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By John L. H. Patterson

Handheld XRF has become the favorite way of measuring the content and identity of alloys in the field. This is because of the very portable nature of the instrumentation and its simple operation. However, these analyzers have been unable to determine the concentration of the light elements like Mg and Si due to the very low energy of the x-rays produced by these elements. In the past accessories such as vacuum and He flush have given some analyzers the ability to determine these light elements with modest detection limits. The introduction of the Silicon Drift Detector (SDD) into this class of instrumentation has added a new level of analysis capability to portable XRF instrumentation. X-ray fluorescence is achieved by exciting a sample with a beam of x-rays, which in recent portable equipment are generated by a small tube. This results in the emission of characteristic x-rays from the sample under test. By measuring the energy of each x-ray it is possible to determine what element generated it. By counting the number of x-rays at each energy it is possible to determine the concentration of each element. The detection limit for each element is dependent upon the number of x-rays which reach the detector. As the number of x-rays increases the detection limit will improve. One of the major factors in an x-ray reaching the detector is the energy of the x-ray. As the energy of an x-ray increases the probability of that x-ray reaching the detector increases. The energy of an x-ray is inversely proportional to the atomic number (AN) of the element generating the x-ray. For example, an iron x-ray (AN=26) is 6.40 keV while an aluminum x-ray (AN=13) is 1.49 keV. As the energy decreases, the detection of the x-ray becomes less and less probable because the x-ray may be absorbed by the windows which are part of the instrument and detector or the air in the path between the sample and detector. In SiPIN based portable XRF analyzers, the lowest element which is detected with acceptable detection limits is normally considered to be Ti (AN=22). The detection limits for 60 second measurements on typical SiPIN XRF analyzer are given in Table I. Thus, portable analyzers have not been useful for measurement of aluminum and titanium alloys as major components of these alloys are Mg (AN=12), Al (AN=13) and Si (AN=14).

Jan 1, 2009

By K. Mansfield

Spent Pot Lining (SPL) is an unavoidable waste product of the electrolytic process in the smelting of aluminium. SPL is considered to be a hazardous waste in various countries because it contains significant quantities of absorbed fluorides along with traces of cyanide. In 1995, Portland Aluminium undertook the investment of AUD$26,400,000 to construct a Research and Development processing facility at Portland, Victoria, Australia, to treat SPL. Extensive research, development and design were carried out over 5 years prior to the investment decision. This study led Portland Aluminium to install an Ausmelt pyrometallurgical furnace to combust and melt the SPL producing a hydrogen fluoride (HF) laden gas, which was cooled and then converted to aluminium fluoride (AlF3). Both the cooling and AIF3 manufacture were processes developed by Portland Aluminium. Many commissioning, equipment reliability and process problems have been encountered that had not been experienced in the trials at Ausmelt or in the developmental process for the treatment of the furnace offgases to form AlF3. Designs based on anticipated process expectations have had to be re-engineered by the SPL team to ensure plant and operational success. In June 2001, the installation of the final major component - a slag granulation process - was completed. This has produced a vitrified (glassy) slag that is expected to have leachability qualities acceptable to the Victorian Environment Protection Authority (EPA) to allow commercial end uses of the slag material to be developed. Today (September 2001), the smelter has successfully used the fluoride product, namely 65- 70% AIF3, in aluminium production and the SPL plant has significantly increased throughput with expectations to be at annual design rates of 12,000 tonne of SPL in early 2002. "The Alcoa Portland SPL Process" has been technically developed and is a proven process for the treatment and recovery of valuable components from SPL materials.

Jan 1, 2002

By Shinroku Matsuzaki

Data the measurement sensor installed with spatial distribution on the blast furnace were successively accumulated online from the process computer to the database system over a long period. This is a new system that accurately considers the relation with the installation position of each sensor, and picture computerization of the measurement data was developed. The overall operation state of a blast furnace, which skilled operators can see in their mind?s eye, was objectively visualized as pictorial information.

