Search Documents

By Hiroyuki Matsuura

Treatment of electric arc furnace (EAF) dusts has become an important issue from the viewpoint of the environmental protection and recycling of variable resources because these dusts contain considerable amount of zinc and lead. A new recovery process of these metals has been proposed, in which the metals in the dusts react with waste polyvinyl chloride to form metal chlorides. Therefore, it is important to clarify the physicochemical properties and behaviors of zinc, lead and those chlorides and oxychlorides. In the present study, the kinetics of chlorination of ZnO, PbO and ZnFe2O4 mainly contained in the EAF dusts were investigated at 1023 K to 1273 K with Ar-O2-Cl2 gas. Based on these results, the selective chlorination and evaporation process of zinc and lead from the mixture of Fe2O3-ZnFe2O4-ZnO-PbO was examined and the high efficiency of selectivity has been demonstrated.

Jan 1, 2006

By Vinod K. Namilakonda

In situ synthesis of discontinuously reinforced aluminum alloy metal matrix composites was investigated. Aluminum alloy (A356: Al-7 wt% Si) was reinforced with dispersed AlN particles. Thermodynamic calculations were made for the composition determination of various phases formed during bubbling of NH3 gas into the Al alloy melts in the temperature range 1173-1473 K. Experiments were carried out for in situ production of AlN particles with the reaction between Al melt and NH3 gas in high temperature resistance furnace at 1473 K. The products were characterized using SEM, EDS and XRD. Effect of bubbling time of NH3 gas on the AlN formed in the composites was studied. The amount of AlN reinforcement in the Al alloy composites was observed to be in the range of 5 to 35 wt%. Good agreement was observed between the experimental and thermodynamic calculated data on the composition of AlN in Al alloy composites.

Jan 1, 2006

By Kimio Itagaki, Makoto Ohtsuka, Kouki Chiba, Minoru Matsumoto

"The properties of Ni-Mn-Ga films such as chemical composition, crystal structure, microstructure and transformation temperature were investigated with respect to sputtering conditions in the present study. The Ni-Mn-Ga films were deposited on a polyvinyl alcohol substrate with a radio-frequency magnetron sputtering apparatus using the NisoMn2sGa2s and Nis2Mn:«1Ga24 targets. After separating from the substrates, the films were annealed at the temperature between 873 and 1273 K for 3.6 ks. The chemical composition of the films depended on the radiofrequency generating power, however, there was no dependence on the heat treatment temperature. Each deposited film had a columnar grain structure. After heat treatment, the width of columnar grains widened and then became indistinct with increasing heat treatment temperature. The Heusler type cubic crystal structure of the fi4n with heat treatment at 1073 K changed to the tetragonal one through the martensitic structural transformation during cooling. The martensitic structural transformation temperature increased with increasing nickel content of films, while the Curie temperature decreased. The film obtained at 200 W using the Nis2Mn24Ga24 target after heat treatment at 1073 K showed one-way shape memory effect through the reverse martensitic structural transformation during heating.IntroductionThe ternary intermetallic compound NiiMnGa has a Heusler-type crystal structure and is an intelligent material, which has a shape memory effect and a ferromagnetic property. The martensitic structural transformation occurs within the ferromagnetic temperature region. The cubic crystal structure of L21 at high temperature changes to a tetragonal one through the martehsitic structural transformation during cooling. The films of this compound can be applied for an actuator of micro-machines."

