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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 Musa Karakus

Zirconia-based refractorics arc finding increasing use for specialized applications in steelmaking technology, making optimization of their resistance to corrosion by steelmaking slags more important. Samples of calcia- and magnesia-stabilized zirconia refractories have been exposed to slags in the CaO - FeO - SiO, system at 155WC for the purposes of measuring corrosion rates. Examination by SEM/EDX and cathodoluminescence of the mineralogy of the attacked specimens reveals important clues about the mechanism of attack.

Jan 1, 1992

By M. Rubinstein, N. C. Koon, B. N. Das, V. G. Harris

"Copper and gold - based alloys having giant magnetoresistance properties were produced by melt spinning from arc melted and cast rods. The ribbon width varied between 1 and 2 mm and the ribbon thicknesses were in the range of 30 to 50 11m. The uniform microstructure of the cast rods indicated the composition homogeneity in the starting material. The ribbons showed composition uniformity across the cross section from EDX analysis. However, the spun ribbon microstructure changed from a 'frozen in' region near the wheel side to a nanosize spherically precipitated phase towards the freely frozen surface. The evolution of the microstructure from the spun ribbon state to the annealed ones was studied by optical microscopy, SEM and TEM. The structural information of the spun and annealed specimens was obtained from X - ray, electron diffraction, electron microscopy and ferromagnetic resonance. Magnetoresistance was measured by the four point probe method.IntroductionRecently. Giant Magnetoresistance. GMR. has been observed in sputtered thin films alloys of Ag. Au and Cu with Co and Fe [1. 2. 3]. The sputtered films are produced by condensation of the alloys from the vapor phase. These Ag. Au and Cu alloys are miscible and homogeneous in the vapor and liquid phase (except Ag alloys which exhibit phase separation even in the liquid phase) but immiscible and heterogeneous in the solid phase. In our work we have produced thin ribbons of the Cu and Au alloys about 30 µm thick from the miscible state in liquid phase by rapid solidification melt spinning. The microstructural development of the ribbons was investigated in the as - spun condition and on annealing. The other properties such as magnetization. GMR and Mossbauer Spectroscopy were also investigated in the various microstructural conditions of the ribbons."

Jan 1, 1994

By R. D. Osmanson

A series of batch roasting tests was performed on minus 1/2 inch gold bearing refractory samples from the Gold Acres deposit, and 67 select particles were polished and the sulfide alterations were examined microscopically. The suite of specimens represents two hour batch roast treatments at 600°C, 700°C, 725°C, 750°c, 800°C, and 900°C. Auriferous pyrites were found to alter sequencially to pyrrhotite, magnetite and finally to hematite. It was found that the decrease in cyanidation extraction with high temperature roasting is likely due to the increas ing stability of magnetite and more crystalline hematite, and the decrease in porosity with these phases which occlude the gold. Gold has been noted to occur very early in the mineralizing sequence, with gold being found in quartz and in clay/carbonate rock matrix. No gold was found in the two pyrite phases, but numerous gold grains were found in pyrrhotite after pyrite and in subsequent iron oxides. Gold mineralization had apparently ended by the time base metals were introduced into the deposit.

Jan 1, 1987

By Bo Björkman

Four different arsenic containing dusts from the Boliden plant, Boliden mineral AB, Sweden have been examined. A kinetic study of the As elimination was performed in a laboratory scale roasting furnace for roasting furnace ESP dust and smelting furnace ESP dust. Characterisation and thermodynamic calculations were carried out to determine the mineralogy, and the stability of compounds in the dusts studied. The characterisation methods used were chemical analysis, X-ray diffraction analysis and microprobe analysis. It was found in the experiments that a high degree of As elimination was obtained for roasting fumace ESP dust and a low degree for smelting fumace ESP dust. Derived kinetic models are given. A prediction of the As-elimation for settling furnace dust and converter ventilation dust is presented.