Jan 1, 2006

By Manoj Kumar, Vinay Kumar, Nikhil Dhawan, Manish Wadhwa

"Electronic waste (e-waste) is a collective name given to discarded electronic devices such as Television, Cellular Phones and Personal Computers. Among the heterogeneous metals present in the e-waste are the base metals: copper, aluminium, nickel, tin, zinc, iron and precious metals: gold, silver, palladium, platinum apart from several hazardous and halogens metals. Hence there is a need to recover these metals from electronic scrap by recycling and then re-use, which can meet large amount of metals demand. Hydrometallurgical processing was employed for the recovery of metals from television printed circuit board (TV PCB). Different lixiviants such as hydrochloric acid, Sulphuric acid, and nitric acid were used to understand the dissolution behavior of copper, iron and lead present in the TV PCB. Effect of increasing concentration of nitric acid was also studied. Selective recovery of tin over 95% in the form of tin oxide was precipitated. The precipitated tin oxide was identified by X-ray diffraction technique. Tin oxide of purity more than 99.9% was obtained.IntroductionThe electrical and electronic industries comprising computers, television, mobiles, etc, which are manufactured utilizing printed circuit, boards, capacitors, resistance, soldering material etc. During production, at the end-of service life and degradation due to the advanced version with latest features generate valuable metallic and non-metallic constituents. European Union Council on waste electrical and electronic equipment (WEEE) has classified these into different categories as listed in Table 1 [Streicher-Porte et al., 2005]. Among these the information technology, telecommunications and consumer equipment constitute electronic waste (e-waste) [EC, 2002]. Almost all e-waste consists of an integrated part of printed circuit boards which is a valuable source of several metals such as copper, tin, lead, aluminium, iron, silver, gold, platinum etc. [Relay et al., 1990]."

Jan 1, 2008

By Rudolf Keller

"EMEC Consultants is developing a process to extract oxygen, aluminum and silicon from lunar anorthositic soil. The process will provide oxygen in space for propulsion, aluminum as a structural material, and possibly silicon for the construction of solar cells.The evolution of the process concept in the course of our present NASA-sponsored SBIR effort is discussed. A molten salt electrolysis producing aluminum and oxygen is the central step; inert anode technology is to be employed. Silicon will be produced by reducing the anorthite, CaAI2Si20S' with aluminum. In a steady-state operation, all components of the ore added have to be removed from the process, and the removal of calcium is a major topic of our experimental studies.Utilization of Lunar ResourcesUtilization of lunar resources may play an essential role in the exploration of the solar system and the conquest of space. High costs are involved in overcoming Earth's gravity to supply missions in space. Even at a low projected cost of $ 300 for transporting a pound of payload into Earth orbit -- today's costs are many times higher -- it appears attractive to use resources in space to produce needed materials. Processing of lunar resources on the lunar surface is an obvious possibility.Oxygen is a product of major interest. It is required for support of human life in space. Even greater quantities may be needed for propulsion, to conduct further missions into space. To satisfy this demand for oxygen through lunar processing requires a quite different solution than to supply oxygen on Earth, where oxygen gas is abundant and easy to extract from air or water. On the lunar surface, solid oxide materials have to be used. Hydrogen reduction of ilmenite and subsequent electrolysis of the resulting water is being studied [1]. Other suggestions include fluorination of lunar soil [2], reduction with lithium and electrolytic decomposition of the resulting lithium oxide [3], and aqueous HF leaching [4]."

Jan 1, 1988

By Anja Pfennig, Axel Kranzmann, Sabrina Schulze

The CCS technique involves the compression of emission gasses in deep geological layers. To guarantee the safety of the site, C02-corrosion of the injection pipe steels has to be given special attention when engineering CCS-sites. To get to know the corrosion behaviour samples of the heat treated steel 1.7225 42CrMo4, used for casing, and the stainless injectionpipe steel 1.4034 X46Cr13 were kept at T=60 °C and ambient pressure as well as p=lOO bar for 700 h - 8000 h in a C02-saturated synthetic aquifer environment similar to possible geological on-shore CCS-sites in the northern German Basin. The isothermal corrosion behaviour obtained by mass gain of the steels in the gas phase, the liquid phase and the intermediate phase gives surface corrosion rates around 0.1 to 0.8 mm/year at ambient pressure and much lower about 0.02 to 0.2 mm/year at 100 bar where the C02 is in its supercritical state. Severe pit corrosion with pit heights around 4.5 mm are only located on the 42CrMo4 steel. Main phase of the continuous complicated multi-layered carbonate/oxide structure is siderite F eC03 in both types of steel.