Jan 1, 2000

By Gopalakrishna B. Prabhu, David L. Bourell

"Three mol% Yttria-Stabilized Tetragonal Zirconia (YSTZ) was prepared by a sol-gel synthesis technique using zirconium tetrachloride and hydrated yttrium chloride precursors. After drying and annealing at 823K, the particle size was in the range 10 to 20 nm. The zirconia powder was sintered using a uniaxial hot press at an applied stress of 20 to 40 MPa. One hour, isothermal sintering was performed in air after initial heating at 50K/min. Theoretical density was obtained at densification temperatures above 1498K. After sintering, grain coarsening characteristics were studied using constant heating rate anneals followed by quenching, based on a model for grain coarsening in a linear heating rate cycle. The microstructural change was studied using SEM and TEM and the phases were determined using x-ray diffraction.IntroductionThe ability to sinter nanocrystalline materials to full density several hundred degrees below the normal sintering temperatures is one reason for their current interest. [1-5] Yttria Stabilized Tetragonal Zirconia (YSTZ) of grain size of about 300 nm has exhibited superplasticity, with elongations as large as 800%.[6-7] Fine grain size is critical for superplasticity. Retention of the fine grain size during sintering of nanocrystalline powder is important if a material is to exhibit superplasticity or to exhibit physical or mechanical properties associated with the ultra fine structure. This paper investigates the sintering behavior and the grain coarsening characteristics ofnanocrystalline YSTZ.Techniques for synthesizing nanocrystalline materials have been studied in great detail earlier. [8-12] The techniques used to synthesize nanocrystalline zirconia include alkoxide synthesis [9], the chloride method [11], the peroxide method [13] and the acetone-toluene method. [13] In this paper the method used in the synthesis of zirconia is the chloride technique. With this precipitation technique, either zirconium chloride or oxychloride and a corresponding yttrium salt or even pure yttria are used."

Jan 1, 1994

By R. Rajiv Srivastava

Brine leaching of a TSL processed zinc-plant residue (ZPR), containing 83.3% anglesite, has been investigated for lead recovery. A prior treatment of ZPR in acid solution did not show any significant effect of acid concentration in zinc dissolution. The study reveals that the solubility limits of PbCl2 is as an important factor with respect to the brine concentration and pulp density in lixiviant. The dissociated sulfate ions hinder the formation of PbCl2 on prolong leaching (above 60 min), while exhibiting the reverse solubility of lead as PbSO4. A 3-step leaching process could yield >92% leaching efficiency when the parameters were maintained as: 10% pulp density in a 250 g/L NaCl solution, 80 °C temperature, and 60 min time. This leaves the insoluble ferrite, sulfides and oxy-sulfates of zinc and lead in the final residue as revealed by the XRD characterization.

By D. Georgiou

Direct sulphuric acid leaching of nickeliferous limonites is the process of choice to recover nickel and cobalt from equatorially located lateritic ores. These ores are rich-in-iron (-45 wt%) existing in the form of goethite enriched with nickel. The merit of this process is due to its high nickel selectivity because of simultaneous iron separation and acid regeneration. Under acid leaching conditions (-250 to 270°C) iron follows an acid dissolution-hydrolytic precipitation path yielding a very low concentration level depending on temperature and acidity of the final leach liquor. The primary precipitation product of iron is hematite which also forms as a scale on reactor internals along with co-existing aluminum. In this paper, an overview of the behaviour of iron solid products under process conditions is made. The evolution of goethite to hematite transformation, as well as the role of iron in reactor scale production, are studied using SEM/EDX characterization techniques.

Jan 1, 1995

By R. J. Kuczynski

The U.S. Bureau of Mines operated a 2,000-9 (4.4-lb) batch process development unit for recovering platinum-group metals (PGM) from automobile catalysts. Virgin monolith, used pellet and used monolith catalyst samples were tested. Leaching twice with 1-pct sodium cyanide (NaCN) solution at 160' C for 1 h in a pressure vessel dissolved over 95 pct of the PGM from virgin catalysts and over 90 pct from used pellet catalysts. Over 85 pct of the PGM was dissolved from used monolith catalysts when a third leaching step was added. PGM concentrates as metallic powder containing over 99.8 pct of the dissolved PGM and analyzing greater than 70 pct PGM were recovered by heating the pregnant leach solutions from virgin catalysts to 250' C and used catalyst to 275" C for 1 h. The solution after heating contained primarily sodium carbonate from cyanide decomposition and less than 0.2 ppm total cyanide.

Jan 1, 1993

By Sunil Jayasekera

This paper describes the results of a study carried out to examine the feasibility of electrolytic recovery of silver from cyanide leach liquor generated from a Western Australian silver mine tailings using a novel high mass transfer electrowinning cell. The proposed circuit involves heap leaching and electrowinning in a closed loop. The filter-press-like closed electrode arrangement of the cell allowed much improved mass transfer of metal ions to the cathode surface, making direct electrowinning of metals from dilute solutions feasible. The tests were conducted both in the laboratory and at large scale using a prototype with ~1.0 m2 cathode area. The results showed that the recovery of silver from as low as 250 mg L-1tenor was feasible. The silver deposit produced with the prototype cell was non-adherent and powdery and could be readily removed from the closed cell. A system was developed so that silver powder was discharged continuously during the run.

