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By F. Ajersch, P: Tsantrizos, K: Shanker

"TiN films have been deposited on various substrates by a novel reactive plasma technology. In this process, a nitrogen source (NH3 or N2) and TiCl4 are reacted in the jet of a plasma torch, and are deposited onto a substrate forming TiN films at a high growth rate ( > 2µm/min). It was found that the process parameters strongly affect the microstructure, thickness, density, and growth rate of the TiN films. These parameters include source of nitrogen (NH3 or N2, N/Ti ratio, temperature of substrate, and spray distance. In general, it was found that thick and dense coatings were deposited when the N:Ti ratio was kept low, and the substrate temperature was high. Also, for the series of conditions investigated, NH3 was found to give much better results than N2•. The limitations and advantages of this technique are also discussed in this paper.IntroductionTiN is an extremely hard material and is used in many wear applications, particularly as a protective coating on cutting tools to extend their Iife(1.2). Owing to its excellent chemical stability, TiN is also frequently used as a diffusion barrier in the electronics industry for sub-micron Al/TiN/Si ohmic contact systems (3) or as a coating on high-temperature resistant alloys in gas turbine applications (4), based on its good resistance to oxidation. Other applications include decorative coatings in the jewelry industry, and specialized applications such as solar energy absorbers and transparent heat mirrors(5).TiN films can be deposited/formed using various techniques. The main techniques of deposition are CVD (Chemical Vapour Deposition) and PVD (Physical Vapour Deposition). Each of these techniques can have many variations in equipment characteristics, reactants as well as a range of process parameters (pressure and temperature). In the CVD process, TiN is generally deposited onto a heated substrate where a chemical reaction takes place. The reaction can be one of reduction(6) (e.g.: TiCI4 + 0.5N2 + 2H2 --> TiN + 4HCI), of thermal decomposition(7) (e.g. decomposition of titanium dialkylamide), or of displacement (e.g. TiCI4 + NH3 --> TiN + 3HCI + 0.5CI2)' The displacement and reduction reactions are the most common."

Jan 1, 1994

By Jianxun Song, Hongmin Zhu, Qiuyu Wang, Jungang Hou, Shuqiang Jiao, Xiaobo Zhu

This work presents the results of a study on the Ti3+/Ti2+ couple redox potentials vs. Cl–/Cl2 at the temperature range (673 to 1073 K) in fused LiCl-KCl eutectic by direct potentiometric method. Initial concentrations of TiClx in solvents did not exceed 5.0 mol%. Basic thermodynamic properties of the reactions TiCl2+1/2Cl2(g)=TiCl3 were calculated using the temperature dependencies of apparent standard potentials of the couples E* Ti3+ /Ti2+.

Jan 1, 2014

By Jeong-Soo Sohn

Physical treatment and chemical treatment of spent lithium-ion battery were studied in our research team. Especially we developed two types of acidic leaching for crushed powders containing LiCoO2 of spent lithium ion battery. One of them is sulfuric acid leaching with H2O2 as a reducing agent. The leaching rates of cobalt, lithium and the other metals were above 99 % at the condition of 2 M H2SO4, 10 vol. % H2O2, 75 °C, 300 rpm agitation speed, 250 g/5L solid liquid ratio and 75 minutes reaction time. And the other leaching process is the oxalic acid leaching. In this process more than 99% of Li and less than 1% of Co were dissolved at the condition of 3M oxalic acid, 80°C reaction temperature, 300rpm agitation speed, 50g/L initial solid/liquid ratio and 90min extraction time. Each process has its advantage and disadvantage. In sulfuric acid leaching, leaching reagent is very cheap and cobalt could be recovered into cobalt hydroxide. On the other hand, oxalic acid is more expensive than sulfuric acid but lithium could be dissolved selectively. Also cobalt could be recovered into cobalt oxalate and it could be changed into cobalt oxide after heat treatment. In order to select the effective recycling process, recovery rate and purity of cobalt hydroxide and cobalt oxalate were compared and it was investigated which process was more environment-friendly and economical.