Jan 1, 2013

By Guojun Qi

This work relates to wafer bumping technologies for flip chip packaging applications in the electronics industry. Nickel and its alloys are alternative under bump metallization (UBM) materials because of their slower reaction rates with Sn-based solder as compared to Cu-based UBMs. In this study, we compared the morphologies of the intermetallic compounds (IMC) formed between Sn-bearing solders (Sn3.5Ag and eutectic Sn-Pb) and two types of nickel- based UBMs, electroless Ni-P (EN) and sputtered nickel. Both chunky-type and needle-type of intermetallics were observed between the EN UBM and the solders. In the case of sputtered Ni UBM, there is only a layer of scallop-type intermetallics formed. The morphology change and growth kinetics of the IMC in thermal aging process were analysed. Kirkendall voids were noticed from samples of Sn3.5Ag solder vs Ni-P UBM that have undergone prolonged thermal aging at high temperature.

Jan 1, 2003

By Guojun Qi

This work relates to wafer bumping technologies for flip chip packaging applications in the electronics industry. Nickel and its alloys are alternative under bump metallization (UBM) materials because of their slower reaction rates with Sn-based solder as compared to Cu-based UBMs. In this study, we compared the morphologies of the intermetallic compounds (IMC) formed between Sn-bearing solders (Sn3.5Ag and eutectie Sn-Pb) and two types of nickel- based UBMs, electro less Ni-P (EN) and sputtered nickel. Both chunky-type and needle-type of intermetallics were observed between the EN UBM and the solders. In the case 'of sputtered Ni UBM, there is only a layer of scallop-type intermetallics formed, The morphology change and growth kinetics of the IMC in thermal aging process were analysed. Kirkendall voids were noticed from samples ofSn3.5Ag solder vs Ni-P UBM that have undergone prolonged thermal aging at high temperature.

Jan 1, 2003

By K. Krishnapisharody, G. A. Irons

"The modeling of gas-liquid plumes in steelmaking ladles has been the subject of many investigations. In most studies, the “modified” Froude number, based on the momentum of the injected gas, has been employed to characterize two-phase plumes. This approach has several shortcomings and is critically reviewed in the present work. Based on an extensive review of previous work and theoretical considerations, it is demonstrated that the injected momentum and consequently, the modified Froude number has no significance to gas blowing operations in Ladle Metallurgy. Instead, an approach based on the “plume” Froude number, previously shown by the authors as the proper form for Froude similarity, is extended as a simpler alternative.IntroductionGas injection is central to most Ladle Metallurgy operations. During ladle processing, the steel melt is usually stirred by an inert gas like Argon through porous plug(s) fitted in the bottom of the ladle or a lance inserted deep into the melt. The purging serves several purposes viz., homogenizing the melt, flotation of inclusions, enhancing the rates both of refining reactions and dissolution of alloying elements and promoting inter-phase interactions in the ladle.The topic of gas injection into liquid baths has been the subject of several investigations in the past. A great deal of this work, both experimental and computational, was devoted to describing the structure and properties of two-phase plumes as reviewed recently [1]. Generally, the ascending two-phase mixture is sub-divided into three distinct regions [2]: the jet core, transition and the bubble plume, respectively. The jet region, where the momentum of the injected gas is transferred to the bulk liquid, is also called the ‘momentum region’. In a similar manner, the plume is called the ‘buoyancy region’ where the motion of liquid is caused by the buoyancy force exerted by the bubbles. The proper characterization of these regions is important for the analysis and modeling of stirring operations in Ladle Metallurgy. Although many mathematical correlations exist for this purpose, some issues of theoretical and practical interest to the modeling of gas-liquid plumes need further attention."

Jan 1, 2012

By Jun Enriquez

Kennecott Utah Copper aims to extend anode furnace campaigns to more than three years. As part of that goal improvements are sought on anode-furnace tuyere-area refractory performance. Kennecott and Praxair developed high pressure nitrogen refining for the Oxidation Stage which shortened anode furnace fire refining cycles by up to two hours per cycle. Future developments include optimizing the Reduction Stage’s steam-gas reforming and achieving coherent jet tuyereless refining.