Jan 1, 2003

By V. G. Papangelakis

The implementation of a flow-through yttria-stabilized zirconia (YSZ) sensor for pH measurements in high temperature and concentrated electrolyte systems relevant to hydrometallurgical processing of nickeliferous laterites is discussed. Instrumentation involved the use of a custom made flow-through titanium electrochemical cell. Accuracy and validity of the pH measurements at temperatures up to 250C were assessed using concentrated sulphate process solutions ranging from synthetic binary sulphuric acid ? water solutions to progressively multicomponent metal ? sulphate solutions simulating laterite Pressure Acid Leach conditions. The measurements were also compared with theoretical models using recently obtained thermodynamic data. A difference of ±0.25 pH units was observed between measured and calculated pH values at temperatures. This is an acceptable difference given that these are the first direct high temperature pH measurements ever on the concentrated acidic sulphate solutions. This result is encouraging more research for the development of industrial electrochemical systems for direct pH measurements in autoclaves.

Jan 1, 2003

By J. W. Dini

Introduction The mission of the Materials Fabrication Division (MFD) is to provide fabrication services and technology in support of all programs at Lawrence Livermore National Laboratory (LLNL). MFD involvement is called for when fabrication activity requires levels of expertise, technology, equipment, process development, hazardous processes, security, or scheduling that is typically not commercially available. Customers are encouraged to utilize private industry for fabrication activity requiring routine processing or for production applications. MFD is .a large diversified service organization including approximately 400 full time employees. The group provides a wide variety of processes including all common machining and fabrications operations, laser and water jet cutting, electrical discharge machining, lapping, electron beam and laser welding, vacuum brazing, heat treating, forming, electroplating and metal finishing, optical polishing and grinding, vacuum coating, vacuum engineering and a variety of plastics operations. These operations occupy more than 1,250,000 square feet of floor space. For more detail on the many fabrication related services available from MFD, see Reference 1.

Jan 1, 1992

By Gerardo R. F. Alvear, Alistair S. Burrows, Stanko Nikolic, James S. Edwards

"The copper ISASMELT™ process has evolved over more than a quarter of a century and can now be considered mainstream, with single furnaces producing more than 340,000 tpa of copper in matte. The next evolutionary step for the ISASMELT™ technology is to directly challenge the dominance of the Peirce-Smith converter by the implementation of a continuous copper converting process on a commercial scale. The present work describes the status of the continuous converting process – ISACONVERT™.Continuous converting has been performed successfully in pilot scale ISACONVERT™ plants, where operating results have verified the predictions of fundamental research and reinforced the underlying confidence in the design parameters. From a matte feed rate of 250 kg/hr, a calcium ferrite slag and a low-sulfur blister have been produced. Design is now complete for the first commercial application of the ISACONVERT™ process. The present paper describes the status of ISACONVERT™ by summarising results of recent pilot plant tests and describing the first commercial plant design."

Jan 1, 2009

By Neal Schwartz, Robert De Saro, Richard Rosenthal, Ed Kear

"A Stack Melter has been installed and is currently operating at Lexington Die Casting. The Stack Melter consists of a 1 meter (3 foot) diameter refractory tube, 2 meters (7 feet) high. Specification ingots are continuously fed to the top of the melter and piled to nearly the top. A burner fires through the scrap which melts the lower portion and preheats the upper portion. As the lower portion is melted, it is drawn out and the upper preheated scrap falls to a lower level where it in tum melts. The molten metal is fed to one of two holding furnaces for eventual delivery to a casting machine.The Stack Melter's energy use is approximately 2900 joules/g (1,250 Btu/lbm), resulting in an overall energy savings of about 58%. This energy savings is brought about primarily because the flue gases preheat the scrap and the flue gas temperature is dropped to well under 528°C (1000°F)."