Jan 1, 2006

By Chen Ya

Layered LiMn0.5Ni0.3Co0.2O2 was prepared from Mn(NO3)2, Ni(NO3)2, Co(NO3)2 and LiOH by co-precipitation and solid state reaction. XRD, C-V and galvanostatic charge-discharge methods were used to examine the structural and electrochemical characteristics. The LiMn0.5Ni0.3Co0.2O2 delivered a high discharge capacity of 167 mAh/g between 2.5 and 4.3 V with excellent cycling stability.

Jan 1, 2006

By Alwin Frei, Aldo Steinfeld, Peter G. Loutzenhiser, Enrico Guglielmini

"Using concentrated solar radiation as the energy source of high-temperature process heat, the carbothermal reductions of Al2O3 to Al and SiO2 to Si were examined thermodynamically and demonstrated experimentally at vacuum pressures. Reducing the system pressure favors Al(g) and Si(g) formation, enabling their vacuum distillation and avoiding contamination by carbides and/or oxycarbides. Exploratory experimentation in a solar reactor was performed with mixtures of charcoal with alumina and silica in the ranges of 1300-2000 K and 1997–2263 K, respectively, at 10-3 bar by direct exposure to concentrated thermal radiation. Distilled samples contained up to 19 wt% of Al in Al-Al2O3 mixtures and 79 wt% of Si in Si-SiO2 mixtures. When the reducing agent is derived from a biomass source, the solar-driven carbothermal processes are CO2 neutral.IntroductionMetallurgical extractive processes for producing Al1-2 from Al2O3 and Si3-6 from SiO2 are characterized by their high specific energy consumption and concomitant emissions. Alternatively, concentrated solar energy can be used as a high-temperature heat source to drive the carbothermal reductions and, thus, avoid greenhouse gas emissions and other pollutants derived from fossil-fuel-based processes7-12. When the reducing agent is biomass charcoal, the solar-driven carbothermal reduction is CO2 neutral. The carbothermal reductions of Al2O3 and SiO2 are represented by the simplified overall stoichiometric reactions:"

Jan 1, 2011

By C. Lupi

The electrorefining of primary copper is a well known technology: in this work copper scrap was directly processed in the same way. he copper and copper alloy scrap was previously pressed by means of a 20 tons apparatus in order to avoid pyrometallurgical operations. The samples obtained in this manner showed a good compactness so that they were used as anodes in the electrorefining tests. The tests were carried out on anodes made by copper scrap, copper alloy scrap and a mixture of the two. The electrorefining tests were performed at both 303 and 333 K, in a perspex cell having a volume of 500 ml using a current density of 250 A/m2. The cathode used was always a sheet of pure copper and the electrolyte composition was 40-50 g/l Cu as CuS04 and 150-200 g/l H2SO4. Current efficiency in the range of 92-97% and specific energy consumption ranging from 0.14- 0.20 kWg of copper were reached in all the tests. The refined copper deposits were analyzed by AAS to verify their purity and observed by SEM to highlight their morphology.

Jan 1, 1998

By Ali Akbar Mottahedi

Chromate conversion coating is a process for making a complex layer at the surface of zinc galvanized steel which makes the metal more resistant to corrosion, especially at marine atmosphere, and increases the adhesiveness of color. In this work the influences of various compositions on commercial zinc galvanized steel sheet to the color of chromate conversion coating has been investigated at normal temperature and the factors that affect the control and optimization of the process have been determined. A bath composition of 20 g/liter Cr203 and 10 g/liter NaOH and a dipping time of 50 seconds at room temperature (25-30°C) make a desirable color of chromate coating. A slow agitation at a constant pH of I (with additions of NaOH or H2SO4) assures a constant bath condition and develops the color. This kind of coating has more corrosion resistance and this bath condition and composition are also more economical.

