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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 Joni M. Barnes

A strain of Pseudomonas stutzeri isohted from selenium contaminated surface waters, was found to be effective . in reducing selenate (Se04 2) stoichiometrically to selenite (Se03 2 '), which was further reduced to elementaJ selenium (Se0 ). These reactions were concurrent with the microbial oxidation of lactate. In order to assess quantitatively the amounts of seilenate and selenitein solution, improvements to existing analytical methods (ion exchange chromatography and inductively coupled plasma atomic emission spectrophotometry technique) .were made.

Jan 1, 1991

By C. Burton Clark

The important role of the petrographic microscope in the petrology of refractories is discussed, based on 45 years of industrial experience by the author. Highlights of his career are used to illustrate improvements in equipment and techniques during the period. Two specific investigations are described which emphasize the interrelated use of the petrographic microscope with other instruments such as the x-ray diffractometer and scanning electron microscope. Emphasis is placed on the use of phase equilibrium diagrams for guidance in predicting and interpreting reactions that occur under non-equilibrium conditions in the manufacture and use of refractories.

Jan 1, 1982

By A. J. van der Zeeuw

The use of SME 529 in the extraction of copper from acidic liquors and of copper and nickel from ammoniacal solutions, is illustrated with results of laboratory and bench scale mixer/settler experiments. Special features of SME 529 are its high loading capacity and the ability to keep the complexes dissolved in the organic phase up to quite high concentrations.

Jan 1, 1976

By R. E. Moore

The lining systems currently in use in BOF furnaces, certain steel ladles, and the slag line of electric are furnaces were developed during the late seventies through the mid-eighties using a trial and error method of combining aggregate, carbon sources, additives and binders. They are currently based on magnesia, graphite, metal additives and resin binders, the selections of each being tied to the anticipated intensity of the use conditions. The general functions of the respective constituents are well appreciated, however, there is still a great deal that is not known about how the socalled antioxidants protect the graphite nor how impurities from the graphite and the aggregate enter into the wear processes. In a simplified assessment of wear processes, it appears that if the deoxidized layer can be kept very thin, less than 810 mm in depth, and if the viscosity and quantity of the matrix glassy phases can be controlled to resist erosion of the deoxidized layer, lining life can be maximized for the various applications. This paper will discuss the characteristics of the starting materials systems currently being employed for applications requiring a deoxidation function to realize extended wear. It will not attempt to explain all the complex interrelationships between the respective constituents but will point to the potential for improvements through the use of improved constituents.

Jan 1, 1991

By Bora Derin

This work deals with the recovery of valuable metals from the ancient copper smelting slags located in Küre-Turkey. In this process, copper and cobalt were recovered in metallic form and/or as their compounds, whereas iron was recovered as magnetic oxide or pigment. Abrasive grit material was produced using reduced final slag. The process stages involved carbothermal reduction in a DC arc furnace, granulation, leaching, chemical precipitation, selective sulfidizing roasting and product preparations. In this paper, the process stages were described as theoretically and experimentally whereas slag and products were characterized in detail.

Jan 1, 2003

By Sue Xue, Carl C. Nesbitt

A project was completed which investigated the efficacy of recycling lead or lead monoxide from various fire assay wastes including crucibles, cupels and slag. The scope of the project was to determine optimal hydrometallurgical parameters so that direct separation and recovery of lead salts was economically feasible. A process was developed from the study which could use either acetic acid or nitric acid as a leachant, followed by several precipitation processes which could directly recover litharge (PbO) or other lead salts, such as lead carbonate or lead sulfate. The economics of the process is discussed. Analytical equipment such as the atomic absorption spectrophotometer and x-ray diffractometer supplied much of the information required for the study. However some novel analytical approaches using these instruments had to be developed to help in the determination of leaching kinetics and process quality control which are discussed.

Jan 1, 1999

By James C. Foley

In-situ characterizations of green state part density and sintering state have long been desired in the powder metal community. Recent advances in non-contact electromagnetic acoustic transducer (EMAT) technology have enabled in-situ monitoring of acoustic amplitude and velocity as sintering proceeds. Samples were made from elemental powders of Al (99.99%), Al (99.7%), Ag, (99.99%), Cu (99.99%) and Fe (99.9%). The powders were pressed in a uniaxial die and examined with acoustic waves for changes in velocity and amplitude during sintering. The changes in acoustic properties were correlated with mechanical properties. Evolution of a series of reverberating echoes during sintering is shown to provide information on the state of sintering, changes in sintering kinetics as well as having the potential for detection of interior flaws.

