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By M. Tangstad, H. Mølnäs, J. D. Steenkamp

"Temperature affects several aspects of pyrometallurgical systems, including thermodynamics and reaction kinetics. Reliability of temperature measurements in laboratory and plant applications is thus important from process, safety and financial perspectives. This case study briefly introduces different techniques utilized for temperature validation, and demonstrates temperature validation on laboratory scale utilizing the wire-bridge method. Pt/Ptl3Rh thermocouple hot junctions were constructed by mechanically connecting thermocouple wires through a pure metal bridge consisting of copper, gold, nickel or palladium wire. When heating the wire-bridge thermocouple alongside a regular Pt/Ptl3Rh thermocouple, temperature offsets were quantified as the wirebridge thermocouple short-circuited at the melting points of the pure metals. At the melting points of gold (1064°C) and palladium (1555°C), average measured temperature offsets were -2.1°C ± 2.3°C and 0.2°C ± 0.4°C, respectively. Results from the copper and nickel wire-bridges were inconclusive. The paper concludes with a discussion on the potential industrial applications of the technique.IntroductionThermocouples are probably the simplest of all temperature sensors, but are widely utilized due to simplicity, versatility and ability to handle a variety of experimental conditions and industrial applications. Additionally, thermocouples are often the only option in research laboratories requiring high temperature measurements, and a high level of reliability is usually required from thermodynamic, kinetic as well as safety points of view.The study presented here originated from a test program where the compatibility between different types of carbon-based refractory materials and industrial slag produced in silicomanganese furnaces were investigated on a laboratory scale utilizing the static crucible test[l]. Due to the nature of the silicomanganese production process, the compatibility tests were to be conducted at 1600CC[2]. Details of the experimental set-up utilized for the compatibility tests are discussed in the Experimental Set-up and Method Statement section later in this paper."

Jan 1, 2012

By Mei Yang, Wei Gao, Jian Yang, Qingcai Liu, Wenchang Xi

"TiO2 has been loaded on cordierite porous ceramic to prepare the SCR catalyst carrier by using both APCVD and sol-gel technology. In APCVD method, TiC14 and O 2 were used as reaction precursor. TiC14 was gasified by using N2 as carrier gas which was controlled to 500sccm. Its reaction temperature and reaction time were limited to 773K and 30min respectively. The physical properties, SEM and SEM-EDX of the TiO2-cordierite carrier and the properties of SCR catalysts prepared by these carriers have been tested. The tests showed that TiO2 loaded by APCVD method were of graininess shape and even accumulation. The loading rate of TiO2 and the specific area of carrier sample were increased 114% and 21 % respectively comparing with sol-gel technology. In the result of sol-gel method, the maximal difference of Ti content was 66.92%, while the result of APCVD method was 18.89%. It demonstrated that TiO2 was uniformly attached with the cordierite ceramic by using APCVD method, which would ensure more active ingredients well loaded on the Ti02-cordierite carrier. This difference made the denitrification ratio of catalyst prepared by APCVD method was 8.1 % higher than that of catalyst prepared by sol-gel method.IntroductionIn recent years, the emission of NOx, which were caused by coal-fired power plants, has gotten more and more attention. SCR (selective catalytic reduction) is the most effective technology to DeNOx [ll. The core technology of it is the catalyst. The SCR catalyst usually uses Ti02 as the carrier, and V2O 5 as the active component [2, 3] . However, the thermal stability and mechanical properties of TiO2 carrier are unstable, which would influence the performances of the catalyst. The commercial catalyst generally uses WO3 or MoO3 to promote its heat stability at present [4-7] Besides, TiO2 is expensive. Compared with TiO2, the cordierite is of good thermal stability and lower price. So loading Ti02 on cordierite porous ceramic as carrier to produce SCR catalyst is of good prospects [S, 91 • Currently, TiO2 is usually loaded on cordierite by the sol-gel method. But some research has shown that the sol-gel method easily reduced the loading performances of TiO2, such as distribution, combination, etc. APCVD (atmospheric pressure chemical vapor deposition) has many advantages to preparing TiO2 films, such as high bonding strength, fast reaction rate and so on [l0-13l_ In this paper, TiO2 has been loaded on cordierite porous ceramic to prepare the SCR catalyst carrier by using both APCVD and sol-gel methods. The properties of the carriers prepared by the two processes have also been compared."

