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By Dany Racine, Daniel Marceau, Denis Laroche, Dmitry Lukovnikov

Carbon base materials play a critical role in the performance of Hall-Héroult cell. The determination of their thermo-physical properties is of primary importance for modeling and designing complete cell systems. However, overcoming the associated experimental hurdles is complex and often underestimated. Of them are the Poisson’s ratio measurements and the continuous oxidation/burning of the materials at temperatures above 200°C. The novel procedure developed in this research is based on the Gleeble® 3800 system. Its vacuum chamber allows test with a chosen atmosphere at temperature of more than 1000°C. Young’s modulus, Poisson’s ratio and the coefficient of thermal expansion values can all be adequately measured using a single test. Cylindrical carbon samples (: 50mm, L: 100mm) were tested in the modified system at temperatures ranging from room to 950°C without any trace of oxidation. The resulting values were also in good agreement with literature data for a specific graphite material.

Jan 1, 2015

By Jafar Safarian

Bauxite is the main raw material used for the production of alumina (Al2O3) through the well-known commercial Bayer process. This process has significant challenges such as limitation in using low-grade bauxites as they contain significant amounts of impurities such as Fe, Si, Ti. The Bayer process residue, which is known as red mud, is also a global environmental challenge due to huge amount of this low value residue production. An alternative sustainable process with high potential to solve these problems and produce valuable and consumable by-products is a pyrometallurgical-hydrometallurgical process in which the low-grade bauxite ore is treated through a smelting-reduction process, yielding iron alloys and a calcium-aluminate slag. Alumina is then produced from the slag by hydrometallurgical treatment. In the present work, the reduction of pellets produced from different bauxite ores by hydrogen is studied and it is shown that complete iron oxides reduction is possible. Further smelting and smelting-aluminothermic reduction of the reduced pellets show that iron and silicon ferroalloys can be produced, in addition to a proper slag for alumina extraction.

By Günter Petzow, Hans Leo Lukas, Hans Jürgen Seifert

"The CALPHAD method (CALculation of PHAse Diagrams) has been extensively developed in the last 25 years and became a useful tool in materials science. Thermodynamic descriptions for the functions of state of unary, binary and ternary phases are derived by the optimization of phase diagrams. These functions are stored in computerized thermochemical databases and can be combined to extrapolate to multi component systems. Depending on special demand, the actually most advantagous presentations of the calculated results can be chosen: tables or in a clear graphical form as phase diagrams, phase amount diagrams or volatility diagrams. The method will be desribed by the system Ti-Si-C-N-O including the ceramic subsystem Si3N4-SiC-TiCi,N1_1,-C-N-O which is very important for the development of ceramic composites. The calculations give the thermodynamic stabilities of the condensed phases as function of temperature, concentration and partial pressure of different gas species. Adjusting the sintering conditions to these results the formation of unfavourable compounds or liquid phases can be suppressed.IntroductionThe CALculation of PHAse Diagrams (CALPHAD-method) of multicomponent systems provides the possibility to plan experiments very efficiently and avoid the experimental trial and error approach for the development of materials. The main problem for best use of calculated results is their interpretation with regard to the specific applications under consideration. Tables give the exact quantitative data for the treated phenomena. However, most important to make best use of these thermodynamic data is their graphical representation especially designed for the solution of specific problems, scientific as well as application oriented. Only well chosen graphical representations support a comprehensive understanding of the thermodynamic interrelationships and the transfer to the problem."

Jan 1, 1996

By P. R. Taylor

Diamond films have been successfully formed in an inductively coupled plasma (ICP) chemical vapor deposition (CVD) system from several gas mixtures: CH,-H,, C2112-112, and C2112-112-02' Our previous thermodynamic study indicated that the substrate temperature could be lowered by the presence of oxygen species at moderate system pressures (0.3-0.5 atm) and that higher volumetric growth rates required a high temperature source and a moderate pressure system in CVD processing. The principal experimental results were consistent with the thermodynamic predictions. The deposited films were characterized by laser Raman spectroscopy, scanning electron microscopy, and X-ray diffraction. The films were well faceted and uniform, with the growth rates over 10 pm/hr on molybdenum substrates. The crystal size ranged between 1 and 2 microns for a two hour experiment. It was possible to decrease the substrate temperature to below 800 °C in this system.