Jan 1, 2001

By Susumu Okabe, Etsuji Kimura

"The Mitsubishi Continuous Copper Smelting and Converting Process is the typical applications of injection metallurgy to nonferrous metallurgical operation, where the top blowing multiple lance system is employed for the continuous feeding of the raw materials and reaction gases into the molten bath. This results in an effective dispersion of the reactants into a strongly agitated bath. These are considered as the major advantage of the process with respect to the high production efficiency. On the other hand, however, the strong agitation may cause a considerable amount of refractory wear, and the melt splash generated by the lancing may also have negative effects on the productivity, i.e. the increase in the refractory wear, the metal loss, the heat loss, and the accretion growth, etc. Therefore, the optimization of the blowing condition as wen as furnace design is very important to achieve a stable and efficient operation, and fundamental understanding of the injection, agitation, and splashing is badly needed.In this paper, fundamental aspects of the Mitsubishi Process regarding injection, especially splashing phenomena, are discussed. The splashing on a vertical plane caused by the top blowing gas injection onto liquid surface was investigated through physical model study. As a result of the study, the splashing rate on the furnace wan was wen correlated with the physical properties of the bath materials, gas velocity, cavity shape, lance/wall distance and ceiling position. Obtained equations were compiled in a computer program and have been successfully applied to the evaluation of the furnace design. IntroductionInjection metallurgy is an application of gas/solid-in-liquid dispersing operation to the metallurgical processing, and has been widely adopted in various fields in order to improve their efficiency or productivity. The dispersed small particles of gas or solid materials in the liquid phase result in increased interface area, and injected momentum causes an agitation and enhanced heat and materiel transfer. Typical examples of injection metallurgy are LD converter for steel making, PS converter, Noranda process, Isasme1t for copper making, and Mitsubishi Material's continuous copper smelting and converting process, and so on."

Jan 1, 1996

By Keiji Toyabe

Several purifying techniques have been developed for controlling the impurity levels in the copper electrolyte at Niihama Copper Refinery. These have been carried out as follows; i ) the study of the reaction in liberation made it possible to raise the current efficiency for arsenic removal by more than 50% and to decrease generation of arsine sharply. By applying this method, a good performance was attained at commercial operation. li) the antimony in the electrolyte can be successfully removed by contacting it with activated carbon. This procedure is applicable particularly when there is a large amount of antimony in the copper anode. lli) for the nickel sulphate recovery from the electrolyte, an electric evaporating system was developed. The characteristics of this process are, capability of continuous operation with less manpower, the high recovery ratio of nickel sulphate (more than 85% as nickel) and no black acid formation in the treated solution.

Jan 1, 1987

By Claudio Toro, Alex Moyano, Jonkion Font, Carlos Caballero, Pedro Morales

"Codelco-Chile in the last decade has carried out industrially-oriented research as an alternative to the traditional batch-type converting process. In a first stage carried out preliminary evaluations in a rearranged Peirce Smith (PS) converter, and then an exploratory test in a “Convertidor Teniente” (Teniente converter, TC) for the Codelco-Chile Continuous Converting Process. However, the validation test for this process in the TC was delayed up to the second quarter of 2007 where the validation studies were done satisfactorily.Thus, the objective of this paper is to present the results of the campaign tests validating the Codelco-Chile Continuous Converting Process in the TC1 of the Codelco Norte smelter.The results of charging the solid or liquid matte or high grade matte (“white metal”) by Garrgun, or by mouth of the 22 m x 5 m TC1 are presented. Some features of the industrially validated process are discussed, and the pilot test results of the matte injection are also presented."

Jan 1, 2009

By L. A. Harris

In the present study the open gradient magnetic separation' (OGMS) method has been used to beneficiate the -30 + 100 mesh fraction of two high volatile bituminous coals. The evaluation of the effectiveness of the magnetic separation for cleaning these coals is the subject of this paper. Coal petrography in combination with scanning electron microscopy (SEM) and x-ray diffractometry (XRD) were used to characterize the magnetically separated coal fractions. These analyses revealed that the majority of the pyrite and non-pyrite minerals were concentrated in the positive magnetic susceptibility fractions. The bulk of the starting samples (-80 weight percent) were located in the negative magnetic susceptibility fractions and showed significant reductions in pyrite and non-pyritic minerals. The magnetic separation appears to effectively split the samples into relatively clean coal and refuse.