Jan 1, 1994

By Kazuya Kitatani, Gen Sasaki, Naoto Ohta, Hideharu Fukunaga, Makoto Yoshida, Jin Pan, Kenya Nagahisa, Toshihiro Ishikawa

"A sintered SiC (Tyranno-SA) fiber-reinforced MAS glass matrix composite was fabricated by using a slurry infiltration method and hot-pressing. The microstructure and mechanical properties were investigated: To prepare the preform, the MAS glass slurry including a dispersing agent was infiltrated into a bundle of the fibers. The preform was then hot-pressed under the conditions of 1473 K, 30 MPa, 3.6 ksec. A unidirectionally-reinforced oxide matrix composite with 50% Vf. of the fiber and a density of 2.84 g/cm3 was obtained. As the mechanical properties at room temperature, the three-point flexural strength- and quasi-static adsorbed energy were 500 MPa arid 6,000 J/m2, respectively. Without graphite or an h-BN pre-coating on the surface of the fiber, pull-out and bridging of the fibers from the matrix was found, and this leads to a high value of the adsorbed energy. By TEM observation, nano-scale crystalline products were found between the fibers and the glass matrix. The push-out test reveals that this layer causes the appropriate debonding of the interface during the fracture process of the composite.Introduction It is known that the CFCCs (continuous-fiber-reinforced ceramic matrix composites) are characterized by their non-linear fracture behavior, which is' hardly found in monolithic ceramic materials. It is inevitable for the CFCCs to exhibit a large fracture toughness so 'that debonding of the fiber/matrix interface; pull-out and bridging of the fibers then' occurs during the fracture process. This series of fracture behavior is known as the so-called ""the mechanism of toughening of the CFCCs"". Thus, different from the MMCs in which strong interfacial bonding is necessary, the interfacial strength of the CFCCs has to be controlled. As techniques for controlling the interfacial strength, it is also known that both a CVD-graphite coating and an h-BN coating are effective to induce the mechanism of toughening[1,2]. In the case, of the Si-C-O or Si-Ti-C-O fibers/glass or crystalline oxide matrix composites, it is reported that the formation of the in-situ graphite layer, which is also effective to increase the fracture toughness of the CFCCs, is often found during the fabrication process such as hot-pressing. The lower the crystallinity of the Si-C-O fibers, the higher is the tendency to form the in-situ graphite layer as found by the chemical reaction between the fibers and the glass matrices[3-12]. On the-other hand crystallized stoichiometric 'SiC fibers are attractive for high temperature service because of the higher phase stability compared to the Si¬C-O or Si-Ti-C-O fibers. However, in the previous, studies, the mechanical properties and the interfacial chemical reaction of the crystallized SiC fibers / glass matrix Composites have still been unknown. In this study, a polycrystalline 'sintered SiC fiber-reinforced MAS glass composite was fabricated. The mechanical properties and microstructure were then investigated. The slurry infiltration technique followed by hot-pressing was used to prepare the composites. The formation of the in-situ graphite layer and the relationship between microstructure and mechanical properties at room temperature were examined by the TEM observation of the fiber/matrix interface."

Jan 1, 2000

By I. A. Ibrahim, A. K. Ismail, A. A. I. Afifi

"Synthetic rutile for paints industry is conventionally produced by a combined smelting and leaching process. Smelting process is an energy intensive step and represents economic burden in view of the increasing energy costs. Egyptian ilmenite ore containing 40% TiO2 and 38% total Fe was thus directly leached with sulphuric acid to produce eventually synthetic rutile. The process-involves digestion of the ore with sulphuric acid whereby both TiO2 and Fe are dissolved. The solution was then treated with iron powder to convert Fe3+ to Fe2+ to avoid co-precipitation of iron during the hydrolysis step. After solid/liquid separation and clarification, Fe was crystallized as ferrous sulphate hydrate by chilling. The titanium pregnant liquor was concentrated by evaporation and then hydrolyzed to precipitate hydrated titanium dioxide which was then calcined to produce synthetic rutile containing 98.6 TiO2 and 0.58% Fe2O 3. The optimum conditions of all the processing stages were determined.IntroductionSynthetic rutile for paints, welding rods and other industries could be produced from ilmenite ore by sulfuric acid leaching process. This process is a batch process and nearly 80% of all TiO2 produced in the world is made by this process [1]. Figure l shows simple block flowsheet of the process. The process involves the following stages.Digestion: In this stage, ilmenite ore is treated with concentrated sulfuric acid where both iron and titanium are converted to their respective sulfates according to the following equations:"

Jan 1, 2000

By Patrick R. Taylor

This investigation studied the inflight calcination kinetics of nuclear waste simulant using a thermal plasma reactor. A series of experiments were performed to determine the conversion of insoluble aluminum compounds to the soluble compounds and the decomposition of complex organic and nitrite compounds present in the simulant waste. Thermodynamic calculations based on free energy minimization were performed to establish a theoretical basis for this investigation. A kinetic model to describe the conversion of gibsite to sodium aluminate has been proposed. The products of the calcination were characterized using XRD, Gas Chromatography, and chemical analysis by ICP. The results of this investigation indicated 85% gibsite conversion to sodium aluminate, 90% of nitrate decomposition, 52% TOC decomposition and 90% conversion of chromium to soluble compounds. A process is identified for inflight calcination of wastes. Key words: Plasma, waste, simulant, calcination