Jan 1, 2011

By William R. Opie

Considerable effort by extractive metallurgical research organizations has been devoted recently to developing pollution-free processes for treating copper sulfide concentrates. A number of hydrometallurgical processes are in various stages of development and have been subjected to economic evaluation. Although the hydrometallurgical approaches eliminate SO2 emission problems, they create objectionable effluents and residues, make precious metals recovery complex, and are not very efficient for treating chalcopyrite. Furthermore, they are consumers of considerably more energy than pyrometallurgical processes which produce blister copper that can be electrorefined to commercial grade cathodes. This paper discusses a pyrometallurgical process under development by AMAX Base Metals Research & Development, Inc. (1) The original objectives set for the process development were: 1. Sulfur control of at least 95% with elimination of fugitive emissions. 2. Copper and precious metal recoveries as good as or better than conventional processes. 3. Low capital cost. 4. Competitive operating costs 5. Use of known proven technology where applicable.

Jan 1, 1976

By Eric Klaffenbach

Valorization of slag from metallurgical industrial processes becomes ever more important as this may help optimizing and reducing the use of natural resources such as rock and sand. In view of this objective, metallurgical processes have to be analyzed in order to modify the slag composition so that it will meet the expected requirements of potential users of these resources. This paper gives the results of a thermodynamic analysis of the flash smelting process to understand the impact of operational parameters on slag chemistry and elemental partitioning in the process. It is shown that an increase of the matte grade and temperature leads to higher deportment of Pb, Zn and As to the slag. With increasing matte grade the volatilization of these elements decreases. Furthermore, the results indicate an increasing solubility of Cu and S in slag at higher temperatures.

By Gus Van Weert

Solvent extraction of iron from zinc refinery liquors has been investigated before, mainly on the MEHPA / HC1 stripping combination. Leakage of chloride into the zinc electrolyte and the costs of handling the ferric chloride eluate have prevented this option from being adopted. This work explores the stripping of the ferric loaded organic phase with nitric acid to take advantage of the possibility of regenerating up to 6N nitric acid, and clean spheroidal hematite production by autoclave treatment of ferric nitrate solution. The work was carried out with DEHPA (di 2-ethyl-hexyl phosphoric acid) in kerosine. Degradation testing proved the DEHPA to be very stable, when exposed to nitric acid solutions up to 6N and temperatures up to 70" C over a period of five days. Ferric iron was removed completely froma synthetic hot acid leach liquor, irrespective of the DEHPA concentration. Stripping the ferric turned out to be the problematic step. Although the stripping efficiency was considerable better at 50 than at 20° C, it decreased with increasing DEHPA/Fe ration in the organic phase. Eluates of no more than 5-10 g/l ferric nitrate were produced. surprisingly, nitric acid was found to be a less efficient stripping agent than sulphuric at equivalent normality and its efficacy levelled off above 4N. It was concluded that DEHPA does not appear to be the S.X. reagent to take advantage of the low cost autoclave decomposition of ferric nitrate opportunity in zinc hydrometallurgy and that another S.X. reagent, also resistant to nitric acid, but based on weaker compound formation is needed.

Jan 1, 1998

By O. C. Gaspar

The mineralogical and textural characteristics of the volcanogenic massive sulphide ores from the Aljustrel and Neves-Corvo deposits have been studied by ore microscopy techniques since 1977. Several ore types have been recognized, and the ore paragenesis, ore textures, and behaviours of different ore types during grinding and concentration processes, have been determined. An ore classification was established for use in metallogenetic studies, ore reserve calculations, selectivity during mining, and control of the ore beneficiation processes. In addition, an empirical method was developed for supplying, on time, the qualitative and semi-quantitative information needed for processing the Aljustrel ores and for optimizing the Neves-. Corvo copper and tin concentrators.

