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By Raghavan Srinivasan, Y. V. R. K. Prasad, William G. Frazier, Steve C. Medeiros

"Aerospace gas turbine disks operate in an environment of relatively high stresses caused by centrifugal forces and elevated temperatures. These severe conditions necessitate the need for materials with good high temperature strength and low cycle fatigue resistance. One class of alloys used for this task is the nickel base superalloys, out of which, lN 718 is the most widely used in the aerospace industry [I]. The properties of IN 718 are attributed to the combined effects of the chemistry, heat treatment, and microstructure. The chemistry is tailored not only for solid solution strengthening but also for precipitation hardening developed during heat treatment, which combined with a fine grained microstructure lead to excellent mechanical properties such as low cycle fatigue resistance and elevated temperature strength. The properties of a gas turbine disk are sensitive to the microstructure, in particular the grain size, which is dependent on the processing history. The ability to precisely control the microstructural development during forging is dependent on controlling the process so that the workpiece is deformed within a ""safe"" region where no microstructural damage or flow instabilities occur. The microstructural mechanisms during deformation may themselves vary within the ""safe"" region and it is desirable to determine them within the range of parameters that are commonly used in industrial processing. The objective of this work is to establish a relationship between the grain size and the process control parameters i.e., temperature and strain rate, in the hot working of IN 178.BackgroundIN 718 belongs to a class of nickel-iron base superalloys with a face-centered cubic (FCC) austenitic matrix strengthened by precipitation of ordered intermetallic or carbide precipitates and is a nickel-rich alloy strengthened by ordered body centered tetragonal (BCT) precipitates, Y"". The alloying of nickel and iron results in the formation of the austenitic matrix, y, while the addition of chromium and molybdenum cause solid solution strengthening. Also, alloying with niobium causes precipitation of the metastable hardening constituent Y"" (Ni3(Nb,Ti)). Extended aging treatments in the temperature range 650 °C - 980 °C allow the more stable orthorhombic 8 phase (Ni3Nb) to form. Trace amounts of boron are also added to serve as grain boundary strengtheners for high temperature creep resistance. Hot deformation of IN 718 is performed between the Y"" and 8 solvus temperatures to facilitate recrystallization and to control grain growth. While deformation below the Y"" solvus (""""962°C) produces no change in grain size, deformation above the Y"" solvus but below the 8 solvus will lead to a dynamically recrystallized microstructure. The presence of the 8 precipitates will pin the grain boundaries after recrystallization and restrict grain growth so that a fine grain microstructure is obtained. Deformation above the 8 solvus ("""" 1038°C) will lead to a microstructure which has undergone grain growth during deformation."

Jan 1, 2000

By Juliana G. Gutierrez-Paredes, Gabriel Plascencia-Barrera, Fidel Reyes-Carmona

In Mexico, many tonnes of nickel from waste petrochemical catalysts are dumped every year. In order to recover all that nickel, a hydrometallurgical reactor was designed. This design was performed in a systematical fashion, which included the chemistry of the system under study, both a kinetic and mass transfer study, and finally the use of the RID function, to optimize the reactor size. It was found that the NiO leaching with sulfuric acid is well represented by a first order reaction. The mass transfer results are in good agreement with the experimental results, obtaining over 95% nickel extraction in both cases. A marketing study was also completed that determined that it is possible to make a good profit by processing this residue provided the capital cost was low.

Jan 1, 2000

By Nobuo Kikumoto

Recently, the treatment of industrial waste materials has been a serious social problem here in Japan. Filling them in ponds is now strictly prohibited due to a limited land area and incineration method is also regulated as not to generate DXN. In these conditions, Onahama Smelter has begun to treat shredder dusts (SD) of car at reverberatory furnaces to recover various metals such as copper, gold, silver and palladium without generation of DXN. The total volume of these dusts is expected more than 1 million metric tonnes a year in Japan. Onahama Smelter is now planning to treat about 20% of them in the near future by using tonnage oxygen. In this paper, the heat balance, control method of DXN and treatment of these dusts in reverberatory furnaces are described. DXN : Dioxin (The generic term of PCDD and PCDF)