Jan 1, 1981

By den Bulck A. Van

In Europe, 50% of the copper originates from recycling. High-Cu containing scraps are regularly rich in impurities like Fe, Ni, Sn and Pb. Many high-Cu containing scraps are fed directly into anode-furnace casting installations or furnaces with limited refining capability. The impurities levels of the anodes produced in these processes should however remain acceptable for further electro-refining. The distribution of Sn between copper and slag has been investigated for conditions relevant to copper converting. Unlike previous studies, this work focuses on the behavior of Sn relevant to fire refining conditions, which are essential for anode refineries.In this study, liquid Cu–1Sn and CuOx–FeOy–SiO2 slag, with CaO additions, were equilibrated at 1300 °C in vacuum sealed SiO2 ampoules. After metal–slag equilibration, the samples were quenched in water. The composition of the slag and Cu metal was investigated with Electron Probe X-ray Microanalysis. The distribution coefficients of Sn between slag and Cu metal were determined as a function of slag composition.

By H. Y. Sohn, M. Y. Mohassab-Ahmed

"As part of research to develop a novel flash ironmaking process using reduction of iron ore concentrate by natural gas or hydrogen, sulfur and phosphorus distribution ratios between MgOsaturated slag and iron were determined in the temperature range 1550-1650°C under three different gas atmospheres: H2/H2O, H2/H2O/CO/CO2, and CO/CO2. The distribution coefficients of sulfur (Ls) were 4.0, 2.0, and 0.8, respectively, under these atmospheres. The distribution coefficients of phosphorus (Lp) were, respectively, 8, 17, and 20 under these atmospheres. In the flash process over -25 wt% P and S volatilize during ore concentrate downward flight in the reactor shaft in addition to avoiding coke. Therefore, iron produced by the flash ironmaking process would have much lower sulfur contents than the typical hot metal produced by the BF.IntroductionGiven the issues related to large carbon dioxide emissions and energy consumption in the existing ironmaking technologies, a novel flash ironmaking technology was conceived by Sohn [1-3] at the University of Utah. This technology is the first ironmaking process that will convert iron ore concentrate directly to metallic iron in-flight. This process will produce iron directly from concentrate without requiring pelletization or sintering and avoid the need for coke. In addition, this process concept takes full advantage of the fine particle size of concentrate with a large surface area, which permits rapid reduction by a gas. In this novel ironmaking process, potential reductants and fuels are H2, natural gas, and coal gas. Therefore, an iron-slag bath is expected to be at equilibrium with gas atmospheres of mainly H2/H2O or CO/CO2/H2/H2O, respectively, corresponding to the use of H2 or natural gas/coal gas. Since the effects of an H2O- containing atmosphere on slag properties have not been studied before, it is critical for the development of the novel flash process to determine these effects. In H2-H2O-CO-CO2 gas mixtures under ironmaking conditions, H20 was found to have the most pronounced effect on the slag chemistry [ 4, 5]. In addition, it was found in this laboratory that water in the gas atmosphere affected the distribution of Mn between slag and molten iron [6]. Most previous work used CO/CO2 gas mixture to control oxygen partial pressure (p02) [7, 8]. Others used only inert atmospheres [9], although Kor and Richardson [10] used a mixture of C02/H2 to control p02. For phosphorus, previous research focused on Ar [11], Ar-CO mixture [12], CO [13], CO/CO2 [14] or N2/CO [15]. Therefore, it was necessary to investigate the effect of water vapor content in H2-H2O-CO-CO2 mixtures on the equilibrium distribution of sulfur and phosphorus between CaO-MgOsatSiO2-Al2O3-FeO- MnO (0.2-0.8 wt%)-P2O5 (0.1-0.9 wt%) slag and molten iron as part of the development of the novel flash ironmaking technology."

Jan 1, 2014

By Guo Chen, Xuefeng Liao, Tu Hu, Shengzhou Zhang, Hongying Xia, Jinhui Peng, Libo Zhang

Pine nut shell is as raw material for preparation of high surface area activated carbon (HSAAC) by microwave induced KOH activation. The effects of microwave power, activation duration and KOH/C mass rate (R) on the iodine adsorption capability and activated carbon yield were investigated. Additionally the surface characteristics of HSAAC were characterized by nitrogen adsorption isotherms and SEM. The operating variables were optimized utilizing the response surface methodology and were identified microwave power 738W, activation duration 17 min, and R 4, corresponding to a yield of 46.28 % and an iodine number of 2154 mg/g. The key pore structure parameters of HSAAC such as the Brunauer–Emmett–Teller (BET) surface area and total pore volume were estimated to be 3819 m2/g and 2.09 mL/g, respectively. The findings strongly support the feasibility of microwave heating for preparation of HSAAC from spent pine nut shell by microwave induced KOH activation.

