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By E. Bélisle, Christopher W. Bale, S. Petersen, C. Robelin, K. Hack, J. Melançon, G. Eriksson, A. D. Pelton, P. Chartrand, S. A. Decterov, I. H. Jung, A. Gheribi

The FactSage® package consists of a series of information, database and calculation modules that enable one to access pure substances and solution databases and perform thermochemical equilibrium calculations. FactSage was originally founded by process pyrometallurgists and has since expanded its applications to include hydrometallurgy, electrometallurgy, corrosion, glass technology, combustion, ceramics, geology, environmental studies, etc. With the various modules one can perform a wide variety of thermochemical calculations and generate tables and graphs of complex chemical equilibria and phase diagrams for multicomponent systems. This paper presents examples of recent and current developments in FactSage in areas of particular interest to Dr. David Robertson. These include both ferrous and non-ferrous processing, as well as solidification and refining simulation. The paper also includes reference to the Internet Fact-Web education package.

Jan 1, 2014

By Dong Joon Min, Joo Hyun Park, Mi Sun Choi, Jae Hong Shin

Sublimation of ZrCl4 is important for the production of nuclear grade metallic Zr in Kroll’s process. The sublimation kinetics of ZrCl4 was investigated by TGA under both isothermal and non-isothermal conditions. The sublimation rate of ZrCl4 increased with increasing temperature under isothermal conditions. ZrCl4 sublimation was confirmed to be a zero-order process under isothermal conditions, whereas it was first-order kinetics under non-isothermal conditions. The activation energy of ZrCl4 sublimation under isothermal conditions was 21.7 kJ/mol. The activation energy for non-isothermal sublimation was 101.4 kJ/mol and 108.1 kJ/mol with the Kissinger method and Flynn- Wall-Ozawa method, respectively. These non-isothermal activation energies were very close to the heat of sublimation (103.3 kJ/mol). Sublimation occurs by two elementary steps: surface reaction and desorption. Therefore, the overall activation energy of ZrCl4 sublimation is 104.8(±3.4) kJ/mol. The activation energy of the surface reaction and desorption steps are proposed to be 83.1 kJ/mol and 21.7 kJ/mol, respectively.

Jan 1, 2014

By P. J. Mackey

Over the course of Dr. Robertson’s career, the ferrous and non-ferrous plants have seen enormous changes in technology and increases in plant capacity, essentially amounting to a “technological revolution”. In iron and steel, the “mega” blast furnace of some 6,000 m3 working volume is now standard (~10,000 tonnes (mt) of pig iron/day). Similar huge changes in process technology and plant size have occurred in the non-ferrous industry. As an example, the fuelfired reverberatory furnace, once the mainstay of the copper industry, has disappeared - replaced by large capacity flash and bath smelting technologies. The energy consumption per unit mass of metal produced has also been reduced considerably. Our understanding of the thermodynamics and mechanisms of metallurgical reactions, a field to which Dr. Robertson has significantly contributed, has made great strides. This paper reviews these changes with particular reference to the copper smelting industry, providing also comments on expected future trends.

Jan 1, 2014

By Michele L. Bustamante, Gabrielle Gaustad

In recent years, t h e future supply of tellurium has been called into question due to the anticipated rapidly increasing demand from thin film cadmium telluride photovoltaics. Since tellurium is produced as a byproduct of other extractive processes – principally, the electrolytic refining of primary copper sulfide ore – it is important to explore the dynamics of the parent metal extraction and processing – in this case copper – when attempting to answer this question. This research explores the changing landscape of global copper production; introducing system diagramming and the concept of byproduct intensity (BPI) to illustrate concerning downward trends in tellurium supply potential. Upon closer inspection, it is concluding that, while a likely contributor to these downward trends, the increased use of non- traditional copper production techniques alone are not responsible; other factors include market substitution and incomplete data reporting. Additionally, a review of literature on tellurium recovery processing reveals a promising outlook for future supplies; highlighting potential for improvements in yield, which allow producers to make better use of what is available, even in the face of suppressed BPI.