Jan 1, 2003

By Xia Hong-ying, Peng Jin-hui, Zheng Zhao-qiang, Zhang Li-bo

"Preparation of activated carbon from the walnut shell by microwave assisted steam activation was studied. Influences of the three parameters, activation temperature, activation duration and steam flow rate on the adsorption capacity and yield of walnut shell activated carbon(WSAC) were investigated,optimization process was obtained by the Response Surface Methodology (RSM). The optimum preparation conditions were as follows: activation temperature of 980°C, activation duration of 41 min and steam flow rate of 1.66 ml/min. The optimum conditions resulted in an activation carbon with an iodine number of 1025 mg/g and a yield of 52.17%, while the BET surface area, total pore volume and average pore diameter of WSAC were 1328m2/g, 0.72ml/g and 2.2nm respectively. The study supported the potentiality of comprehensive utilization ofWalnut shell and the benefits of the microwave heating.IntroductionActivated carbons are one of the most important adsorbent materials in modern society because of its abundantly developed pore structure, strong adsorption ability, high surface area and thermo stability. They have extensive application in many industries fields which include gas purification [1], catalyst supports [2] and other pollutants [3]. However, in recent years, the industrial production of activated carbon is facing the problem of raw material scarcity and high cost, which limit to be widely used. Therefore, the selection of an appropriate precursor plays an important role and it has become hot sport to seek cheap raw material to lower preparation cost. As a kind of reproducible resource, the waste from agriculture and forestry is a high-grade raw material for preparing activated carbon due to is high carbon content, such as palm shell [4], rice hull [5], and coconut shell [6]. At present Walnut shell is widely accepted to be a renewable source of biomass. According to statistics, there is more than 1000,000 tonnes of walnut shells are produced in China annually [7]. As a good precursor for activated carbon production, Walnut shell is a major agricultural waste, to make better use of the cheap and abundant agricultural waste, it is proposed for activated carbon production."

Jan 1, 2014

By J. Leon-Torres, D. M. Stefanescu, P. A. Curreri, S. Sen

"Experiments were performed under terrestrial gravity (lg) and during parabolic flights (10·2 g) to study the solidification and macrosegregation patterns of Al-Cu alloys. Alloys having 2% and 5% Cu were solidified against a chill at two different cooling rates. Microscopic and Electron Microprobe characterization was used to produce rnicrostructural and macrosegregation maps.In all cases positive segregation occurred next to the chill because of the shrinkage flow, as expected. This positive segregation was higher in the low-g samples, apparently because of the higher heat transfer coefficient.A 2-D computational model was used to explain the experimental results. The continuum formulation was employed to describe the macroscopic transports of mass, energy, and momentum, associated with the solidification phenomena, for a two-phase system. The model considers that liquid flow is driven by thermal and solutal buoyancy, and by solidification shrinkage. The solidification event was divided into two stages. In the first one, the liquid containing freely moving equiaxed grains was described through the relative viscosity concept. In the second stage, when a fixed dendritic network was formed after dendritic coherency, the mushy zone was treated as a porous medium.The macrosegregation maps and the cooling curves obtained during experiments were used for validation of the solidification and segregation model. The model can explain the solidification and macrosegregation patterns and the differences between low- and high-gravity results."

Jan 1, 1999

By I. A. Ibrahim

Ilmenite, in its natural form, is an inactive mineral from which the selective removal of iron is rather difficult. The reactivity of ilmenite. so that it can be leached with dilute hydrochloric acid, can be enhanced by chemical reduction in solution using a suitable metal as a reducing agent. The present paper aims at the evaluation of an Egyptian ilmenite ore for the production of synthetic rutile by direct leaching with hydrochloric acid in presence of iron powder. In this process, the titanium and iron contents are dissolved; meanwhile, the dissolved titanium is hydrolyzed and re-precipitated leaving mainly iron in solution. Leaching conditions were optimized to obtain less iron in the final solid product. Addition of sufficient amount of iron powder during leaching reduces the dissolved Fe3+ to Fe2+ and reduces the dissolved Ti4+ to Ti3+. The creation of Ti3+ in solution is assumed to have a role in dissolving the ferric iron and hence increasing the reactivity of the ilmenite ore. Synthetic rutile of about 90% TiO2 and 0.77% Fe2O3 was obtained from ore with a grain size 100% passing 200 mesh and a 5-hour leach time with 20% HCl at boiling temperature (110°C) and 0.11 g iron powder / g ore.