Jan 1, 1995

By John P. Hager

One possible approach for the recovery of mercury from acid plant blow-down sludge in smelters is the use of a vacuum retort reactor for the vaporization of the mercury with subsequent collection of metallic mercury in an attached condenser. An experimental study was undertaken to investigate the vaporization of mercury when present as a compound in the Hg-S-O and Hg-Se systems. A transpiration reactor was modified to operate under reduced pressure and with a continuous flow of inert sweep gas. A water-cooled cold finger was inserted into the exit end of the reactor to provide for the rapid quenching of the exit gases and the collection of the mercury. Rates of vaporization were measured at several temperatures for each compound and were generally found to be constant at a given temperature and reactor pressure. The results were used to determine the minimum operating temperature for 100% vaporization of the compound in 60 minutes. For Hg2SO4, HgSO4, and HgSO/2HgO the required temperatures. for a reactor pressure of 50 Torr. were determined to be 634°, 622°. and 603°C. respectively. For HgO, HgSe, and HgS the required temperatures were 557°. 451°. And 382°C. respectively. For HgS the rate of vaporization was also measured at a reactor pressure of 1 00 Torr. The rate of vaporization was found to be slower resulting in an increased vaporization temperature of 423°C. It was also determined that the mercury vapor present in the exit gas stream can back-react with the other gas species to a significant extent and can result in very little condensed metallic mercury. For the vaporization of both HgS and HgSe. the mercury vapor was found to have back-reacted to the extent that virtually none of the vaporized mercury was collected in metallic form. For the vaporization of Hg2S04? HgS04, and HgSO4*2HgO the amount of metallic mercury recovered varied from approximately 50% for HgS04*2HgO to approximately 10% for Hg2S04 and HgS04. Only for HgO was the recovered mercury in primarily elemental form. The application of the results to the operation of a vacuum retort and condenser system is discussed.

Jan 1, 2001

By Samson Adeosun, Sanmbo Balogun, David Esezobor

"Iron and steel making processes give rise to large amounts of usable and unusable materials, the latter generally being termed wastes. It is sometimes difficult to distinguish between re-usable by-products and wastes which cannot be sold or land-filled. Much depends on circumstances such as the local market for the material. This can itself vary from time to time with by-products which cannot be used or sold becoming wastes and vice versa. This paper defines the concept of “waste-free technology”, discusses its development in the steel industry and highlights the benefits of the technology to the manufacturing sector and the environment. The paper also articulates how the “waste-free” technology could be applied in the proposed Ajaokuta integrated steel plant in Nigeria.IntroductionIn the past, nature was considered an inexhaustible store. Its resources were consequently exploited and waste products therefrom were discarded. Today, attitudes have not changed appreciably even as raw materials cost rise by the year to pose a series of socio-economic problems, which, among others, may include the rational and optimum utilization of resources, environmental protection and reduction of waste formation. Consequently, industrialists now face unexpected regulatory pressure in areas of pollution prevention, waste minimization and hazardous waste disposal.Iron and steel making processes give rise to significant amounts of usable and un-usable materials, the latter generally being termed waste. It is sometimes difficult to distinguish between re-usable by-products and wastes which cannot be sold or land-filled. Much depends on circumstances such as the local market for the material. This can itself vary from time to time with by-products which cannot be used or sold becoming wastes and vice versa. In this paper, the term waste refers to those materials that are either irrationally utilized or, land-filled and part of the byproducts that are not utilized. It includes that part of used materials which is not incorporated into the products manufactured during a process stage and which in contrast to reuseable materials, is considered not suitable for any further use, owing to technical or economic factors. In general, these materials are inorganic and parts of them are either utilized or passed to the other processes; the other part should be disposed of using well-established waste disposal practices to avoid any environmental threat.Thus, creative methods must be developed to modify the manufacturing processes to reduce emissions and process wastes by fully utilizing all resources. One method of eliminating the negative effect of waste formation is the use of purification and cleaning structures (pollution control system, PCS). These are, however, quite expensive."

