copper and zinc from mine waste waters. This investigation included field tests of a mobile, pilot plant-scale, continuous-flow LEM system. The system was tested at copper mines with solutions containing from 100 to 1,400 ppm Cu, and at a zinc mine with a solution containing 115 ppm Zn. Typical results from the copper tests were >90% copper recovery, and zinc extraction from waste water also was typically>90%. Although all of these waste waters contained high impurity levels, pure products were produced. On several of these field tests, integrated systems were tested that resulted in recovery of metal by-products, selectiv~ precipitation of iron, and polishing to reach discharge targets for essentially all of the contained metals. In addition, some results are included from laboratory-scale tests.

Jan 1, 2000

By B. Madelin

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

Jan 1, 1990

By A. V. Reddy, C. Beckermann

"The DC continuous casting of a grain refined AI-4.5%Cu round ingot with realistic boundary conditions is numerically simulated. Of particular interest are the effects of the transport of free solid in the form of equiaxed grains on the macro segregation patterns and the final grain size distribution. The study uses a previously developed two-phase model that incorporates descriptions of heat transfer, solute redistribution, melt convection, and solid transport on the system scale with microscopic models of solutal undercooling, microsegregation and grain impingement. The numerical results indicate that grain transport inhibits the formation of inverse segregation in the ingot shell and promotes negative centerline segregation. This is explained by the reduction in the solid coherency next to the mold and the advection of solute-lean grains towards the centerline. Comparisons with the experiments of Finn et al. [5] illustrate the need for considerable improvements in the model. IntroductionMacrosegregation continues to be one of the concerns in DC continuous casting of aluminum ingots. The variation in composition over the ingot cross section results in the need to adjust alloy composition in order to meet mechanical property specifications in finished products. The extent of macrosegregation is greatly affected by the casting conditions, such as casting speed, superheat, cooling rate, mold size, alloy composition, and grain refining practices. Thus, it is of great interest to develop a comprehensive mathematical model to simulate the casting process, enabling the selection of conditions that minimize macrosegregation while maintaining a high productivity."

Jan 1, 1994

By Takeshi Nagano

Copper pyrometallurgy in Japan has experienced quite fundamental changes in last fifteen years. The severe environmental restriction coupled with increase of energy costs accelerated the development work of the new continuous process in Mitsubishi Metal Corporation. After several years of pilot plant test work the commercial plant was put into operation at Naoshima Smelter in 1974, the design capacity of which was 4,000 tonnes of copper per month. Many modifications and improvements have been incorporated into the process and 7,200 tonnes per month of copper production was achieved in 1983, proving that continuous process was much more economical than conventional process. It is now possible to design and operate the continuous process in wide range of capacity. This paper will review the process and describe the progress of the process in these 10 years. 311

Jan 1, 1985

By S. Sugiyama, M. Kiuchi

"New metal working processes, such as the mashy-state mixing, mashy-state forging, mashy-state rolling and mashy-state extrusion are developed and applied to manufacture the so-called particle reinforced metals, fiber reinforced metals, particle reinforced cladding metals and so forth. These metal-ceramics composites are made of metal sheets, metal powders, ceramics particles and ceramics fibers. The mashy-state processes are also used to work those composites into bars, wires, tubes, plates, sheets, machine parts and other products. The working conditions necessary to manufacture sound composite products are clarified and the mechanical properties of the products are investigated. Through the investigation, it becomes clear that the mashy-state processes are useful and effective to manufacture metal-ceramics composites. It is al so known that these processes may be applied in various ways to development of new metal matrix compounds. IntroductionThe so-called metal-ceramics composites and processes to manufacture them are now being widely investigated in order to comply with increasing demands for new materials with novel and excellent mechanical properties and functions. The metal-ceramics composites are expected to have superior characteristics with respect to the elastic modulus, hardness, anti-wear resistance, high temperature strength and other mechanical properties to those of conventional metallic materials.The present authors ha v e been investigating into new metal working processes which are based upon the characteristics of metals and their alloys in the mashy-state. In the mashy-state, the metal (or alloy) includes both of the solid and liquid components. According to the fact that the partial melting takes place and the liquid component usually exists at grain boundaries, the metal in the mashy-state has quite different mechanical properties from those of the metal in the solid-state. Because of that the bonding force among grains is very weak due to the partial melting occurred at grain boundaries, the mashy metal has distinctively low flow-stress and high deformability. The mashy metal splits into grains or particles and sticks to others very easily. It is so soft as to be stirred up just like a lump of sherbet, but it is sufficiently viscous to be mixed up with other materials, such as ceramics particles and ceramics short-cut fibers."

Jan 1, 1988

By Yanlong Li, Lifeng Zhang, Ying Ren

In this work, a multiphase mathematical model for the fluid flow in argon-stirred steel ladles was established and validated by experimental measurement of wood's metal. Alloy dispersion in the molten steel was calculated. The melting and mixing of alloy was faster with smaller size of the alloy particles, larger superheat and bigger slip velocity. The current mixing time is approximately 300 s with 30 mm alloy diameter and 91.5 K superheat.