Jan 1, 1996

By A. A. Hejja

The first part of this study deals with the importance of surface tension of slags produced in the smelting of sulphide concentrates. Theoretically the method of determining the surface tension of slags was laid down by Boni and Derge. The values obtained experimentally for a series of main oxide components were grouped into a useful correlation incorporating experimental constants for the relevant oxides present in the slag, some of these giving the surface tension value for the particular slag. These estimated values were coupled with or incorporated into the slag viscosity plots to show the correlation between the two factors. This is also important from a refractory attack point of view in the furnace operation. In the second part an attempt is made toward the optimisation of slag composition relevant for electric furnace smelting processes. Using the knowledge of the viscosity and electrical conductivity of the slags at the temperature of furnace operation, the mode of optimisation is based on correlations which utilize the trend of the mostly parabolic plots of viscosities and conductivities. The results obtained by this method agree well with the optimum slag compositions being used in established operations derived from years of practical experience for various slags used in the furnaces. However, due to extensive turbulence in suspension and gas injected bath smelting processes, the outlined methods cannot be used for these processes. Also great caution should be exercised in their application for three electrode circular furnaces with separate slag cleaning.

Jan 1, 1997

By G. A. Eltringham, A. F. Sarofim, A. A. Shook, M. P. Heap, B. R. Adams, K. A. Davis

This paper discusses the use of a reacting CFD model to determine chalcopyrite kinetics in a drop tube furnace and to predict the reaction of a chalcopyrite concentrate in the reaction shaft of an industrial smelter. Reacting CFD codes can be applied to determine the consequences of the interaction of gas with particles and therefore improve the ability to derive kinetic parameters that take into account the different temperature and oxidation histories that different particles will see. This paper describes the application of such a model to derive improved kinetic parameters for the pyrolysis and oxidation of chalcopyrite. The improved kinetic parameters derived from the drop tube studies are used to simulate chalcopyrite concentrate reactions in the reaction shaft of an industrial smelter. The reaction shaft model includes the effects of turbulent fluid mechanics, entrained flow mixing, turbulent particle dispersion, heterogeneous particle reactions, radiative and convective heat transfer, and surface and bath deposition rates. Particle reaction and composition characteristics are predicted as a function of particle trajectory and deposition and are used to aid in evaluating shaft performance.

Jan 1, 1999

By Hebi Yin

A two-dimensional finite element solidification model was developed to simulate the transport phenomena occurring during laser deposition of AISI 410 stainless steel during the Laser Engineered Net Shaping (LENS®) process. The molten pool geometry and the distribution of temperature, solute concentration and velocity were calculated during deposition of a thin wall plate. An analysis of the simulations results revealed the importance of heat transfer by both conduction and convection as well as the roles of the driving forces for convection in the molten pool. The heat transfer and the flow pattern in the molten pool are considerably dependent on the travel speed of the laser beam. For the alloy and process parameters in the simulations, no significant macrosegregation was observed. The temperature-dependent properties and thermodynamic variables involved in solidification modeling were calculated using Thermo-Calc software. The results of this work contribute to the current understanding of transport phenomena in the molten pool of laser deposition processes.

Jan 1, 2008

By P. S. Dunn, A. D. Rollett, H. D. Lewis

"The results of preliminary work on the modeling and measurement of the heat transfer coefficients of metal/mold interfaces is reported. The system investigated is the casting of uranium in graphite molds. The motivation for the work is primarily to improve the accuracy of process modeling of prototype mold designs at the Los Alamos Foundry. The evolution in design of a suitable mold for unidirectional solidification is described, illustrating the value of simulating mold designs prior to use. Experiment indicated a heat transfer coefficient of 2 kW/m /K both with and without superheat. It was possible to distinguish between solidification due to the mold and that due to radiative heat loss. This permitted an experimental estimate of the emissivity, ~ = 0.2, of the solidified metal.IntroductionA feature that distinguishes casting processes from welding processes is the presence of an interface with a low heat transfer coefficient between the mold and the casting. Especially when chill casting, the interface delays the start of solidification and increases freezing times significantly. By comparison welds can be assumed to have a very high heat transfer coefficient. The heat transfer coefficient controls such phenomena as folds and laps on the surface of castings which can be crucial to the acceptability of a casting. The time delay for the start of solidification influences the occurrence of cold shut defects. The standard mold material for uranium casting is high quality graphite which is an excellent refractory when used in vacuum and coated with a refractory wash. Graphite is an effective chill material and has a thermal diffusivity approximately twice that of uranium. Experience has shown that practicable superheat without mold pre-heat is not sufficient for avoiding cold shut defects when casting in graphite molds.TheoryIt is possible to calculate the position of the freeze front s, as a function of time, t, the superheat and interface heat transfer coefficient, h, [1]. However, the value of h cannot be obtained explicitly. The Virtual Adjunct Method (VAM) [2] offers a method for extending the standard equation for an insulating mold where s is proportional to the square root of time. By considering the effect of the interface to be equivalent to finite thicknesses of mold and metal, the following quadratic equation is obtained,"