Jan 1, 2014

By Baozhong Ma, Yonglu Zhang, Yongqiang Yang, Chengyan Wang, Yongqiang Chen

During the past decades, slurry electrolysis (SE) has been implemented commercially for the processing of bismuthinite and complex Pb-Cu bearing gold concentrates. Recently, SE was proven effective for the treatment of As-rich antimonic gold concentrates. Laboratory test results suggest over 98% of the antimony was extracted, while the extraction of arsenic and gold was less than 0.5%, and that of iron was less than 6%. Moreover, the cathode antimony contained over 98% antimony and less than 0.3% arsenic. Considering the disadvantages of traditional 3 kA slurry electrolysis baths, such as smaller electrode area, reduced capacity, and greater electrode deterioration, the authors have developed an innovative 12 kA slurry electrolysis bath equipped with mesh and fence type titanium alloy electrodes. Furthermore, the technique was successfully used within a pilot scale plant yielding results similar to those observed in the laboratory. The technique yielded ametallic antimony ingot of 99.9% purity after arsenic removal via the addition of Na2CO3.

Jan 1, 2014

By Mansoor Barati

The present paper is based on a term project for final year undergraduate students, requiring them to evaluate a process for producing silicon from rice husk. The traditional method for production of silicon involves carbothermal reduction of quartz in electric arc furnaces at temperatures exceeding 2000 °C. The technology consumes a considerable amount of electrical energy as well as fossil fuels, resulting in significant CO2 emissions. A flowsheet for production of silicon metal from rice husk is laid out in this paper. The technology will consist of combustors, which will generate steam using the rice husk biomass, power generator, and electric furnace for reduction of the rice husk. Materials and energy balance calculations presented here indicate that such process can be operated independent of external electricity.

Jan 1, 2014

By Xin Li, Hai-Xing Fang, Bing Xie, Hong-Yi Li

Chromium-containing vanadium slag (V-Cr slag) was obtained by an industrial smelting process of Hongge Ore, which is valuable vanadium-titanium magnetite to extract V and Cr in China. Sodium roasting thermodynamics of V-Cr slag in presence of oxygen were calculated to evaluate the reactivity of chemical compounds. Results showed that the oxidation of FeV2O4 was intensified in presence of Na2CO3 while the oxidation tendency of FeCr2O4 was far lower than that of FeV2O4. It was probably that reactions of impurities including Al2O3, SiO2 and Fe2O3 with Na2CO3 happened and the products can promote the oxidation of vanadium or chromium compounds in lower valence. Based on thermodynamic analysis, a two-step selective extraction process of vanadium and chromium was proposed. Extraction rate of vanadium was 88.6% while 7.0% for chromium in the first extraction step; extraction rate of 90.7% and 95.4% for vanadium and chromium, respectively, were obtained in the second step.

Jan 1, 2014

By Do-Hyeong Kim, Tae-Jung Kim, Seung-Yeon Won, Jong-Jin Pak, Min-Kyu Paek

Liquid iron alloys containing V, Mo, and Ni can be produced by the carbothermic reduction of spent catalysts used in petrochemical industry. Thermodynamics of carbon in these alloy melts is important for refining these alloys. In the present study, the carbon solubility in Fe-V, Fe-Mo, Fe-Ni, Fe-V-Mo, Fe-V-Ni, Fe-Mo-Ni and Fe-V-Mo-Ni alloy melts of various compositions was measured at 1873 K. The temperature dependency of vanadium effect on carbon solubility in liquid iron was also measured in the temperature range from 1823K to 1923K. The additions of vanadium and molybdenum significantly increased the carbon solubility in liquid iron alloys while nickel decreased the solubility. The experimental results were thermodynamically analyzed using Lupis’ relation at constant activity to determine the first- and the second-order interaction parameters of vanadium, nickel and molybdenum on carbon at carbon saturated condition. Using thermodynamic parameters determined in the present study, the carbon solubility in Fe-V-Mo-Ni alloy melts of various composition were accurately predicted and verified experimentally at 1873 K.