Jan 1, 2014

By J. L. Johnson

Remediation of small-arms firing ranges is being investigated by the Naval Civil Engineering Laboratory and the U.S. Bureau of Mines. Scheduled closures of military installations, as well as the management of active ranges, require the development of methodologies for heavy metals removal to prevent their entering the surrounding environment. The impact berms contain high concentrations of metals, and the soil and vegetation surrounding the berms were found to have slightly elevated levels. The heavy metals characterized are in the form of whole bullets, a wide size distribution of free fragments, smeared lead on the surface of the soil grains, and very finely attached particles. Gravity beneficiation can remove liberated metal contamination effectively. Weak acetic acid leaching shows promise in lowering the final metal contamination to allow the soil to pass the Environmental Protection Agency's (EPA) Toxicity Characteristic Leaching Procedure (TCLP) criteria.

Jan 1, 1991

By Bart Blanpain, Muxing Guo, Zhuangzhuang Liu

In order to stabilize free lime in the basic oxygen furnace (BOF) slag to achieve high value products, quartz sand and other additives are injected into slag. However, the current hot stage slag stabilization does not work in case of slag (before treatment) with a liquid fraction lower than 90%, where the slag containing solid particles is too viscous. Therefore, it is essential to understand how solid phases affect the viscosity of the slag system. In this study, the industrial BOF slags were investigated with respect to the correlation between volume fraction of solid phases and its viscosity. Slag viscosity was measured with a rotating type viscometer at temperatures below the liquidus. The volume fraction of solid phases was quantitatively calculated with FactSage. The Einstein-Roscoe equation was employed to predict the viscosity of BOF slag.

Jan 1, 2016

By T. Innmi

The potential of the nickel matte anode was measured during the matte electrolysis in the commercial cell. The slime layer consists of elemental sulfur and was found to greatly influence the potential of anode. The measurements of porosity and permeability of the slime suggest that the voltage drop of the slime layer dominates the potential. Furthermore, the diffusion of the electrolyte through the slime layer is also one of the factors to determine the potential. In addition, the copper content of the nickel matte anode was found to affect the change in the anode potential during the electrolysis. The role of copper on the anodic dissolution of nickel matte is discussed in this work.

Jan 1, 1988

By Jay R. Hitchings

A technique that enables excellent color photograph production from black and white negatives of electron microprobe x-ray images is described in this paper. The photographs are made by superimposing one, two or three negatives of black and white x-ray images individually through assigned primary color filters directly onto color print paper. When used to examine metallurgical or geological microstructures, the resulting color photograph provides detailed, qualitative information about spatial arrangements, elemental associations and relative concentrations of at least three elements. The technique is simple and straightforward, requiring only standard darkroom equipment. The use of color to display or present complicated microprobe data also allows a non-technical reader or audience to better understand the data.

Jan 1, 1981

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

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

Jan 1, 2000

By Colin Dessemond

Since 1950, the traditional process has been dominating the production of lithium compounds from spodumene ores to sustain the lithium market because of its economic viability and the markets need for technical grade (99.5% purity) product. This traditional process includes thermal conversion, acid roasting and lithium leaching. However, this process has not been challenged and very few studies have tried to explain its limitation (95% lithium yield) or optimize the thermal treatment. Here, α to β spodumene conversion and lithium extraction were performed in a rotary kiln on a 2 mm to 2 cm spodumene concentrate instead of a micrometric one using a 1050 °C, 30 min conversion treatment and 250 °C, 30 min, 30% H2SO4 excess leaching treatment. X-Ray Diffraction analyses were performed on the converted material to determine the conversion rate by Rietveld analysis. It was observed after thermal treatment that the α-spodumene particles fractured and divided while the impurities remained compact. A sifting was performed after thermal treatment and it was determined that 65% of the initial mass became finer than 180 μm. X-Ray diffraction analyses and lithium content measurement were performed on both fractions and it was determined that the finer fraction had a very high lithium content of 3.24 wt%. Lithium extractions were performed on both fractions separately. While the coarser fraction’s lithium yield was only 61% the finer fraction’s lithium yield went up to 99% without any additional treatment. These observations may open more economical ways for the traditional process by potentially bypassing two third of costly steps such as grinding.

By J. H. Ahn, J. K. Yoon, Jung-Eui Lee

"A concentration change during grade transition operation in steel thin slab casting is predicted with computer simulation, water model and plant trial. Fluid flow and mixing patterns in various tundish levels and flow rates were analyzed through three-dimensional mathematical modeling. Comparing with water model experiments, a simple, efficient and accurate computational model has been suggested to predict the concentration profile at outlet of tundish. Based on the model, mixing in/below the mold was analyzed considering EMBR. The predicted concentration profiles show good agreements with the measured values. It is found that the lower vortices in the mold are suppressed by the electromagnetic field and the plug-like flow region develops which decreases the intermixing of two different grades of steel and shortens the length of transition region.1. IntroductionContinuous casting is the primary mode of production of semifinished steel products as it offers tremendous advantages in terms of energy savings, increased yield and higher productivity over the traditional ingot casting process. Efforts have to be made constantly to improve the quality of the cast product, reduce costs and thus increase the competitiveness of the steel manufacturer. One way of reducing costs is to reduce the amount of intermixed steel during the grade transition operation.Several different procedures exist to handle the casting of dissimilar grades for the conventional slab casting. Each procedure has its own merits and demerits. In order to choose the best method for a particular operation, there are a lot of researches. In the case of present continuous thin slab casting of POSCO mini mill, the only possible method is to change ladle during the grade transition. Due to the high casting speed (3.8m/min-4.4m/min) it is impossible to change the tundish and due to the thin thickness of slab it is also impossible to insert grade separator."

Jan 1, 2000