By G. Gao

Flyash from municipal solid waste (MSW) incinerators is frequently classified as a characteristic hazardous waste due to its lead and cadmium content. Extensive investigation has therefore been carried out to detoxity the flyash by leaching and to recover lead, cadmium and zinc. Detoxification can be accomplished by leaching in HCI/NaCI solutions. Optimization of leaching conditions for effective detoxification and subsequent metal recovery can be achieved by controlling the acidity of the lixiviant and flyash to lixivaint ratio. Lead and cadmium In the leaching solution is recovered by cementation with zinc dust. Leaching and cementation experiments have shown that zinc concentrations suitable for electrowinning, > 15 g/liter, can be achieved. Experiments have also been performed to determine the effects of pH, particle size of the zinc dust used, quantity of zinc added and dissolved impurities on the cementation kinetics. After recovery of lead and cadmium, electrowinning or electrowinning coupled with solvent extraction can be used to recover zinc. A process flowsheet is presented.

Jan 1, 1991

By Ravi S. Bellur-Ramaswamy, Daniel A. Tortorelli, Robert Haber, Nahil A. Sobh

We optimize continuous quench process parameters to produce functionally graded aluminum alloy extrudates. To perform this task, an optimization problem is defined and solved using a standard nonlinear programming algorithm. Ingredients of this algorithm include 1) the process parameters to be optimized, 2) a cost function: the weighted average of the precipitate number density distribution, 3) constraint functions to limit the temperature gradient (and hence distortion and residual stress) and exit temperature, and 4) their sensitivities with respect to the process parameters. The cost and constraint functions are dependent on the temperature and precipitate size which are obtained by balancing energy to determine the temperature distribution and by using a reaction-rate theory to determine the precipitate particle sizes and their distributions. Both the temperature and the precipitate models are solved via the discontinuous Galerkin finite element method. The energy balance incorporates nonlinear boundary conditions and material properties. The temperature field is then used in the reaction rate model which has as many as 105 degrees of- freedom per finite element node. After computing the temperature and precipitate size distributions we must compute their sensitivities. This seemingly intractable computational task is resolved thanks to the discontinuous Galerkin finite element formulation and the direct differentiation sensitivity method. A three-dimension example is provided to demonstrate the algorithm.

Jan 1, 2001

By Feng Liu

A thermal upgrading process by which nickel value can be concentrated in a ferronickel alloy is a possible alternative to treat Sudbury pyrrhotite (Po) tailings with nickel content of 0.5–1.5 wt%. The basis of this process is precipitation of Ni from Po at high temperature once Fe/S ratio in the iron-deficient Po is shifted towards stoichiometric or near stoichiometric FeS (troilite) either by the addition of iron and/or the removal of sulfur. For the iron addition route, the reaction between elemental iron and nickeliferous pyrrhotite to produce ferronickel alloy and Ni-depleted iron sulfide phase plays a critical rule. In this paper, the formation mechanism of ferronickel alloy was investigated using the diffusion couple technique to better understand the nickel diffusion behavior in the iron and sulfide phases.

By Yuhsuke Mizukami

Crude high Cr containing steel such as tool steel, heat-resistant steel or stainless steel is produced by dissolution of high carbon ferro-chromium into molten crude steel. In the refining process, decarburization is performed at the first stage, and deoxidation is followed in the next stage. Therefore, the equilibrium relation between dissolved Cr and 0 in molten Fe-Cr alloy after decarburization is very important when yield of deoxidizer is considered for the ovemll control and optimization of the process. It is well known that the yield of deoxidizer does strongly depend on the kinds of refractories of furnace in the secondary refining process. In the present work, the equilibrium relation between dissolved Cr and O in molten Fe-Cr alloy has been measured in a Cr2O3, MgO or Al2O3 crucible at steelmaking temperature. O contents at given Fe-Cr components have been lower in order of Cr2O3, Al2O3 and MgO crucible. The present results have been discussed based on the activities of the constituents in pure solid Cr2O3, and FeO-Cr2O3, MgO Cr2O3 and (AI,Cr)2O3 solid solutions.