Jan 1, 2000

By V. M. Sokolov, Jr. DuPlessis

The technology for recycling fine wastes, grinding sludges or swarf, and solids such as slag that contain a high content of metallic material needed improving. The objective was to produce a master alloy that met the tight requirements of the Western manufacturers and achieve improved yields of the valuable elements, nickel and cobalt, to over 90%. The alloys from the production of Alnico. magnets were chosen for this work. A process is proposed .that is able to recycle all kinds of Alnico wastes. This process is able to reduce all detrimental elements, which are contained in the wastes, to within acceptable levels. Molybdenum, if present, is an exception. Depending on the levels of contamination of undesirable elements different recycling strategies are proposed. The majority of the wastes can be recycled by melting and refining with a liquid slag layer using unique melting furnaces that are relatively unknown in Western nations. The proposed technologies allow the reelamation of over 95% of the cobalt and nickel from any kind of Alnico waste, and there are no limitations on the proportion of different kinds of wastes in the charge. The proposed processes and technologies could also be applied to the recycling of grindings, turnin

Jan 1, 2000

By D. Silva-Galvan, R. D. Morales, S. Gonzáelez-López, A. Romero-Serrano, G. Plascencia-Barrera, F. Chavez-Alcala

This work is focussed on lead decopperising by two techniques: conventional top addition of sulfur and injection of sulfur powder. It is found that the first method proceeds under equilibrium conditions and the second one depends on kinetic considerations. Experiments were carried out using 15 kg lead baths at two temperatures, 340°C and 380°C. The carrying gas used for the injection trials was nitrogen at flow rates of 6.3 and 18.6 L min- 1• The results show that 'decopperising process is more efficient at temperatures close to the melting point of lead for the sulfur top addition process, whereas high temperatures produce better copper removal for the injection of sulfur powder. Besides, the sulfur injection with the higher nitrogen flow rate (18.6 L min-1) produced higher decopperising rates. Thermodynamic and kinetic models are used to simulate this lead refining process.

Jan 1, 2000

By Li Yuhai

Kinetics of non-isothermal precipitate process and crystal growth of perovskite (CaO ? Ti02) phase in CaO-TiOz-Si02-AlP3-MgO system were studied. The experimental results show that the relative volume fraction can be described by the equation given by K. Matusita et at. and the experiential expression of average crystal radius was obtained. The particle coarsening in non-isothermal process has important effects on the crystal growth of perovskite phase.

Jan 1, 2000

By Masahiro Sasaki, Wu Kepeng, Chang-Yong. Kang, Kohji Okada, Naohiro Igata, Kazuya Miyahara

"The damping capacity of the Fe-12 mass % Cr-6 to 30 mass % Mn alloys has been investigated. Particularly the effects of microstrucutre composed of the phases of a , a ' , y , and e on the damping capacity have been clarified. Various fraction of these phases were formed depending on the Mn content and cold work degree. The combination of 22 mass % Mn and 50% cold rolling formed the largest volume fraction of e martensite and showed the highest damping capacity. The other phases of a, a' and y had very small effect on the increasing of damping capacity.IntroductionFe-Mn alloys are known to be one of the high damping capacity materials [l-3]. In the present research, the damping capacity of the Fe-12 mass % Cr-6 to 30 mass % Mn alloys, in which 12% Cr is added for the improvement of corrosion resistance of the Fe-Mn alloys, has been investigated. Particularly the effects of microstrucutre composed of various phases of a (bee), a ' (bet martensite), y (fee), and e (hcp martensite) on the damping capacity have been clarified. The results of preliminary research on Fe-Cr-Mn alloys are reported by Igata et al. [4] Various volume fraction of these phases were formed depending on the Mn content and cold work degree. The combination of 22 % Mn and 50% cold rolling formed the largest fraction of e martensite and the measurement indicated clearly that e martensite had the largest effect on the damping capacity. The other phases of a ' y and a I had very small effect on the increasing of damping capacity."

Jan 1, 2000

By S. S. Chabot, S. E. James

A recent survey of CEOs from major steel companies worldwide revealed the importance of recycling zinc units from EAF dust, mill scale, blast furnace dust, and other zinc containing streams in their plants. Many processes were developed and installed in response to this challenge. The most successful approach involves the production of a crude zinc oxide and selling it to primary zinc producers to recover the metal value. The problem with this process is the high concentration of halides in the crude oxide. This type of material cannot be processed directly in an electrolytic zinc plant because of corrosion problems it will cause in electrolysis. In 1999, BRZ installed a zinc oxide receiving and washing plant to minimize the impact of halides to its circuit. A description of the washing plant and initial operating results are included.