Jan 1, 2000

By Takayuki Watanabe, Yoshiki Shimizu, Yusuke Moriyoshi

"B-C-N nanotubes prepared by a flush evaporation method using a de arc plasma were mainly characterized by transmission electron microscopy (TEM) and electron energy· loss spectroscopy (EELS). The nanotubes obtained· were divided into three types such as carbon boron nitride and carbon or carbon nanotubes surrounded with boron nitride nanotubes. These types of nanotubes were obtained at higher temperatures than about 3000 K, however, these were not formed at lower temperatures than about 3000K. On the other hand, 11anocapsules were· formed at all the experimental temperatures and nanocapsules with a homogeneous phase were obtained at lower temperatures than about 3000 K. The effect of additives on the formation of B-C-N nanotubes was not clear. Based on these experimental data depending on temperatures and corresponding microstructures, the formation mechanisms of both nanotubes and nanocapsules were briefly .discussed 1 Introduction As reported previously, nano tubes have unique electrical properties1, 3) The preparations of nallotupes have been usually carried out by flush evaporation methods using either a de arc plasma or a laser4 -5) By these methods the reaction rate is so rarid that we have no data of intermediate products between initial raw materials and. final products of nanotubes 6-9). So, the formation mechanisms of nanotubes have been mainly speculated only from the microstructures of resultant nanoiubes. In order to have more reliable formation mechanisms, it is particularly important to have the information of intermediate products at the corresponding temperatures. From the viewpoints, we have studied about the effects of temperatures on the preparation of nanolubes. Here we report mi firstly some problems on the preparation of B-C-N nanotubes 10), secondly the effects of temperatures on the preparation of B-C-N nanotubes, and finally the formation mechanisms of nanotubes."

Jan 1, 2000

By Marcel Sturzenegger

Though the extraction of copper is well established, generation of sulfur dioxide (S02) is still a troublesome issue. Conventional processes are further challenged by the increasing amount of impurities in the concentrates. Direct decomposition of the metal sulfides into the metal(s) and elemental sulfur under concentrated solar radiation offers a promising path to solve both problems. Thermogravimetric measurements under inert atmospheres have shown that synthetic chalcocite or chalcopyrite yield copper at temperatures as low as 1773 K. Even though optimum reaction temperatures might be somewhat higher, such temperatures are straightforwardly accessible in solar chemical reactors. The absence of oxygen will reduce the extent of slag forming reactions and thereby alter the evaporation characteristics of volatile impurities such as arsenic or antimony. Chemical equilibrium calculations for a chalcopyrite-enargite feed, e.g., have shown that under inert atmospheres arsenic compounds are completely evaporated at temperatures above 1000 K and an effective separation of arsenic from the matte is expected. An important step towards a solar production of copper is the design and testing of prototype solar chemical reactors for this reaction. Numerical modeling is a key tool supporting a rational design but it requires data of the high-temperature properties that prevail in these processes. Development of techniques for determining the essential quantities such as decomposition rates or radiative properties at temperatures up to 2000 K is therefore a main activity in our laboratory in order to control and optimize the process. Though developed in the frame of high-temperature solar technology, the experimental techniques are also suited to advance the understanding of conventional high-temperature processes. Keywords: Solar technology, Sulfur dioxide, Solar Radiation, Thermogravimetry, Chalcocite, Chalcopyrite, Numerical modeling.

Jan 1, 2003

By P. N. Anyalebechi

The effects of solidification rate on the cast microstructures of aluminum alloys 6009 and 6016 have been investigated with directionally cooled laboratory-size ingots, at 0.2-10.1 K/s and 0.4- 23.1 K/s, respectively. These ranges of solidification rate are within those observed in commercial-size ingots. In both alloys, the average dendrite cell size and second phase particle size decreased with increase in average solidification rate and with a decrease in average local solidification time. However, at comparable solidification rates, the dendrite cells and second phase particles are finer in the shorter freezing range alloy 6009 than in the longer freezing range alloy 6016. This is provisionally attributed to the earlier formation of second phase intermetallics at higher temperatures during solidification and to the formation of greater amount of the relatively coarse plate-like ß -phase (Al9Fe2Si4) phases in alloy 6016. In general, in both alloys, the types and relative amounts of the second phase particles in both alloys are independent of solidification rate.

Jan 1, 2006

By A. A. el-Geassy

High-grade iron ore fines rejected from the DRl plants (>96%Fe20) were isothermally reduced in 30-60%COIH2 gas mixtures at 973-1273K. The freshly reduced reaction products were then subsequently carburised in either H2/CO or H2/CO/S mixtures at 823-1073K for 30-120 min. The thermogarvimetric technique was used to follow up both of reduction and carburisation reactions as a function of time. The carburised samples were characterized by X-ray and Mossbauer techniques. Chemical and carbon analyses were also applied. The influence of temperature and gas composition on the reduction behavior was investigated. The calculated values of apparent activation energy, application of gas-solid mathematical formulations were correlated with the microstructures to predict the reduction mechanism, The influence of carburization time, temperature, CO contents in H2/CO or H2/CO/S were investigated. A conversion extent of Fe to Fe3C was taken as a measurable index for the efficiency of carburization reaction under the different experimental conditions.