Jan 1, 2003

By Gi-Chun Han

This study focused on stabilization of heavy metals and removal of chlorine in MSWI bottom ash by artificial carbonation with washing. Artificial carbonation was carried out by applying CO2(g) injection in washing for fractions above and below 4mesh for reuse as construction materials like aggregate, As a result, carbonation with washing could satisfy Korean environmental regulation and remove chlorine in bottom ash more effectively by resolving residual friedel?s salt(3CaOAl2O3CaCl210H2O).

Jan 1, 2006

By C. M. Dentan

Conventional testing of crude kaolin ores emphasizes physical properties as they relate to end uses of kaolin products. This approach to evaluating crude ores does not reveal the basis of behavioral differences between typical coarse and fine kaolins from central Georgia. Optical and scanning electron microscopy in combination with XEDS have been employed to characterize both coarse Cretaceous and fine Tertiary kaolin in order to shed light on the reasons for the gross differences in their properties. Routine evaluation of various parameters was also carried out. Bulk densities were 1.48 g cc-l for the coarse clays and 1.53 g cc-1 for the fine clays. Surface areas were 15 m2 9-1 and 25 m2 9-1, respectively. Brookfield viscosities were low for the coarse clays at 70% solids, and high for the fine clays. The situation was reversed for Hercules viscosities. Sixty percent of the coarse clays had particles of less than 2 um and the fine clays had 90% less than 2 cm. Micrographs of thin sections prepared from blue-dyed epoxy-impregnated crude ores and of SEM fabric samples demonstrated vivid differences in texture. Cretaceous kaolins appeared to be completely recrystallized residual products of former aluminous sediments, while Tertiary kaolins retained their essentially sedimentary character. Differentiation of the coarse and fine kaolins is rapidly accomplished by both optical and scanning electron microscopy, and should be considered a valuable analytical technique in evaluating kaolin ores.

Jan 1, 1981

By P. Maraboutis

Iron removal by precipitation as jarosite from Fe-Ni-Co sulfate solutions, (synthetic or real, resulting from laterites leaching) has been investigated. Precipitation was carried out at 95 C, and at an initial pH 1.6, which was either kept constant with CaCO3 or Li2CO3 additions, or left to drift with the evolution of the reaction to lower values. The precipitation of K-, NH4- and Na- jarosite was initially examined using synthetic solutions. In all cases, hydronium ions were incorporated into the precipitate as well. Residual iron in solution was lower (0.2-1 g/1) and equilibrium was achieved faster (within 4-8 h) when precipitating K¬jarosite at constant pH, using CaCO3 for neutralization. Nickel and cobalt losses were small. Na- jarosite precipitation was also studied from real solutions with high initial iron content, under constant pH=1.5, controlled with CaCO3 additions, and it was shown that low residual iron concentration in solution (0.3-0.5 g/1) can be achieved again, with relatively small nickel and cobalt losses. The thickening and filtration characteristics of the precipitates were excellent in all cases examined.