Jan 1, 2000

By S. Subhawong

Following the startup of the zinc plant in Clarksville, Tennessee, in 1978, the original effluent treatment plant did not perform as designed. The sludge, produced in a conventional lime neutralization treatment, settled poorly and began to fill the permitted lined impoundment within two years, well short of the original design capacity. Another sludge pond had to be constructed. This led to a new process modification of the original design. Although the design is still based on the conventional lime precipitation of heavy metals, the current effluent treatment plant has evolved into a hydrometallurgical circuit, capable of producing good quality water without generating sludge. Undesirable elements are bled from the zinc circuit and are rejected through the effluent treatment operations. Wallboard grade gypsum is produced, instead of sludge, and all the gypsum is sold to cement and wallboard plants. This operation also recovers and returns more than 1,500 tonnes of zinc annually to the 105,000 tonne/y zinc plant.

Jan 1, 2000

By Satoshi Yamashita, Noboru Masuko

"Newly prepared bipolar membrane is promising to become a key material of an electrolyser for a production process of strong reducing solvent. This research is basic research for using bipolar membranes as electrolysers of reducing agents, Cr(II), TI(III) and V (II) on the laboratory scale. In this report, a bipolar membrane was tried with an electrolyser, reducing chromic chloride to chromous chloride. An analysis of mass balance demonstrates advantages of it over the former electrolyser equipped with an anion and/or. cation exchange membrane. The effects of current density and concentration of Cr(lll) on the reduction rate of Cr(II) and the current efficiency were examined No deterioration of the bipolar membrane resulted from the electrolytic reduction of Cr(III). IntroductionRecently, bipolar membrane that was the development subject for a long time in the industry of ion exchange membranes has met the stage of the practical application at last [l]. The expectation of the application to the hydrometallurgy field increases. We took up the manufacturing of the strong reducibility solvent as part of the application of bipolar membrane to hydrometallurgy technology. This laboratory has much experience in the electrolytic reduction of Cr (II) aqueous .solution such as chromous sulfateusing bipolar membrane were compared in theory to chromous chloride aqueous solution manufacturing of the strong reducibility solvent. The advantage of applying bipolar membrane by substituting ion exchange membrane is described, and the experimental result is reported."

Jan 1, 2000

By C. F. Ferron

A process has been developed to treat the copper gold ores from the Guelb Moghrein mine in Mauritania. The process consists of pressure leaching the sulphide concentrate, neutralising with the oxide ore, recovery of copper by SX/EW and of gold by cyanidation of the autoclave residue. This paper focuses on the pressure leaching step, and presents data from bench and pilot plant test programs. In particular, attention is drawn to the effects of temperature, grind size, neutralisation, retention time and solution recycle on the kinetics of copper dissolution from various flotation concentrates. Likely leach mechanisms are briefly discussed.

Jan 1, 2000

By J. N. Hryn, E. J. Daniels, M. Askew, Kirchner. G.

This presentation addresses the changing regulatory climate towards aluminum dross and salt cake in Europe and in the United States. Although sporadic, the trend in the U.S. continues to be away from command-and-control regulation of these materials. This trend began in the early 1980s when the Environmental Protection Agency was successfully sued in court and prevented from classifying dross as a hazardous material. The situation in Europe is different. Because of Council Directive 96/61/EC from the European Commission, European Union member countries have all passed legislation that will essentially cause all salt cake and drosses to be reprocessed. The implementation date of the legislation varies from country to country: from 2001 in the United Kingdom to 2007 in Germany, France, Austria, Italy, and Spain. The European aluminum industry is urging the EC to use the approach adopted by the U.S. EPA, which declassifies the majority of aluminum drosses and salt cakes.

Jan 1, 2000

By Bingchen Chen, Zhitong Sui, Junwei Ma

"In the blast furnace slag, titanium disseminated in various mineral phases Titanium could be concentrated mainly in perovskite, which could be selectively precipitated and grown by optimizing the operation factors like the slag composition, temperature of heat treatment and additive agents. This study aims at establishing the titanium slag mineralogy and its distribution in the treated slag and the as-received slag, as well as the methods of perovskite separation. After heat treatment, the grain size was grown from 5 - 20µm to 80 - 200µm, the distribution of Ti02 in perovskite was increased from 48% to 81 %, the morphology was changed from snow-shaped grain to coarsening dendrites or equiaxed crystals. A concentrate were produced by gravity separation analyzing 35.25% Ti02 with a recovery of 68.28% and a tailing analyzing 9.53% Ti02 , and a possibility of flotation upgrading was discussed. I INTRODUCTION CHINA is rich in mineral resources of titanium, 92.4% of which is vanadium-titanium bearing magnetite. About 53% titanium were in iron concentrate after mineral processing, by which the blast furnace slag containing about 25% TiO2 were produced[11 • The content of TiO2 in such slag is too low to separate titanium dioxide, and it is also too high to produce slag cement[21. It has been accumulated to 50 million tons so far, which is still increasing at a rate of 3 million tons per year, and results in a waste of titanium resources and pollution of environment. Due to the dispersed distribution of titanium component in various mineral phases, very fine grain(<10µm) and complex interfacial combination, it is very difficult to recovery titanium component from the slag by traditional separating technique. In this paper, a novel technique to recovery titanium from the waste slags was proposed [3H4l, on which three continuous processes were involved: selective concentrating, selective growing and selective separating. Perovskite was designed as a titanium-rich phase, in which the most titanium was concentrated promptly, then perovskite could be selectively grown and coarsened by optimizing the heat treatment and the appropriate additives [ 5l[6l. The grain size of perovskite phase was larger than 80 µm, and the crystals appeared as coarsening dendrites or equiaxial grains like lump."