Jan 1, 1986

By M. A. Llavona

In Spain, as in many countries, the gold content of jewellery must be officially hallmarked. The official methods of assay are gravimetnc cupellation (a method which is highly accurate but both time and sample consuming), potentiometry, gravimetry and volumetry. In this paper, a procedure for measuring gold by flame atomic absorption in jewellery samples is described. The method is based on the acid digestion of a 40 mg sample. The quantity of aqua regia necessary for dissolving the gold, the ideal weight of a sample in order that the error may be minimal, the effect of the acids employed, the type of material used for its storage, and the necessity of employing a buffer to avoid the ionization of the solution are described. The method proposed is simple, highly accurate and causes little damage to the jewellery.

Jan 1, 1999

By R. H. Hanewald

INMETCO, a subsidiary of Inco Limited, is the only facility in North America that provides High Temperature Metals Recovery for nickel-, chromium-, and iron-bearing wastes. Since 1978, this process has prevented more than 775,000 tons of materials from becoming part of the nation's waste stream. The paper describes Inco's experience in metals recovery, traces the development and explains the operation of the High Temperature Metals Recovery Process, and examines the procedures and criteria used to determine whether spent catalysts meet process feed specifications. An overview of the current requirements for transporting spent catalysts is provided. The paper concludes with brief case histories of catalysts users employing High Temperature Recovery to manage spent catalyst.

Jan 1, 1995

By Veneta Groudeva

A pyritic ore containing zinc, lead and copper as? the relevant primary sulfide minerals, .as well as gold and silver finely disseminated in the sulfide matrix, was? leached in percolation columns. Each column contained 30 kg of ore crushed to minus 10 mm. Firstly, zinc and copper were efficiently leached by means of chemolithothrophic bacteria? in acidic sulfate bearing medium. Zinc was leached more rapidly than copper but the final extractions of these metals were similar (about 75% in 300 days). A part of the galena was oxidized to the. insoluble lead sulfate during the leaching. The pyr:ite was, however, relatively slightly attacked. The ore was then leached by means of FeC11 - HCl solutions both in the presence and in the absence of bacteria to solubilize the lead. The chemolithotrophic bacteria grew in media containing both chloride and sulfat~ ions and maintained a high ferric to ferrous ion ratio in the percoiating solutions. The chemical leaching was, however, more efficient since ft was possible to carry it out at higher chloride ion concentrations. About 10% of the lead was leached in this way in 90 days. Finally, the ore was leached by thiourea in the presence of a gold-oxidant (oxone) to extract the gold and silver. Over 60% of the gold and over 55% of the silver were extracted from the ore in 150 days, while. the extractions of these precious metals from an untreated ore sample were lower than 25%.

Jan 1, 1991

By Susumu Okabe

Top blow injection has been applied to continuous copper smelting and converting by Mitsubishi Materials Corporation since 1974. In this process, injected feeds are captured by and dispersed in the molten bath immediately and effectively, and the reaction is enhanced by the agitation of the bath. The continuous motion of the molten bath, however, may cause severe damage of furnace lining materials, if the injection is not controlled and the furnace is not designed properly. In order to suppress refractory wear, especially at the bath line, surface wave of the molten bath should be moderated. A cold model study was carried out with water bath in a cylindrical vessel and the physical model was derived which correlates the oscillation of gas jet impingement on the bath surface and the surface wave. It was found that a half of the proper frequency of the gas jet impingement coincides the proper frequency of the surface wave.