Jan 1, 1988

By J. D. Sunderkötter, M. F. Stroosnijder, V. A. C. Haanappel

"TiAI-based intermetallic compounds have attracted considerable interest as structural materials for high-temperature applications due to their low density and substantial mechanical strength at high temperatures. However, one major drawback hindering industrial application arises from the insufficient oxidation resistance at temperatures beyond 700 °C. In the present contribution some general aspects of high temperature oxidation of TiAI-based intermetallics will be presented. This will be followed by a discussion of the influence of alloying elements, in particular niobium, and of the effect of nitrogen in the oxidizing environment on the high temperature oxidation behaviour of such materials.Extended AbstractIntroductionTiAI-based intermetallics are being considered as construction materials for high temperature components, e.g. in aircraft and car engines, due to their low density and substantial mechanical strength at high temperatures, see e.g. [1,2]. The best ductility can be attained with alloys consisting of y-TiAI with around 5-15 vol.% Q2-Ti3AI. However, one major hindrance to industrial application arises from the insufficient oxidation resistance at temperatures beyond 700 aG. In spite of their high aluminium content, TiAI-based intermetallics do not generally form long-lasting protective alumina scales. After longer exposure times the scales, which are initially rich in alumina, deteriorate and scales consisting of mixed alumina and titania predominate, with high growth rates similar to pure titania.It is not the intention of the present paper to present a general overview of the high temperature oxidation behaviour of TiAI based intermetallics, for which the reader is referred to the literature [3,4]. In the present contribution some general aspects of high temperature oxidation of TiAI-based intermetallics will be presented. This will be followed by a discussion of the influence of alloying elements, in particular niobium. The effect of nitrogen in the oxidizing environment on the high temperature oxidation behaviour of these intermetallics will also be considered."

Jan 1, 1996

By Hong-ying Xia, Bao-bao Wang, Jin-hui Peng, Bing-guo Liu, Li-bo Zhang, Zhi-qiang Li

Based on optimization using response surface methodology designed by Box- Behnken, to study the interaction of wet industrial salt with moisture drying temperature (50-90 ); duration (10-50s); and the weight of the materials (20-60g). The results show that: the experimental parameter conforms to the quadratic equation model to influence the moisture content and the dehydration speed., in analyzing the significance and the interaction of various factors, the optimum by the Design Expert software conditions for drying with microwave radiation include temperature of 90 , duration of 10s, and sample mass of 26g. Verified by experiment, the moisture content after drying is less than 0.25% and the dehydration rate reached 1.37g/min, between the predicted value and the actual value confirmed good fitting degree.

Jan 1, 2015

By Kurt A. M. Westerlund

The basic function of primary gas handling downstream non-ferrous pyro-metallurgical processes is cooling hot sticky gases to treatable temperature levels (e.g. entering ESP). That means managing efficient the critical gaseous components from a molten via a sticky to a solid phase. The article outlines the modem gas cooling methods combined with efficient heat recovery. Examples of the alternative use of recovered steam energy are outlined; as e.g. drying of concentrate and power generation. The heat transfer impact of the insulating dust is called fouling and circumstances causing fouling are described. Modem cooling surface design and cleaning techniques to keep fouling in reasonable limits are described. Leakage- and false air ingress into the gas handling lines often limits smelting capacity. The objective is generally to minimize the infiltration of air but it still takes place at open interfaces (e.g. at reactor hood, feed port). Leakage air at furnace roofs for example can be reduced to a minimum by adopting the pressure gas sealing used at present In-Bath-Lance furnaces. Modernization and optimization methods to de-bottleneck existing waste heat boiler gas cooling capacity by highly efficient surface cleaning systems and false air avoiding (e.g. bundle roof boxes, dust discharge) are detailed described.

Jan 1, 1999

By Christophe Thiébaut

Keywords: Pyrochemistry, Salts Treatment, Distillation The pyrochemical purification of metal generates spent salts. When this metal is an actinide such as plutonium, the slags cannot be discarded and are thus disposed in nuclear facility. In order to handle with these slags, the decision has been taken to reduce stored quantities. The development of a pyrochemical treatment is in progress in the CEA Valduc centre. The feed salt, typically composed of various Pu and Am species contained into monovalent or divalent chloride matrix, is first oxidized to convert the actinides into oxides. Then the chlorides are separated from the actinide oxides by vacuum distillation. Temperatures higher than 750°C for monochloride salts mixture NaCl/KCl and higher than 1100°C for divalent CaCl2 base salts, are required to produce an industrial flow of vaporization. Inactive qualification of the process for NaCl/KCl base salt has been carried out with lanthanide surrogates. Then, a pilot equipment, called distillator has been designed and built for production-scale distillation of NaCl/KCl and CaCl2 oxidized plutonium salts. Industrial flows of vaporization have been obtained with this pilot equipment : about 4 g/cm²/h for NaCl/KCl at 800?900°C and 1 Pa, and more than 1,5 g/cm²/h for CaCl2 base salts between 1000?1200°C at 0.1 Pa. The last step, now in progress, is the integration of the distillator into a glove box.