Jan 1, 1991

By L. Petitnicolas

The experimental study of nitrogen absorption and its removal from a liquid Ni-20%Cr alloy at 1873 K has been undertaken, using an experimental, apparatus based on the Sieverts technique in order to determine the solubility of nitrogen in the alloy. as well as the kinetics of nitrogen transfer across the gas/melt interface. Experiments show that nitrogen solute equilibrium content can be calculated using the Sievens law. Measurements point out the nitrogen absorption reaction rate to be well described by first order kinetics, whereas experiments on nitrogen removal reveal that the rate is better expressed using a second order equation.

Jan 1, 1996

By Takeshi Ohgai, Hisaaki Fukushima, Tetsuya Akiyama, Joon-Seo Ki

"Recently, an intensive attention has been paid to the electrodeposition of Zn-Cr alloy in the field of the production of super-highly corrosion-resistant alloy plated steel sheets for the next generation. In this study the electrodeposition of Zn-Cr alloys from the sulfate baths was conducted to investigate the codeposition mechanism of Cr with Zn. As a result, Cr was codeposited with Zn at higher current densities in both polyethyleneglycol(PEG)-free and PEG- containing baths. However, PEG made it possible to reduce Cr+ to the metallic state and Cr existed in the form of Cr(III) hydroxide in the deposits obtained from PEG-free bath. The measurements of the partial polarization curve of Zn and the pH in the cathode layer revealed that PEG acted as a polarizer to shift the cathode potential to the reduction potential of the composited hydroxides of Zn and Cr formed due to the pH rise in the cathode layer.1. IntroductionRecently, much attention has been paid to the electrodeposition of Zn-Cr alloys because of its application to the production of super-highly corrosion-resistant alloy plated steel sheets for the next generation1Hl_ Some researches have already tried to commercialize this type of steel sheet. High corrosion-resistance of this steel sheet is brought about by codeposited Cr in the alloys. According to Piontelli's classification5l concerned with metal deposition from aqueous solution, Cr belong; to an inert metal and its deposition is associated with a large amount of hydrogen evolution. Therefore the current efficiency for Cr deposition is extremely poor. It has been also reported that Cr is unable to codeposit in the electrodeposited Zn film in the absence of a certain additive in the solution. 0-compounds group colloids7l, ether group organic compounds8), 9>, peptide based compounds10l, etc., have been found to be effective additives to induce the codeposition of Cr with Zn. However, few studies have been made on the codeposition mechanism of Cr with Zn. In this research, the fundamental electrodeposition behavior of Zn-Cr alloys from sulfate baths was investigated to clarify the codeposition mechanism."

Jan 1, 1998

By Tim B. Vander Wood

Standard methods of determining clay mineral powder aspect ratios involve manual scanning electron microscopy analyses of shadowed particles in order to measure both platelet thickness and diameter. We present a method whereby the diameters of platelets are quickly determined by automated scanning electron microscopy and their images are recorded and digitally transferred to a transmission electron microscope equipped for parallel electron energy loss spectroscopy. Thickness' of platelets whose diameters are known from the previous analyses are determined by measurement of the ratio of scattered and unscattered electrons in the beam after it has been transmitted through the platelet.