Jan 1, 2008

By Milton Syamujulu

In 2004, KCM Nkana Smelter commissioned a 1200 tonne per day flash dryer and associated dry concentrate transport and injection system on the existing Teniente Modified converter (CT) unit. The aim was to upgrade the existing smelting unit, increase copper output and improve energy efficiency. This paper reviews the design, installation and commissioning phases of the introduction of this new technology and also discusses the initial two years of operating results for both the flash dryer and injection system at Nkana.

Jan 1, 2006

By Mark William Kennedy

Modern metallurgical plants typically have complex flowsheets and operate on a continuous basis. Real time interactions within such processes can be complex and the impacts of streams such as recycles on process efficiency and stability can be highly unexpected prior to actual operation. Current desktop computing power, combined with state-of-the-art flowsheet simulation software like Metsim, allow for thorough analysis of designs to explore the interaction between operating rate, heat and mass balances and in particular the potential negative impact of recycles. Using plant information systems, it is possible to combine real plant data with simple steady state models, using dynamic data exchange links to allow for near real time de-bottlenecking of operations. Accurate analytical results can also be combined with detailed unit operations models to allow for feed-forward model-based-control. This paper will explore some examples of the application of Metsim to real world engineering and plant operational issues.

Jan 1, 2014

By Yuzura Sato

Viscosity has been measured for various molten binary alloys of nickel with iron, cobalt and chromium in order to clarify the behavior of viscous flow of molten nickel alloys. The entire concentration range for iron and cobalt and 0-67at% of chromium content were studied. The measurement method was an oscillating cup viscometry using an alumina crucible that was precisely machined. The temperature was up to about I 880K for all the measurements. The results represented good Arrhenian relationship although some measurements included overcooled temperatures. The isothermal viscosities increased monotonously with an addition of iron and chromium into nickel. The addition of cobalt increased after stationariness. The isothermal viscosities showed concave curves. Activation energies increased monotonously by adding all the elements into nickel. These phenomena were considered to be related to the thermodynamic properties 'such as the heat of mixing and the structures of mixture melts.

Jan 1, 2003

By Zhang Huaiwei, Shi Xiaoyan, Li Xinlin, Sun Fei, Hong Xin

"The control of the slag properties has become very essential in improving the separation between the slag and the matte in the copper slag cleaning process. The goal of the present work is to characterize the copper converting slag through chemical analysis (XRF), X-ray diffraction (XRD), scanning electron microscopy (SEM) coupled with energy dispersive spectroscopy detection (EDS) and thermal analysis (DSC). The majority of the identified elements were Fe, Cu, Si and 0. The XRD has presented compounds such as Fe2Si04, Si02, CuFe204, Fe304, and Cu. The main existence of copper element was the metallic copper due to the entrainment loss. Slight amounts of copper were existed as the CuFe204 in the slag. The density, viscosity, electric conductivity and the thermodynamic property of the molten copper converting slag were also investigated in the study.IntroductionCopper slag, which is produced during pyrometallurgical production of copper from ores, contains materials like iron, alumina, calcium oxide, silica etc. For every tonne of metal production about 2.2 ton of slag is generated [l]. The slags of copper converting process contain about 5% of copper and about 20% magnetite. The copper are present in the slags either as physically entrapped or in chemically dissolved [2-3]. The traditional slag cleaning method is electric furnace process including two steps, intensive slag reduction and quiet sedimentation. Although the process is suitable for the various copper slags, it is also with the higher energy consumption [ 4-7]. The slag characterization studies are the fundamental step in the definition of an appropriate recycling process for saving the energy consumption."