Jan 1, 2014

By P. Chris Pistorius

An example is presented to illustrate the joint effect of local reaction equilibria and mass transfer limitations, for reactions during ladle refining of steel. The example relies on some of the kinetic principles that David Robertson has employed to quantify many metallurgical processes. In calcium treatment of alumina inclusions in aluminum-killed steels, solid CaS forms as an intermediate reaction product. During subsequent reaction, CaS disappears and calcium aluminate forms; at the same time, aluminum and sulfur dissolve in the steel. Kinetic analysis shows that the rate of this reaction is not limited by mass transfer of dissolved aluminum and sulfur away from the reacting inclusions. The reaction rate is likely limited by transport of dissolved calcium. This example also illustrates the use of FactSage macros for kinetic modeling.

Jan 1, 2014

By Mark E. Schlesinger

Engineering design follows a six–step sequence. Demonstration of this sequence in materials engineering is less common. A case study is presented, using the 1989 paper by Gafner on the development of 990 gold-titanium alloy. This paper identifies a need, develops the problem, identifies alternatives, demonstrates the use of metallurgical principles to identify alternative responses, and shows how more favorable options are selected. The paper can also be used to illustrate engineering design as an iterative process. The paper is also useful as a starting point for more in-depth examination of specific elements of the design process, and lends itself to the creation of student exercises.

Jan 1, 2014

By Peng Jianping, Feng Naixiang, Di Yuezhong, Wang Yaowu, Pan Xijuan

A vacuum silicon thermal reduction lithium process is developed in present work which used lithium hydroxide, alumina and calcium oxide as raw materials. The process contains two steps, which are that Li5AlO4 clinker is prepared in ambient environment, and that metal lithium is extracted from Li5AlO4 clinker with ferro-silicon alloy as reductant in vacuum. On the basis of thermodynamic analysis and investigative experiments, feasibility of this process is proved. The results show that Li5AlO4 can be generated by calcination lithium hydroxide and alumina, the burning loss is above 31% under the conditions of calicination temperature above 750℃ and time more than 90min. The main phases of calcination product are Li5AlO4 and CaO. When the calcination product is reduced by ferro-silicon alloy in vacuum, the lithium reduction ratio can be over 80% under the conditions of reduction temperature 1200℃ and reduction time 60min.

Jan 1, 2014

By P. J. Mackey, J. B. See, D. G. C. Robertson

The production of iron and steel and non-ferrous metals by pyrometallurgical processes will remain a critical element in meeting the demand for materials in both developed and developing nations. Given the important need to reduce and minimise greenhouse gas emissions the technological focus of future pyrometallurgical R&D by universities and industry alike must concentrate on sustainability issues such as improved energy efficiency, recycling and waste minimization. Continued efforts are also needed on process optimization and new process development with a view to reducing capital and operating costs of the new large “mega” plants. Using the academic and industrial backgrounds of the authors, the present paper reviews the current status of R&D in pyrometallurgy in university departments with a particular emphasis on sustainability issues. The role of industry and government laboratories is also reviewed although primarily for developed countries. The paper also includes comments and suggestions on the future requirements for education and R&D in pyrometallurgy in developed countries to maximise sustainability. It is also suggested that future R&D in pyrometallurgy will be even more concentrated in developing countries – most notably China.

Jan 1, 2014

By Hassan Saalman, Mahmoud Mahmoud, Omneya El Hussaini

The Ferruginous sandstone ore was obtained from Ramlet Hemeyir area, Southwestern Sinai, Egypt, was found to contain 10% rare earth elements (REE). A representative sample has been subjected to sulfuric acid agitation leaching. About 93% of the REE content was released by mixing the ground sample to -100 mesh with concentrated H2SO4 at solid/liquid (S/L) ratio of 1/2 for 5h at a temperature ranged from 250 to 300o C. The REE was precipitated from the prepared sulfate leach liquor of pH 1.0 by adding 35% oxalic acid at 25o C. The precipitation yielded 98% REE. For selective separation of yttrium, the rare earth cake was leached with 31.5% nitric acid. Next, the aqueous solution was contacted with di-(2-ethylhexyl) phosphoric acid (D2EHPA) where 98% yttrium extraction was achieved. Stripping was done with hot H2O (80o C). Finally, a precipitation with oxalic acid was done followed by ignition at 950o C. A yield of 95% yttrium oxide was produced.