Jan 1, 1995

By M. Kobayashi, Y. Nishisu

"Fine multicomponent particles of yttrium and europium were synthesized through the precipitation from homogeneous solution, and the various characteristics related with the fluorescence were investigated. The morphology and the fluorescent characteristics of the synthesized particles were affected by ionic species in the stock solution. In the presence of sulfate ion, some parts of the precipitated particles were aggregated, and _the fluorescent characteristics were not good. On the other hand, in the presence of chloride ion or nitrate ion, the particles precipitated were almost monodispersed, and, the intensity of the fluorescent emission were strong after calcination. Further, these particles were also very attractive as the red phosphor in the mercury-free fluorescent systems.Introduction Eu doped Y oxide particles have been widely investigated for the application to the fluorescent lamps and displays: Recently, the fluorescent lamps are pointed as harmful electric equipments because of using mercury for excitation. Therefore, the use of the mercury in the fluorescent- system will be limited or prohibited worldwide in near future. Then, the development of the mercury-free fluorescent lamp is strongly required without delay. Inert gas such as neon and/or xenon seem to be applicable as new excitation element that replaces the mercury. However, in case xenon the excitation wavelength,' 146 and 172nm, is different from that of the mercury, 254nm, and then, the commercial phosphors which are used in the present fluorescent lamp system are not available. Therefore, the invention of the novel phosphors is essential for the development of the mercury-free fluorescent lamp. Further, the controls of the size and shape of the particles precipitated are also important, because the homogeneity of the size and the shape is very important for the fabrication of the layer of the phosphor particles. That is to say, the development of the phosphor particles with controlled components, size and shape is essential. The precise control of size and shape improves the packing density, and so, the screen performance of the lamp [1]. In addition, these phosphor particles should be also useful for the application of the flat-plane displays, for example, PDP, etc. [2,3]. In the present work, first, the particles including yttrium and europium for the precursor for red phosphor were prepared through precipitation from homogeneous solution. This process was precisely controlled for the control of the components, size and shape of the particles precipitated. Next, the particles precipitated were calcined, and then, their fluorescent properties were characterized. As a result, some of them showed the possibly available characteristics as the red phosphor for mercury-free fluorescent lamp system. These experimental results are presented in this paper."

Jan 1, 2000

By A. S. Rao

In the original roast-leach-electrowin (RLE) circuit at the Chambishi Cobalt Plant, commissioned in 1978, the separation of nickel and zinc from cobalt in aqueous streams was achieved by successive stages of precipitation using lime. However, this technique was not able to meet the increasingly stringent metal quality requirements of customers whilst maintaining acceptable process recoveries. Intensive process development work was carried out and, in July 1988, an ion exchange circuit for nickel removal was commissioned using DOW XFS 4195 resin and for the first time Z.C.C.M. produced high purity cobalt metal containing less than 0.10% nickel. Following further work, a solvent extraction circuit for zinc removal, using DZEHPA, was commissioned in February 1991 in order to enhance cobalt recovery by reducing co-precipitated cobalt losses. This paper outlines the process development, design, commissioning and subsequent operation of these nickel ion exchange and zinc solvent extraction circuits.

Jan 1, 1993

By R. Altman

A Brookfield viscometer fitted with a stainless steel bob was used to measure the viscosity of industrial lead blast furnace slags between 1126 and 1298°c. Slag oxidation state was characterized by first annealing the? slag samples at 750°c in sealed copper tubes in order to precipitate magnetite crystals. The magnetite concentration was then measured on an Outokumpu Saturated Magnetic Analyzer. Using an Arrhenius-type equation, a viscosity model was developed by regression. The equation below accounted for 75% of the variability in the data used to generate the regression coefficients and, on average, could predict viscosity within ± 12% of the measured value. The greatest difficulty encountered in measuring viscosity was due to the occasional presence of solids in the slag which caused, at times, erroneously high viscosity measurements. Precautions to minimize this problem are outlined in the text.

Jan 1, 1985

By Philip Arthur

The ISASMELT process is making a significant contribution to the global metals industry. ISASMELT furnaces are now operating successfully in eight different countries and treating approximately 3 million tonnes of concentrates and secondary materials per year. The process is currently used in both lead and copper smelting. The most recently commissioned plants were in Germany and China, one for treating scrap copper and the other treating low-grade copper concentrates. The Copper ISASMEL T furnace ("CIF") at Mount Isa Mines Limited (UMIM") has continued to set new operational records, with throughput of more than I million tonnes of concentrate per year and very low operating costs. This paper summarises the latest operational data from the Mount Isa Copper ISASMEL T plant and outlines the successful approach to industrial R&D taken by MIM in the development of the ISASMEL T process.