Jan 1, 2013

By Kazuyuki Kakegawa

The sintering characteristics and the change in the compositional distribution in the PbTiO3 PbZrO3-Pb(Mgl/3Nb2/3)O3 system during the sintering process by spark plasma sintering (SPS) method were examined. They were compared with those by a normal sintering method. The densification by the normal sintering was slow even at high temperatures, When SPS method was employed, much lower temperature and shorter period resulted in sintered bodies having almost the theoretical density. As expected in normal sintering, the compositional distribution decreased as the sintered density increased. On the contrary, the change in the compositional distribution by SPS was much smaller than that in the normal sintering. This sintering characteristic of SPS suggested a possibility of fabrication of sintered material having a desired compositional distribution.-

Jan 1, 2003

By Di Yang

The influence of high density (104 -105 A/cm2) electric current pulses (70 us duration) and continuous DC (~103 A/cm2) on the flow stress and ductility in tension of a high carbon steel wire were determined at 204°, 427° and 649°C. Electropulsing (100 pulses per second) with an effective current density of 100-200 A/cm2 gave a 10% enhancement in the uniform elongation of the wire at 204°C, but had no effect at 427°C and 649°C. In contrast, continuous DC either had no significant effect on the ductility or gave a decrease. The electropulsing per se decreased the flow stress only slightly at 204° and 427°C, but gave a significant decrease at 649°C. Continuous DC increased the flow stress at all three temperatures. The present results along with those by others suggest that the enhanced ductility by electropulsing and the reduction in flow stress may be further increased by raising the effective current density through increases in either the pulsing frequency, maximum current density of each pulse or pulse duration. This could conceivably increase the reduction per pass during wire drawing or the number of passes between anneals.

Jan 1, 2001

By Hidekazu Nakagawa

We investigated the anodic dissolution behavior of titanium in TMHA-Tf2N molten salt, which has a wide electrochemical window of about 5 V, in order to develop an electrodeposition method for titanium. By etching a titanium electrode in HF?HNO3?H3PO4 solution, the titanium electrode became electrochemically active, and a redox reaction was observed at around -0.15 V vs. I-/I3- in (TMHA-Tf2N)?HTf2N solution. We identified the redox reaction consists of the reduction of the proton and the oxidation of hydrogen. The diffusion coefficient of the proton in TMHA-Tf2N was calculated to be 6.9 10-8 cm2 s-1 at 50 °C from the cathodic peak current in the cyclic voltammogram. Anodic decomposition of the molten salt was not observed up to 6.0 V vs. I-/I3- on titanium electrode, while it was observed at around 2.0 V vs. I-/I3- on platinum and glassy carbon electrodes. Cathodic decomposition of the molten salt was observed at around -3.0 V on the titanium electrode, as well as on the platinum and glassy carbon electrode.

Jan 1, 2006

By Kouji Mimura, Masahito Uchikoshi, Minoru Isshiki

"HfO2 is expected to be a gate dielectric used in ULSI alternatives to S1O2. Although the materials used in ULSI are required to be significantly pure, commercial Hf contains > 2 mass% Zr. It is important to establish a process for removing Zr from Hf. In the present study, anion-exchange separation using a multi-column method was employed. The separation tests were carried out at variety of temperatures and flow rates. The decrease in the flow rate of the mobile phase made the elution curves of both Hf(IV) and Zr(IV) broaden contrary to the case of Co(II), Cu(II), or Fe(III). This is caused by the difference in adsorption rate on the anion exchange resin. In addition, more than one column was connected in series in order to enhance the separation. As a result, the content of Zr(IV) was successfully reduced to 1/100 of that relative to the raw material.IntroductionHafnium is one of the most important materials in modem society. The main applications of Hf metal are as a control rod in a nuclear reactors because of its large neutron-capture cross-section and as an additive to various alloys because of its corrosion resistance [1]. In addition to those applications, attention has been recently paid to HfCh as a high-x"" dielectric used in ultra large scale integration, ULSI, as well as ZrCh, AI2O3 and La2C>3, which are expected to be alternatives to conventional S1O2 thin films [2].The materials used in ULSI are required to have a high purity in order to avoid unexpected errors due to impurities. Furthermore, high purity Hf is indispensable for investigating the intrinsic properties of Hf metal. Thus, it is significant to establish the purification process for Hf from both the industrial and academic perspectives."