Jan 1, 2005

By Debbie Marshall

Nickel and cobalt in lateritic ores can be extracted by either a hydrometallurgical or a pyrometallurgical route. The high-iron limonitic fraction of a deposit is best processed' hydrometallurgically while the magnesium-rich transitional and saprolitic fractions are more suited for pyrometallurgical processing. During hydrometallurgical processing, it may be attractive, for economic reasons, to blend the limonitic component with transitional and saprolitic ores, which contain higher nickel levels. However, blending increases the concentration of magnesium in the feed, leading to increased acid demands. The decision on how much ore to process then becomes an economic one. Ore samples with different magnesium contents were prepared for the leach test program by blending limonitic and transitional ores. The ore samples were slurried in seawater and tested in the Falconbridge Hydrometallurgical Pilot Plant. As expected, acid consumption increased with increasing magnesium content of the ore. For target extractions of 95% nickel and 92% cobalt, the required residual free acid concentration increased from 30 g/L at 1.7% magnesium to 50 g/L at 2.7% magnesium. When the magnesium content was raised to 3.8% and 4.6% in subsequent pilot plant testing, the final free acid requirements did not increase beyond what was observed at 2.7% magnesium. Thus, the cut-off ore composition to maximize nickel units and minimize acid requirements is between 1.7- 2.7% magnesium. Keywords: high pressure acid leaching, laterites, magnesium

Jan 1, 2004

By W. G. Davenport

Chapter 10 showed that any given smelting task, e.g. production of 65% Cu matte, 1500 K, from CuFeS2, can be done with many different combinations of: blast%02 hydrocarbon fuel blast temperature. This chapter repeats the Chapter 10 calculations but reports the results in terms of the mass industrial oxygen mass hydrocarbon fuel blast preheat energy combinations that will produce 65% Cu matte, 1500 K, from CuFeS2 concentrate. It also determines the energy inputs equivalent to these combinations.

Jan 1, 2001

By Marko Suput

Titanium is a high-strength, low-density metal nearly immune to corrosion, but limited in use by its high price. The high price is due to the cost of smelting and processing the ore. The research on titanium production using the Solid Oxide Membrane (SOM) process aims to consolidate most of the processing steps required for conventional titanium production into a single step making it an energy-efficient and cost-effective method for producing CP billet and ingot and possibly also powders used to make titanium alloys. In the SOM process experiment, a steel crucible contains MgF2-CaF2-TiO2 flux; an inert metal/carbon rod serves as the cathode; an oxygen-ion-conducting yttrium-stabilized-zirconia (YSZ) membrane in the form of a one-end-closed tube contains either a liquid metal that acts as the anode or liquid MgF2-CaF2 ionic flux that connects the YSZ membrane to an anode. During electrolysis, when the voltage between anode and cathode is higher than the reduction potential of titanium oxide, titanium ions are reduced at the cathode and the oxygen ions pass through the YSZ membrane and are oxidized at the anode. The oxygen ions are oxidized at the anode by a reducing agent, hydrogen gas or carbon, forming steam or CO(g), respectively. To date, a suitable MgF2-CaF2-TiO2 flux has been selected and the operating temperature for the SOM process has been determined. Several electrolysis experiments have been performed. As expected, lower valence deposits of titanium oxides have been witnessed at the cathode prior to depositing pure titanium. Continuing work will aim to extend the electrolysis time in order to pass enough charge to produce a significant amount (100 g) of titanium at the cathode.

Jan 1, 2006