Jan 1, 2003

By Sharif Jahanshahi

Calcium ferrite slags are often associated with Professor Yazawa due to his pioneering work on the thermodynamics of this type of melts. Over the past years CSIRO has invested some effort in studying physico-chemical properties of such melts to fill in some gaps in our knowledge and explore opportunities for application of the understanding developed. These investigations cover thermodynamics, transport properties of calcium ferrite based slags, as well as the kinetics of reactions of such slags with refractories. The present paper provides an overview of some of these studies and highlights some of the interesting behavior of such melts. The oxidation state of copper and arsenic in calcium ferrite based slags are predominantly Cu+ and As3+, respectively, at oxygen potentials below 10.1 atm. The concentration ofCu2+ in such slags becomes significant at oxygen potentials of greater than 10'1 atm at 1300 ?C. The activities of CuOo.s and AsOl.S in calcium ferrite slags show strong deviations from the Raoultian Law, while that of CoO is very close to ideal behaviour with respect to pure solid CoO. Addition of Si02 to calcium ferrite slags can have significant effects on the activities of FeO and Fe2O3 and hence the stability of magnetite phase. Transfer of oxygen in calcium ferrite slags is fast with diffusivity of 2xlO?3 cm2/s at 1350 °C and activation energy of 16 kcal/mol Presence of solid phases, such as magnetite, has pronounced effect on the viscosity of calcium ferrite slags. The observed dependence on solid loading and shear rate indicates deviation from Newtonian behaviour. The interfacial tension between copper mattes and calcium ferrite slags is strongly dependent on the matte grade, with the determined values being much lower than the corresponding ones for interfacial tension between similar mattes and iron silicate slags. MgO, Cr2O3 and MgCr2O4 have low solubility in calcium ferrite slags and their solubility increases with increasing copper oxide content of the slag at 1300 °c. The oxidation state of the slag has strong effects on phase transformation, dissolution rate and disintegration of refractories in calcium ferrite slags. Other key factors with major impact on slag-refractory interactions include viscosity and surface tension of slags as well as the contact angle between slag and refractory material.

Jan 1, 2003

By A. Shemi

Tungsten carbide scrap (WC–Co) is material generated from the tungsten carbide manufacturing process and worn out or used carbide parts from industry. Tungsten (W) ores contain about 3 wt% WO3 and their W concentrates about 10– 75 wt% WO3. Tungsten carbide scrap typically contains 40–95 wt% W. The high intrinsic value of W and the fact that the least valuable scrap contains more W than the average tungsten ore makes tungsten carbide scrap a worthy material for re-use. This study has investigated the selective dissolution of the cobalt (Co) binder phase, and recovery of tungsten monocarbide (WC) and Co using an acid leach process. The Co component was selectively leached leaving the WC solid particles intact. Further investigation using a complexing agent-aided acid leach process that takes advantage of organic chelating agents that form a soluble tungsten complex in place of the passive insoluble tungsten oxide is envisaged. The optimal dissolution of the Co binder phase using an inorganic acid in conjunction with an organic complexing agent is a novel approach with the potential of reduced leaching times and possibility of regenerating the unreacted organic acid.

By Pertti Koukkari, Nagendra Tripathi, Karri Penttilä, Justin Salminen

A computational fluid dynamic model for a novel flash ironmaking process based on the direct gaseous reduction of iron oxide concentrates is presented. The model solves the threedimensional governing equations including both gas-phase and gas-solid reaction kinetics. The turbulence-chemistry interaction in the gas-phase is modeled by the eddy dissipation concept incorporating chemical kinetics. The particle cloud model is used to track the particle phase in a Lagrangian framework. A nucleation and growth kinetics rate expression is adopted to calculate the reduction rate of magnetite concentrate particles. Benchmark experiments reported in the literature for a nonreacting swirling gas jet and a nonpremixed hydrogen jet flame were simulated for validation. The model predictions showed good agreement with measurements in terms of gas velocity, gas temperature and species concentrations. The relevance of the computational model for the analysis of a bench reactor operation and the design of an industrialpilot plant is discussed.