Jan 1, 2012

By C. H. Tsau

The intermetallic compounds of Ni-25Al-xFe, x is 20-40 at.%, were prepared by arc melting and drop casting into ingots, and were rapidly solidified into ribbons by melt spinning. The microstructure evolution of these alloys with varied Fe content were examined by the x-ray diffraction, optical microscope, scanning electron microscopy and transmission electron microscopy. The results reveal that two phases, {y'} and {B} phases, are existing in the alloys with low Fe content, and the microstructure changes from the mixture of y' and {B} phases to a single 0' phase when the Fe-content reaches to 40 at.%. Also, the formation of y' phase will be suppressed by rapidly solidified process. For annealing both of the melt-spun and the cast specimens, a disorder 0 phase was revealed in both of the ribbon and the cast ingot of Ni-Al-Fe alloys with higher Fe content. In addition, increasing the increment of iron which substituting nickel in this alloys results in increasing the lattice parameter of both {y'} and{B} phases.

Jan 1, 1992

By James Vaughan

Ionic liquids are solvents of interest for applications such as electro- plating, winning and refining of metals. Of particular interest is the possibility of processing reactive metals such as aluminium, magnesium and titanium that cannot be deposited from aqueous solutions. Aluminium has been electro deposited from AlCl3 : ionic liquid mixtures at low temperatures relative to conventional Hall-Héroult smelting. Imidazolium ionic liquids are have been used in the past due to their relatively high ionic conductivity and cation stability. The less studied and less expensive phosphonium ionic liquids systems may provide a viable alternative to imidazolium ionic liquids for certain applications. New information regarding the physical properties and electrochemical behaviour of phosphonium ionic liquid systems is presented.

Jan 1, 2006

By R. N. O'Brien, E. Peters

"It has been discovered that copper concentrates can be leached in strong (40-60%) sulfuric acid with nitric acid, or with oxygen if nitric acid is present as a catalyst. Chalcopyrite is rapidly decomposed at temperatures well below the boiling temperature of the lixiviant (-150 C.) and the resulting copper and ferric salts are precipitated as CuS04.H20 and FeH(S04)z.4H20. Other metal sulfides such as zinc, lead, nickel, etc. are also converted to sulfates that are nearly insoluble. Sulfur is partially converted to elemental and partially to sulfuric acid. Reduction products of nitric acid can be recovered from the distillate with good recovery. Conversion of as-received copper concentrates is largely complete in about 1 hour. Introduction9 molar sulfuric acid is an unusual hydrometallurgical lixiviant: it has a boiling point of about 150 C. and a low solubility for base metal sulfates. Below about 6 molar acid, the boiling point falls below 120 C. and yields much higher sulfate salt solubility, while above 12 or 13 molar acid and at higher temperature sulfuric acid becomes an oxidizing agent, yielding gaseous S02' Thus, sulfuric acid within this range of concentration is capable of acting well above the temperature of boiling water without requiring autoclave conditions, and if typical oxidative leaching conditions are applied to suspended mineral sulfide concentrates, it is possible to obtain a conversion of these sulfides into 'crystalline sulfates. Thereafter, the sulfates can be separated by filtration or by solid - bowl centrifuge and the solution can be recirculated to the reactor vessel. Meanwhile, the solid sulfates can be treated in a typical hydrometallurgical circuit, i.e., dissolved in a return stream that is essentially water, separated from each other by, for example, solvent extraction, and recovered as metals by electrowinning."