Jan 1, 2003

By Richard D. Hangi

Process mineralogy techniques are uniquely applicable to industrial problems related to the extractive metallurgy of nickel, cobalt, and associated metals. Reflected 1ight microscopy, together with selected determinations by scanning electron microscopy-energy dispersive spectrographic analysis and electron probe microanalysis, provides the means to identify the ore minerals cobalt and nickel ores, determine the abundance of each ore mineral, assess the extent of intergrowth between the cobalt and nickel minerals and other ore and gangue minerals in the ores and concentrates, and predict the potential success of cobalt and nickel extraction by grinding, flotation, pyrometallurgical, and hydrometallurgical treatments. In addition, the extent of locking of the cobalt and nickel minerals with each other and with the gangue minerals can be directly observed by reflected light microscopy. Where ores have been treated by hydrometallurgical procedures, reflected light microscopy can serve to determine the causes of excessive leach consumption. Finally, the partitioning of cobalt and nickel between high-temperature synthetic phases produced by pyrometallurgical treatment can be precisely determined by process mineralogy techniques. Case histories from cobalt and nickel deposits illustrate the value of applied mineralogical techniques in the study of cobalt and nickel ores, beneficiation, hydrometallurgial, and pyrometallurgical products.

Jan 1, 1993

By Jorge Alberto Soares Tenório, Viviane Tavares de Moraes, Denise Crocce Romano Espinosa, Franco Alves Lavacchini Ramunno

"The traditional process for recovery of metals from waste electric and electronic equipment (WEEE) usually involves pyrometallurgical processing. However, the application of this technology to processing waste printed circuit boards (WPCBs) might lead to the formation of dioxins and furans, due to thermal degradation of flame-retardants and polymeric resins present in the board substrate. Therefore, this paper proposes a hydrometallurgical route for the recovery of copper. The acid leaching behavior of copper has been investigated at three different temperatures (25°C, 50°C and 75°C) with and without the addition of an oxidizing agent (hydrogen peroxide - H202). The dissolution kinetics for acid copper leaching was calculated based on chemical analysis by ICP-OES (Inductively Coupled Plasma - Optical Emission Spectroscopy). At 50°C with 1 mol/L H2S04 added 10 mL H202 (30%) each half hour under pulp density of 1 g I 10 mL, 100% of copper was extracted after 3 hours. The dissolution kinetics of copper with H2SO4-H2O 2 followed 1 - (1 - X)113 =Ket, i.e. chemically controlled reaction model.IntroductionThe information regarding the generation of waste electric and electronic equipment (WEEE) are still difficult to obtain because the estimates should take into consideration the historical production and sale of various products and the rate at which they reach the end of their life cycle, whose duration depends on the behavior of consumers [1]. Thus, the estimated overall WEEE generation varies between 25 and 50 million tons each year, which corresponds to more than 5% of all municipal waste generated [2], and this amount will increase at a rate of 3 to 5% per year, approximately three times faster than other individual types of waste [3].Printed circuit boards (PCBs) are essential parts of electric and electronic equipment (EEE), being found in virtually all electronic products, as well as in weapons systems [4]. A PCB is a basic component, which consists of a board where copper tracks are deposited. While the board behaves as an electrical insulator, the tracks connect electrically the various components attached to the board [ 5]. In addition to glass fibers, paper and resins, the PCBs contain significant amounts of metals, such as copper, iron, nickel, lead, stain, silver, gold and palladium [6]. In general, the weight fraction of metal is around 28% and the remainder of the boards is composed of plastic (19%), bromine (as flame retardant - 4%) and ceramic material (49%) [7]."

Jan 1, 2014

By Xuan Cheng

The electrochemistry of sulfide mineral flotation is reviewed with particular emphasis on galvanic interaction among minerals and grinding media, and its relevance to flotation of complex sulfide ores is discussed. Surface alteration due to galvanic interactions among chalcopyrite, pyrrhotite and mild steel is analyzed in terms of voltammetric and chronoamperometric studies on individual minerals and through galvanic current measurements in 2- and 3- electrode combinations. The results are related to laboratory flotation behaviors of chalcopyrite-pyrrhotite mixtures simulating copper-nickel bearing Duluth gabbro.