Jan 1, 2014

By Xiaofei Guan, Adam C. Powell, Uday B. Pal, Srikanth Gopalan

This paper reports a solid oxide membrane (SOM) electrolysis experiment using an LSM– Inconel inert anode current collector for production of Mg and O2 at 1423K. The electrochemical performance of the SOM cell was evaluated by using various electrochemical techniques including electrochemical impedance spectroscopy, potentiodynamic scans, and potentiostatic electrolysis. The effects of Mg solubility in the flux on the current efficiency and the YSZ membrane stability during SOM electrolysis were discussed and examined through experiment and modeling. The electronic transference number of the flux were measured to assess the Mg dissolution in the flux during SOM electrolysis. A negative correlation between the electronic transference number of the flux and the current efficiency of the SOM electrolysis was observed.

Jan 1, 2014

By P. Ying

An auxiliary system connected with SEM-EDX for rapid identification of mineral and rock sample has been developed. With the aid of a synthetic spectrum library created, using the compare and match techniques provided by INCA software in EDX the mineral or rock sample names for refer-ence can be given at the same time analyzed.

Jan 1, 2014

By M. R. L. Blackwell

Over the period 1964 to 1969 Conzinc Riotinto of Australia undertook and completed an evaluation of a large low-grade copper orebody on Bougainville Island in the Territory of Papua and New Guinea. From the outset it was clear that the geographic, climatic and topographic characteristics of the area would necessitate a heavy capital outlay on production and support facilities. Both the physical problems and the magnitude of the investment amplified the need for a thorough and rigorous evaluation of the various strategies for exploiting the orebody. In view of the number of independent and inter-related variables and the flow of new data, a computer-based evaluation process extended the scope and depth of the analysis considerably. The system used permitted an iterative assessment and re-assessment of the various strategies with the results becoming increasingly refined with time. This process encompassed the modelling of the orebody, the simulation of alternative operating strategies and the determination of the financial profitability of the project,

Jan 1, 2014

By A. H. Farazi, C. Quamruzzaman

The freezing and subsequent solidifying of unstable, weak (sands, silts and clays) and/or wet soil to form a desired-shape frozen barrier around a construction area are possibly the main features of the freezing method for shaft sinking. The barrier, along with strengthening the soil, provides a dry environment to ensure sustainable subsurface construction work before placing a permanent lining. The freezing method requires the installation of freezing pipes in boreholes around the construction area and the circulation of chilled salt water through these pipes and has long been a proven technique for dry shaft sinking through unstable and water-bearing seam around the world. As removing heat from the ground is the main feature of the method, an efficient thermal design of the freezing process is mandatory to ensure success of the shaft sinking operation. This applies to both the sustainability and economy of the intended structure. The design presented in this paper is aimed at figuring out the heat-removing ability and operating time of the refrigerative equipment using some simple formulae. The authors adopted a theoretical approach to determine the quantity of heat to be removed from the ground. The amount of energy for the equipment was found to be greater than that for freezing, which proved the validity of the design. The active freezing period was calculated to be 121 days. The authors followed the structural design of the freezing process they proposed in their previous work (Farazi and Quamruzzaman, 2013). Though the first coal seam in the coalfield was encountered at a depth of approximately 352 m in the subsurface, the target depth for cooling and freezing was decided to be 162 m. The formation demands extra care to nullify its risk of the temporary structure collapsing and water rushing in (Farazi et al., 2012). Discussion on the determination of refrigerative equipment parameters was excluded from the scope of this work.