Jan 1, 2014

By G. A. Brooks

Reactive ball milling has been proposed as a new route for producing carbides from oxides through carbothermic reduction. It is claimed that through milling oxide and graphite powders to the nanoscale, amorphous materials with very high reactivity are formed, that allows for easy transformation of the starting material to another in a subsequent thermal process. Thermodynamic analysis of this proposed process suggests that unless particle sizes are reduced to below 10nm, then reduction in size alone cannot explain a change in the stability of oxides. Even with nanometer scale powders, the products formed need to have a lower total surface energy than the reactants before a chemical change will occur. A model developed by Bhattacharya and Arzt for predicting localized temperature changes based on milling conditions suggest that temperature rises less than 400 K will be achieved in laboratory conditions. The present calculations suggest that nanometer scale powders formed through high speed ball milling (> I 0 mls) may have undergone a process analogous to melting and quenching. Further work is required to fully distinguish these features.

Jan 1, 2003

By G. A. Brooks

Reactive ball milling has been proposed as a new route for producing carbides from oxides through carbothcrmic reduction. It is claimed that through milling oxide and graphite powders to the nanoscale, amorphous materials with very high reactivity are formed, that allows for easy transformation of the starting material to another in a subsequent thermal process. Thermodynamic analysis of this proposed process suggests that unless particle sizes are reduced to below 10nm, then reduction in size alone cannot explain a change in the stability of oxides. Even with nanometer scale powders, the products formed need to have a lower total surface energy than the reactants before a chemical change will occur. A model developed by Bhattacharya and Arzt for predicting localized temperature changes based on milling conditions suggest that temperarure rises less than 400 K will be achieved in laboratory conditions. The present calculations suggest that nanometer scale powders formed through high speed ball milling (>10 mls) may have undergone a process analogous to melting and quenching. Further work is required to fully distinguish these features.

Jan 1, 2003

By Jae-Ho. Lee

For some electronic applications where a dispersed electrically-conductive particulate-phase is employed, the conductivity of the surface (or near-surface region) of the particles provides for the primary mechanism which determines its electrical conductivity. Particles of a less expensive material, which may have desirable thermal-expansion properties, when coated with silver offer a means of also obtaining desirable electrical properties and at low cost. The research conducted was focused primarily on the development of silver-coated tungsten particles for thick-film polymeric conductors. The ammoniacal electrolyte was formulated from silver-nitrate, glycine inhibitor and formaldehyde reductant. The reduction, and subsequent deposition, of silver occurred selectively on the surface of the tungsten particles. Coated particles were assessed by SEM imaging. The thickness of the silver coating was estimated to be approximately 100nm on the basis of a mass account and the coating being uniform. The electrical conductivity of a silver-coated tungsten-powder pellet was found to be similar to that of a silver-powder pellet, of identical geometry.

Jan 1, 1997

By Robert Mensah-Biney

The loading characteristics of gold-tetrabromide species onto a weak-base resin, PAZ-4, were evaluated using a completely mixed batch reaction system. The time. to attain equilibrium loading was substantial, on the order of several days. However, abnormally high loading capacity values of 15 to 20 meq Au/g dry resin (1000 to 1300 kgAu/tonne) were attainable in 24 hours. The loading of gold-bromo species by P AZ-4 was visualized as consisting of two processes: (i) the rapid adsorption of [AuBr4r species by simple ion exchange mechanisms and (ii) reduction of [AuBr4r to metallic gold by an electron exchange mechanism. Elution of gold from loaded resin was feasible provided the resin had not been loaded to high capacity values. If loading is carried to high levels, complete elution becomes impractical and the gold may be recovered by ashing the loaded resin. For the high loading capacities observed this option would appear to be cost effective.

Jan 1, 1991