Jan 1, 1998

By Ken-ichiro Uemura

"The DIOS process has been developed for eight years since 1988. The research project was started with the element studies carried out by each of the five integrated steel making companies in Japan, the final two and half years were spent for the pilot plant studies. Operation were conducted in the entirely closed and pressurized system successfully as planned. From the result, the DIOS process was proved to be viable as a future iron-making process substitutable for the conventional blast furnace. In addition, a lot of findings were obtained. Hot metal productivity was primarily determined by a oxygen flow rate, and a coal consumption varied depending on the productivity. The post combustion ratio was a little lower than expected from the result of the element study. It was supposed to relate the gas-reforming with coal or volatile matter in the free space of the furnace. Hot metal carbon content seemed to depend on the char content in slag.INTRODUCTIONThe JISF's DIOS pilot plant (DIOS=Direct Iron Ore Smelting Reduction Process) has finished its last campaign of the operations in January 1996. The project was started in 1988 as a joint research of the Center for Coal Utilization, Japan and the Japan Iron and Steel Federation (JISF) with a subsidy for promoting coal productions and utilization technologies from the Agency of National Resources and Energy, the Ministry of International Trade and Industry(MITI). Throughout the pilot plant test, a total of over 20,000 tons of hot metal was produced for more than 2,000 hours of the operation. Recorded production rate was 538 ton/day for 3 days at a specific coal consumption of approx. 1,000kg/hmt. Long-term operation was carried out in the fifth campaign for 18 days, which has proved that the entirely closed and pressurized DIOS process works well as planned. In Figure 1 is shown the representative operational performance obtained in the first five campaigns. The project is going to be finished by the end of March this year after investigating the technical viability and economic potential of the process, and completing the conceptual design of the DIOS commercial plant. In this paper, the system and facilities of the DIOS process are first introduced and some of the results of the pilot plant test are detailed later."

Jan 1, 1996

By M. K. Patel, K. A. Pericleous, M. Molaei

"The future trading of carbon credits and increased financial cost necessitates substantial cuts in incidental C02 emissions in the production of metals (iron, steel, aluminum, zinc, lead). Although greener methods of production are being developed, in the short term the use of point-source C02 extraction using existing technology remains attractive. Accelerated natural carbonation, in a fluidized bed is a feasible technological route investigated in this research. CFD modelling has been used to study the efficiency of C02 capture in a fluidized bed reactor containing a CaO solid sorbent. A Lagrangian/Eulerian scheme describes describe CaO particle trajectories and exchange of mass, momentum and energy with the carrier gas, with a typical off-gas composition. Different reactor geometries are considered (with uniform, stepped and gradually expanding cross-section), to maximize conversion for a given particle loading and size distribution (100-200 microns). Removal efficiencies of up to 80% are demonstrated, making this a viable process.IntroductionBased on Intergovernmental Panel on Climate Change (IPCC) reports, the major cause of climate change and global warming is due to a high level of C02 concentration in the atmosphere resulting from fossil fuel combustion, particularly in coal-fired power plants [1]. Carbon capture and storage is therefore the most important action proposed to reduce C02 from combustion flue gases. In this process, carbon dioxide is captured and may then be regenerated as pure C02 and conducted to a permanent storage, or simply stored as a solid carbonate [2]. Capture and storage of C02 has an economic penalty and the main cost of this penalty is associated with the capture plant. Capturing C02 with a lime-based solid sorbent (CaO) is a very promising technique, due to the low cost and the wide availability of the reactant. In this process, the CaO reacts with C02 based on the following reaction in a reactor called a Carbonator:"

Jan 1, 2012

By C. F. Ferron

A process has been developed to treat the copper gold ores from the Guelb Moghrein mine in Mauritania. The process consists of pressure leaching the sulphide concentrate, neutralising with the oxide ore, recovery of copper by SX/EW and of gold by cyanidation of the autoclave residue. This paper focuses on the pressure leaching step, and presents data from bench and pilot plant test programs. In particular, attention is drawn to the effects of temperature, grind size, neutralisation, retention time and solution recycle on the kinetics of copper dissolution from various flotation concentrates. Likely leach mechanisms are briefly discussed.

Jan 1, 2000

By Shi Yuan

Molten copper was deoxidized using a one-end-closed yttria-stabilized zirconia (YSZ) tube. A thin layer of porous Ni-Zr02 cermet electrode was deposited on the inner wall of the YSZ tube. The outer surface of the tube was in contact with the melt and the inner surface with a flowing reducing gas. Without applying external EMF, the melt was deoxidized by short-circuiting the melt with the cermet electrode. The deoxidation process was analyzed and the rate controlling steps were identified. These experiments were also conducted at different temperatures to evaluate the effect of temperature on the deoxidation kinetics.

Jan 1, 1994