Jan 1, 2000

By Toshio Suzuki, Machiko Ode, Won Tae Kim, Seong Gyoon Kim

"The Ostwald ripening and growth and coarsening of the secondary dendrite arm are studied using a phase-field model. The phase-field parameters are obtained at a thin interface limit proposed by Kim et al. In Ostwald ripening analysis, the difference of the concentration due ·to· the curvature effect is shown. The third power of the average particle radius Rav is proportional to time and the ripening constant shows a good agreement with the value by Deppers et al. The particle radii distribution shows the transition behavior to attain a self-similar stationary shape. The growth and coarsening behavior of the secondary dendrite arm is also analyzed using a phase-field model. The estimated arm spacing and its dependence on time are in good agreements with experimental data.IntroductionThe ripening or coarsening process controls the microstructure during the late stage of solidification. The ripening phenomena are recognized firstly by the Ostwald [1]. The first quantitative analysis for the Ostwald ripening in the limit of vanishing solid fraction was provided by Lifshitz, Slyozov and Wagner (LSW) [2,3]. In their study, that the mean radius grows proportional to the cubic root of time and the size distribution of precipitations shows a ""self-similar"" shape are shown. Most of the studies for the Ostwald ripening confirm or predict these two general rules above. In case of finite solid fraction, the general rules are observed but the ripening constant is larger and the self-similar shape is wider than the LSW prediction respectively [4-6]. To analyze· the high solid fraction system, the theories that consider the solute field correlation are proposed [4,7-8]. In the theory, however, since the particle is treated as the point, the effect of the concentration field deviation from the monopole field should be taken into account. Recently the numerical simulation, in which not only diffusive transportation of solute but also convection effect is considered, has been done using a phase-field model [9]."

Jan 1, 2000

By Yu. A. Grinin, Yu. A. Sannikov, M. A. Lyamina, V. A. Shumskij, L. V. Slobodkin, N. N. Ushakov

This manuscript describes the Kivcet treatment of lead-bearing materials having high contents of copper and zinc. The tests were carried out on bulk concentrates from the Zyrianovsk Mining and Concentrating complex, "Kazzinc" JSC (Kazakhstan) with the following composition: Pb 37.6%, Cu 10.4% and Zn 6.8%. Two properties of the concentrate were under investigation: their calorific value and their desulphurization rate. By adding flux, the charge properties were brought close to the properties of high-grade lead sulphide concentrate. The charge was melted with high productivity. To ensure high copper recovery, Waelz residue was added to the charge. The residue contained more than 20% carbon and about 30% iron metal. The residue was partially replaced by coke that facilitates high copper recovery into the matte. The smelting achieved a production rate of 20 t/h with one burner. Lead recovery into the lead bullion was 88.8%; copper recovery into matte was 92.3%; zinc recovery into slag was 75.5%; and zinc recovery into the fume was 5.1%.

Jan 1, 2000

By Mahmoud A. Rabah

"In this work, metal values were prepared from used beverage cans. The cans are made of aluminum and minor alloying metals and printed with a multi-color printing ink. A method has been investigated to remove the printed coating using organic solvents or by sand blasting technique in a rotating drum. Metal values of the cleaned cans are prepared applying combined hydro and pyrometallurgical treatments. Factors affecting the efficiency of the suggested method have been studied.The results show that the extent of removal of the printing coating is successfully performed with recyclable methyl ethyl ketone I dimethyl formarnide mixture. With sand blasting, it proceeds regularly with the inner diameter, the rotation speed of the drum, the size of the sand grains and temperature. The removed coating is stripped with the same solvent. Metal alloy(s) are prepared in two ways. In the first way, the cans are pressed into solid blocks using hydraulic press before melting at temperatures up to 1000°C using borax-sodium chloride salt mixture as a flux. The quality of the metal obtained is a function of the salt and temperature. The slag so formed was leached with mineral acid solutions. In the second way, the used beverage cans are directly dissolved in mineral acids whereby different metal values are selectively precipitated. The undissolved part is fused with sodium carbonate at 800°C and processed in the same manner. Results were explained in the light of the thermodynamic properties of the species involved."