Jan 1, 1997

By Okechukwu Anopuo, Gerhard Tober, Petra Maier

"In this study, an investigation on the microstructure of hot rolled steel S355J2+N was conducted to optimize process parameters of complex forming, which combines rolling and bending. The best sets of parameters are worked out based on homogeneous mechanical properties and microstructure within the varied deformation degree with maximum at <p = 1.14 on a 25 mm thick plates. Mechanical properties, especially of heavy plates, are strongly influenced by the local deformation degree, strain rate and temperature. Detailed microstructural analyses showed that the ferrite-pearlite band structure changes near the surface, while maintaining homogeneous microstructure within the deformed work piece. Surface decarburization was also observed and this leads to decrease in hardness. To minimize iron oxide formation which could lead to side cracking, reduction in exposure time to temperature was suggested. On the other hand, temperature reduction below a critical value would risk the accurate forming process.IntroductionThis work presents the preliminary results of research to develop a new complex deformation process of thick steel plates. Complexity is given because the forming process combines rolling to reduce thickness and profiling by bending. The work piece will experience a thickness reduction from 25mm to 8 mm and is double curved. To explain and understand forming of thick plates basics of sheet forming as well as massive forming need to be used. At the moment there is no forming process established to produce double curved plates including reducing thickness in one process step. Technologies nowadays consist of two process steps: flat rolling and pressing in shape. Due to good weldability and formability the final product will be made of steel S355J2+N. This low-carbon steel is well understood and has a low strengthening exponent, which is expected to keep the forming forces down. Reduction of thickness from 25 mm to 8 mm gives furthermore a high deformation degree. Thus, hot forming has to be applied. The determination of process parameters is the main aim of overall research project; temperatures above lOOO°C are expected. Flow curves in literature are given at various temperatures and strain rates [1]. However, experiments with data close to the industrial application are rarely found, especially at low strain rates and high deformation degrees. Pre-test were done by flat rolling, being aware that the influence of bending is eliminated. The microstructure evolution were characterised in relationship to material formability with special attention to grain size change and recrystallization. Representative samples should be selected from specific locations in the deformation zone according to the knowledge about the metal forming process [2]. Due to no further alloying elements in S355, no precipitation hardening is expected to take place during hot forming, which keeps the mechanisms simple and the concentration on the feasibility of the complex forming process is given."

Jan 1, 2012

By K. P. V. Lei

The U.S. Bureau of Mines investigated a hydrothermal sulfidation procedure to recover lead and silver from plumbojarosite. The plumbojarosite, generated during pressure-oxidative leaching of zinc concentrate in a commercial operation, contained, in percent, 25.4 pb, 18.8 Fe, 1.4 Zn, 29.5 SO,2-, 3.2 s?, 13.4 total sulfur, and 7.4 oz/ton Ag. The sulfidation was conducted in an autoclave and converted the plumbojarosite to amorphous iron oxide and liberated the lead and silver as sulfides. The best operating conditions were using 50 9 of plumbojarosite and 7 pct s? (2.04 9 S? added) in 500 mL of 2.0 mol/L NH3, 150? C, and 1 h. The sulfidation product contained, in percent, 37 Pb, 28 Fe, 6 S2-, 2 SO,2-, and 11.2 oz/st Ag. Ferric chloride leaching extracted 98 pct Pb and 97 pct Ag from the sulfidation product.

Jan 1, 1990

By Wenbin Liu

A novel route for rapid synthesis of ultrafine WC-Co cemented carbides with homogeneous binder phase distribution is reported. The composite powder is produced by in situ reduction-carbonization reactions by using WO2.9, Co3O4 and carbon black as raw powders. The reaction equilibrium and phase stability are studied by thermodynamic calculations. The WC-Co composite powder is condensed by spark plasma sintering (SPS) to obtain the cemented carbides bulk. The sintering temperature is lower than that in the conventional sintering methods by 1500C, while the sintering time is remarkably reduced by 3-5 times. The high performances of the hardness and the fracture toughness are obtained. The experimental results confirm that the present processing scheme of in situ reduction-carbonization reactions and subsequent SPS sintering is an efficient way to prepare WC-Co cemented carbides, and is apparently superior to the conventional long-period techniques of preparing composite powder and cemented carbides bulk.

Jan 1, 2008