Jan 1, 1993

By Alberto Oalvez, Lucya Yunus, Pengfii Tan

"Laboratory flotation tests of slow cooled converter slag have showed that 92.5% copper recovery at the copper cut-off grade of 24 - 25 % can be achieved by using a 50:50 ratio of DSP330 and SIBX (sodium isobutyl xanthate) at the natural pH of 7 and with a grinding time of 18.5 minutes. 70ìéç is the P80 achieved at this grinding time. MIBC is the frother and the solid content of the flotation feed was 46%. In the plant trials, two types of collectors at two different feed particle sizes for both the normal and slow cooled slag were operated. The particle size was controlled by the feed rate. The P80 of 75 ìçé at a feed rate between 32 - 36 t/h were tested. The plant trials have demonstrated that the copper recovery in the milling and flotation process of the slow cooled slags was improved by 3%. IntroductionIt is proposed to float the slow cooled converter slag, in the auxiliary circuit of the copper concentrator at Mount Isa, by using the processing conditions identified from several laboratory flotation tests. Among these laboratory tests, one produced a copper recovery of 4 % higher than those achieved from a normal cooled slag with the same slag feed grade and the same copper content (24 - 26 %) in the concentrate. These test conditions were selected for further studies.Laboratory Test Work and Plant TrialsThere has been a lot of work conducted under laboratory and plant conditions [1]. However, the achieved results did not justify their total implementation in the Mount Isa Copper Concentrator. Initially, the lab trials were carried out with slag cooled 100% in air; then it was changed to combined cooling for 12 h with air and 2.5 days with water sprays. The reason for this change was the shortage of space when the slag was cooled 100% in air, as it takes several days to achieve safe temperatures for its removal. The San Manuel Copper Smelter has reported that their slag was left for air cooling in pits for 8 h and then was followed by water cooling for 2-3 days [2]"

Jan 1, 2012

By Jim Hardy, Tim McKnight

"The thermal mass flow controller, or MFC, has become an instrument of choice for the monitoring and controlling of process gas flow throughout the materials processing industry. In the semiconductor industry, these MFCs are used on over 70% of the processing tools. Reliability and accuracy are major concerns for the users of the MFCs. Calibration and characterization technologies for the development and implementation of mass flow devices are described. Sources of inaccuracy in process gas handling are described, and a model to correct for these inaccuracies is outlined. A gravimetric calibrator is described that allows flow sensors to be calibrated in corrosive, reactive gases to an accuracy of 0.3% of reading, at least an order of magnitude better than previously possible. All described capabilities are implemented in a Department of Energy User Facility which is available to industry and universities to test and develop gas flow sensors and controllers and evaluate their performance related to environmental effects, reliability, reproducibility, and accuracy.IntroductionMaterials processing is at the heart of semiconductor manufacturing. To make today's advanced integrated circuits, silicon wafers are subjected to over 200 process steps. Most of these steps involve processes such as etching, implanting, diffusion, annealing, deposition, and lithography (resist deposition and hardening). Often one or more process gases are used to complete the process step. To achieve the quality and performance required in the micro devices, accurate measurement and control of these gases is essential. The Oak Ridge National Laboratory (ORNL), in conjunction with the semiconductor industry, has been working to improve process gas measurement and control accuracy and reliability. Standardized test methods have been developed to characterize and benchmark the performance of mass flow controllers (MFCs), the method of choice for monitoring and controlling gas delivery. Testbeds have been designed and fabricated to produce repeatable and accurate data using these standards. Baseline testing was performed along with development of a unique mass flow instrument, the gravimetric calibrator."

Jan 1, 1997

By G. H. Khoe

Neutralisation of acid uranium mill tailings with lime or other alkaline materials is usually practised to reduce the dissolved concentration of heavy metals and radio nuclides. Computer modelling of this process was carried out using the geochemical equilibrium code MINTEQA2. Computed dissolved metal and sulfate concentrations were compared with laboratory-based experimental data. It was found necessary to include the modelling of adsorption of trace metals (such as uranium and lead) by the precipitated ferric hydroxide in order to obtain acceptable concentrations in the neutralised liquors. There were limitations of the modelling exercise due to important aspects which were not addressed or properly accounted for such as chemical reaction kinetics and the effect of high ionic strength. These are discussed in the paper.

Jan 1, 1991