Jan 1, 2003

By A. A. EI-Geassy

High-grade iron ore fines rejected from the DRI plants (>96%Fe2O3) were isothermally reduced in 30-60%CO/H2 gas mixtures at 973-1273K. The freshly reduced reaction products were then subsequently carburised in either Hz/CO or H2/CO/S mixtures at 823-1 073K for 30-120 min. The thermogarvimetric technique was used to follow up both of reduction and carburisation reactions as a function of time. The carburised samples were characterized by X-ray and Mossbauer techniques. Chemical and carbon analyses were also applied. The influence of temperature and gas composition on the reduction behavior was investigated. The calculated values of apparent activation energy, application of gas-solid mathematical formulations were correlated with the microstructures to predict the reduetion mechanism. The influenee of carburization time, temperature, CO contents in H2/CO or H2/CO/S were investigated. A conversion extent of Fe to Fe3C was taken as a measurable index for the efficiency of carburization rcaction under the different experimental conditions.

Jan 1, 2003

By Ryokichi Shimpo

Much amount of sludge is produced from the wastewater treatments in surface finishing industry. There are many problems for the abandonment of the sludge because of the high water content and heavy metals included. It is often observed that hexavalent chromium, which is toxic, is generated in the course of heat treatments of the sludge for reducing its amount by dispersing water. In this study, conditions of the sludge calcinations for reducing water contents have been examined. Maximum hexavalent chromium generation was observed in the temperature range around 773 K, at which most of the crystallization water decomposed from the sludge. When the heating temperature became higher than 1173 K, the amount of the hexavalent chromium extracted from the calcined sludge became as low as 10 mg/kg sludge. When the sludge was heated with iron oxides, FeO or Fe203, iron ferrite has been synthesized which may be used as a magnetic material. The amounts of hexavalent chromium generated in the heat treatment with iron oxides were not much different from those without iron oxides.

Jan 1, 2003

By Lloyd R. Nelson

Experimental results of three-phase mixing in a physical model of a CCRL for metals refining are presented. The system was operated above a critical lower liquid height-to- width ratio (H,/W) of unity, with adequate bottom gas injection through a line of central, single tuyeres (Q,/A = 7.5 cm/min, or c = 17 W/m3) to sustain levels of interphase transport considered appropriate to an industrial pyrometallurgical refining operation. The application of a thermal tracer technique to elucidate both longitudinal mixing and interphase heat transfer is discussed. The results indicate that even under conditions of significant bottom gas injection, it should be possible to maintain acceptably low longitudinal mixing 1 (D, < 20 cm /s and D,/uL < 0.1) in the CCRL. Interphase mass transfer coefficients of the order of 0.004 cm/s are predicted from the measured interphase heat transfer coefficients (h = 1.3 to 2.0 kW/m2K), using the heat and mass transfer analogy. Adequate rates of rehning are predicted for an industrial CCRL operated under such conditions.

Jan 1, 1995

By Dimitrios Fillippou

Magnesium hydroxide is used in a number of industrial applications, from the neutralisation of acid effluents to the production of pharmaceuticals. High-quality magnesium hydroxide powders can be produced by hydrating slow-reacting magnesia in dilute magnesium acetate solutions. The process of magnesia hydration shows many similarities with a typical hydrometallurgical leaching operation; however, its kinetics are crucial not only for process design and control, but also for the production of powders with a desirable particle morphology. This article shows the results of an experimental work whereby industrial heavily-burned magnesia powders were hydrated in 0.01 to 0.1 mol/L magnesium acetate solutions at temperatures ranging between 333 and 363 K. Examination of the magnesium hydroxide produced and the analysis of the kinetic data suggest that the hydration of heavily-burned magnesia in magnesium acetate solutions is a dissolution-precipitation process controlled by the dissolution of magnesia particles. The activation energy was estimated to be 60 kJ/mol, while the reaction order with respect to magnesium acetate concentration was found to be about one.

Jan 1, 1999