Jan 1, 2000

By Kazuyuki Kakegawa

"Sintered body of lead zirconate titanate (PZT) was prepared through the spark plasma sintering (SPS) technique. When the mixture of raw materials was calcined at 800°C and sintered at 900°C for 10 min. with SPS technique, the sintered body had almost theoretical density but was a mixture of lead titanate (PT) and PZT. When a calcining temperature of 1100°C was employed, sintered body had a single PZT phase but a lower density. High dielectric constant was obtained for a sample calcined at 800°C, sintered with SPS tecbriique and fired again in the air at 1100°C.IntroductionSpark plasma sintering (SPS) is a recently developed technique for sintering metals and ceramics1. The scheme of SPS is shown in Fig. 1. Sample is put in a graphite die in a vacuum chamber. It is pressed and pulse voltage is applied. The electric current heats the die. It is said that the pulse causes a spark-plasma between particles in the sample. Because of the spark- plasma, sample can be sintered at temperatures lower than that in the ordinary sintering by several hundred degrees of Celsius. The sintering period is also very short2Low sintering temperature and short sintering period in SPS technique cause low reaction rate. It is both disadvantage and advantage. In some cases, the reaction cannot be completed under the SPS conditions. If a mixture of several compositions having different properties can be sintered without a compositional change by the diffusion during the sintering, combination of properties, and therefore a design of property will be possible3. The low reaction rate of SPS may enable such combination."

Jan 1, 2000

By M. A. Barakat

Large amounts of zinc ash and flue dust containing more than 80 % zinc are accumulated during galvanization processes at the surface of molten zinc bath and in the chimney respectively. Pyrometallurgical recovery of zinc from both of the ash and dust samples has been carried out. The ash was sieved with the help of an industrial sieve shaker provided with mesh sieve having a pore size 0.9 mm. The oversize fraction cut (+ 0.9 mm) was melted at 550 °C under ambient conditions. The produced ingot (1) was analyzed whereas the coarse fraction of the produced slag (+ 0.9 mm) was treated as the coarse ash or added to it. The dust was enriched with suitable fluxing salt prior to heat treatment at 600 °C for 1 h. The produced ingot (2) was analyzed whereas the resulting slag was mixed with the fines of the ash and treated by hydrometallurgical processing to prepare valuable salts of zinc. Parameters affecting recovery processes such as time, temperature and flux percentage were studied. Results obtained revealed that the two prepared ingots (1&2) were successfully recovered with recovery efficiency amounts to =85 %. The obtained samples meet the standard specifications with relatively low price. Also in the light of the strict environmental regulations of pollution control, reuse of these wastes materials will help in keeping the environment clean.

Jan 1, 2000

By N. Menad

. Electronic wastes are heterogeneous mixture, with mainly copper, aluminium and steel attached to or mixed with various types of plastics and ceramics. In general, small amounts of precious metals are incorporated in this mixture. Today, these components constitute an environmentally problematic fraction in disposal. Their physico-chemical characteristics have been investigated through chemical, x-ray diffraction, infrared spectroscopy, scanning electron microscopy and thermal analysis.

Jan 1, 2000

By S. Ferlay

"The main purpose of the ZIMA VAL project (Label EUREKA EU1367 and LIFE ENV/F/000278) is to demonstrate industrial scale recovery and recycling of the main components of used dry batteries (zinc, manganese dioxide, mercury, and stainless steel) into high added value products. The originality of the ZIMA VAL process resides in:1- the use of hydrometallurgy2- alkaline treatment implementation (highly selective) for zinc and mercury3- electrochemical recovery of high quality products.4- the recycling of all the battery components (zinc, mercury, manganese dioxide, stainless steel) ·5- low operating and investment costs.The process consists of physical classification, mechanical dismantling, hydrometallurgy and electrochemistry. The purpose of the demonstration plant in FALAISE (Calvados - France) is to define the technical and technological parameters of an industrial unit for the treatment of 2400 tonnes per year of used batteries."

Jan 1, 2000