Jan 1, 2014

By C. D. Litton, I. E. Perera

Experiments were conducted to evaluate the response characteristics of commercially available gas, smoke and flame sensors to fires of common combustible mine materials. The experiments were conducted in the large-scale fire gallery located at the National Institute for Occupational Safety and Health (NIOSH) Lake Lynn Laboratory in Fairchance, PA, using ponderosa pine, red oak, Douglas fir, high and low volatile coals, polyvinyl chloride (PVC) and styrene butadiene rubber (SBR) conveyor belts, No. 2 diesel fuel and diesel exhaust. All the experiments (except those using No. 2 diesel fuel and the diesel exhaust tests) were conducted in a similar manner, with combustible materials heated rapidly by electrical strip heaters, producing smoldering fires that quickly transitioned into flaming fires. The sensors included a diffusion-type carbon monoxide (CO) sensor, photoelectric- and ionization-type smoke sensors, a video smoke/flame detector and an optical flame detector. Simultaneous measurements were obtained for average gas concentrations, smoke mass concentrations and smoke optical densities in order to quantify the levels of combustion products at the alert and alarm times of the sensors. Because the required sensor alarm levels are 10 ppm and 0.044 m-1 optical density for CO and smoke sensors, respectively, the different sensor alarms are compared to the time at which the CO and smoke reached these alarm levels (Litton et al., 1991). In addition, the potential impact of using smoke sensors that have met the performance standards from accredited testing laboratories is also evaluated using the response of an Underwriters’ Laboratory (UL)-approved combination photoelectric/ionization smoke detector. The results are discussed relative to fire sensor needs that can have a positive impact on mine fire safety.

Jan 1, 2014

By K. M. Kim

An analysis was conducted to determine the effects of blasting on slope stability and downstream comminution processes. To investigate these effects, the extent of blast-induced rock damage and the magnitude of induced stress were examined. This analysis showed that damage may extend up to 500 m (1 MPa, tensile strength) into the rock mass, a distance that is sufficient to have an impact on the pitscale slope over the long term. In addition, the damage zone was calculated using the assumption that compressive waves are the primary agent in microfracturing during blast fragmentation. The calculated damage zone — up to 2.2 m (43 MPa, rock mass compressive strength) — indicates that microfracturing can occur throughout 20-50% of the entire rock mass in the blasting area, depending on the blast geometry, burden and spacing. Finally, an economic analysis was conducted by comparing two assumed blasts in a copper mine. The change in energy required for crushing and grinding was demonstrated using Bond’s law after increasing the blast energy from 180 kcal/t to 350 kcal/t. A total cost saving of 13.3% ($9.4M) was achieved with the increase. However, the benefits of blast-induced microfracturing must be balanced against the potential impacts to slope stability to ensure safe conditions, a top priority in mining operations.

Jan 1, 2014

By W. G. Pariseau

A study of coal pillar strength at the Beehive Mine in central Utah was done in the 1970s. This study was a cooperative effort by the University of Utah, RE/SPEC, Inc., and the American Coal Company and was funded by the U.S. Bureau of Mines. Mine measurements of closure at 117 points and pillar stress using 119 vibrating wire stress gauges were made during retreat mining in this room-and-pillar operation. Laboratory testing for the strength and modulus of 372 coal cylinders up 0.3 m (1 ft) in diameter and 0.6 m (2 ft) in length was also done. Two-dimensional finite element model analyses complemented the study. However, the real world of mining is three-dimensional and in consideration of the significant advances in computing power since the time of the original study, a revisit of the data seemed warranted. In this regard, a novel finite element method was used that allows for the whole-mine analysis of tabular excavations on the kilometer scale and yet enables details to be obtained at pillar walls on the meter scale. The effects of material properties variability in situ and of joints can also be taken into account. Results that compare computed two- and three-dimensional seam-level closures with mine measurements show noticeable differences; three-dimensional results are reasonable, while two-dimensional results overestimate closure by nearly a factor of two.

Jan 1, 2014