Jan 1, 2016

By K. Fagerlund

Methods for simulation of settler reactions, matte-slag separation and matte settling in copper flash smelting have been examined. The reaction, separation and settling phenomena of slightly oxidized chalcopyrite samples and cuprous sulfide-magnetite mixtures in fayalite type slags were examined at about 1300°C under inert atmosphere. Two methods based on introduction of molten samples of oxidized chalcopyrite concentrates or synthetic matte-magnetite mixtures onto the surface of molten iron silicate slag were tested. In the first method the samples were water quenched and polished specimens were studied and analysed using light optical microscope, scanning electron microscope, energy dispersive spectrometer. In the second method processes taking place after the introduction of samples onto the slag are followed "in situ" using X-ray transmission image monitoring. Great differences were observed in separation and settling behaviour of low and high grade copper mattes produced as a results of interaction of initial samples and slag.

Jan 1, 1997

By M. A. Gimenes

The utilization of chlorination in extractive metallurgy and advanced ceramics areas has been widely investigated as a preparative route in order to obtain intermetallic compounds, which are used as precursors in the development of new materials and process. The major processes of decomposition of rare-earth ores use sulfuric acid and sodium hydroxide at high temperatures, however there is not much work concerning chlorination. In this work, a systematic study of the reaction between xenotime (REPO4), chlorine and carbon has been performed. Particular emphasis was on kinetic studies to establish optimized conditions for the reaction. The kinetics of chlorination of xenotime raw material by rare-earth elements/compounds has been studied over a temperature range from 600°C to 950°C. The influence on the rate of conversion of xenotime to RECl3 on temperature, partial pressure of chlorine, carbon content, and particle size were investigated. A global rate equation that includes these parameters has been developed. The results show that the process follows the unreacted core-shrinking model with a formation of a porous product layer. The powder X ray-diffraction technique corroborated this model showing clearly the patterns related to the formation of yttrium oxychloride (YOCl), indicating that the reaction mechanism involves the presence ofan intermediate step before the formation of lanthanide chloride.

Jan 1, 2000

By M. Wenzel, Dang Thanh Tung, Nguyen Anh Duc, Nguyen Huu Luong, Dang Van Sy, N. Kelly, K. Gloe, K. Kretschmer, Phuc Nguyen Le, K. Schnaars, S. Robles M, L. Götzke, J. J. Weigand

The recovery of rare earth metals from secondary sources has attracted much attention due to their ever expanding demand in the high-tech industry. The studies reported here focus on the hydrometallurgical recovery of lanthanum and cerium from spent fluid catalytic cracking (FCC) catalysts in a two-step process: leaching with nitric acid and solvent extraction by tri-n-butyl phosphate (TBP) and di(2-ethylhexyl)phosphoric acid (D2EHPA). The experiments show a high dissolution yield of about 93% lanthanum and 42% cerium in a single leaching step with 2 M (126 g/L) HNO3 at 80 °C; only 11% aluminum has been dissolved simultaneously. In the subsequent solvent extraction step the best results for this leach liquor could be achieved using a 1:1 mixture of 25% (v/v) TBP (0.92 M) and 25% (v/v) D2EHPA (0.76 M) in n-decane without the need for any pH adjustment. In that case La(III) and Ce(III) can be extracted with 60% and 74% yield respectively in one stage from the majority of accompanying matrix elements. In particular no extraction of Al(III) could be observed under these conditions.

Jan 1, 2016

By Chuandong Wei, Mao Chen, Baojun Zhao, Zhixiang Cui

The first bottom blown copper smelting furnace (BBF) has been successfully operated for 10 years at Dongying Fangyuan Nonferrous Metals. In addition to many advantages of the BBF reported previously, stable operation with spinel-containing slags enabled the BBF refractories to achieve three-year campaign life. Understanding of the degradation mechanisms of the magnesia-chromite refractory will be able to further prolong the service life of the refractories and develop new refractories. In the present study, the post-mortem refractories were collected from different locations of the BBF during the annual maintenance. It is the first systematic study for the used refractories of a BBF. The phases present in the refractories and their compositions have been determined by Electron Probe X-Ray Microanalysis. The degradation mechanisms of the refractories are discussed based on the analyses. The results will be used to optimize the operation and select proper refractories in the furnaces.

Mar 1, 2018

By D. J. Murdock

Cominco Ltd. has developed a number of innovative technologies for electrowinning. The paper discusses the application of these technologies to the copper industry. Tankhouse and cell design will be discussed in addition to anode cleaning and cathode handling. Specific examples of the application of this technology to the copper industry are cited.

Jan 1, 1987