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By Jim Hardy, Tim McKnight

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

Jan 1, 1997

By Zhi-xiang Cui

Dongying Fangyuan Nonferrous Metals Co., Ltd. has developed a new technology to produce anode copper from concentrates through only two furnaces. This new technology is called the Two-Step Copper Smelting Process. This paper presents the commercial application of the Two-Step Copper Smelting Process and its operating conditions. The key features of the Fangyuan Two-Step Process are as follows: (1) feed materials, including concentrates and flux, are mixed without pretreatment and fed into the Submerged Lance Smelting (SLS) furnace; (2) high grade white metal (WM) produced by the SLS furnace is transferred via WM conduit into one of the two Submerged Lance Converting and Refining (SLCR) furnaces; and (3) the two SLCR furnaces blow alternatively to maintain continuous operation of the whole production chain. The new smelter started operation in October 2015 with a processing design capacity of 1.75 Mt/year of mixed feed and has been operating for over 30 months.

By Toshio Kurikami, Koichi Yamazaki

"Toho Zinc Co., Ltd Chigirishima Refinery has the production capacity of electrolytic lead for 95000t/y by sintering- blast furnace electrolytic process. Lead raw materials are lead concentrates, spent batteries and dusts that contain lead from other companies, and these are handled by existing smelting process. There are many circulation materials in the process, because the system has been constructed with improving the recovery rate and protecting the environment. This report describes material balance in each process, distribution of the lead and various components, and it examines present state of the processing. In addition, we report the result that we have tried to improve the work environment.IntroductionThe Chigirishima Refinery of the Toho Zinc Co., Ltd. is located in Chigirishima, an island 4km off the coast of Takehara-city, Hiroshima, Japan. The Chigirishima Refinery began lead smelting operations in 1951.The Chigirishima Refinery adopted the sintering-blast furnace-electrolytic process and has an electrolytic lead production capacity of 95,000 tons/year. The existing smelting process handles raw materials from lead concentrates, spent batteries, and lead-bearing dust from other companies. This system was constructed with the intentions of improving material recovery ratios and protecting the environment; therefore, there are many materials recirculating throughout the smelting process. This report describes the material balance in each process and the distribution ciflead and various components, and it examines the present state of processing. In addition, we report the results of our attempts to improve the work environment."

Jan 1, 2000

By Peter Koh

The velocity solid charge attains when dropping down concentrate chutes is an important boundary condition when developing mathematical models of flash furnace burners and reaction shafts. In this work an experimental rig was developed to measure the velocity attained when nickel concentrate and sand were dropped down a vertical pipe 3m long. The velocity measurements showed that the nickel concentrate did not fall as individual particles. The measured values of the velocity approached, but did not attain, those calculated for solid bodies, the disparity being attributed to friction at the pipe wall and fluid drag losses. After falling 2 m velocities between 5-6 m/s were attained. The analysis was extended and applied to understanding the intermittent problem of puffing which sometimes occurs from the top of the concentrate chute. The pressure at the bottom of the chute is the net result of two opposing pressures, namely that developed by (a)the process air entering through the velocity control device, and (b) the solids falling down the concentrate chute. Flow back up the chute occurs when the former exceeds the latter. The process air pressures in the burner were obtained from CFD simulations of a full burner. Variables considered included air speed through the velocity control device, drop height and furnace draft. The analysis was useful in highlighting the operating conditions which were conducive to puffing and in establishing procedures to minimise its occurrence.

Jan 1, 2006

By Ronald C. Askin

Dredging is a common method of remediating ponds containing contaminated wastes. However, dewatering of the dredged solids is usually not well integrated with the dredging phase. As a result, overall project efficiency can be poor. Specifically, since dredges deliver material in a widely varying slurry form and since dewatering presses require the delivered material to be uniform, union of the two systems often results in inconsistent operation of the overall process. In an effort to enhance overall dredging and dewatering process production rates as well as minimize the return of suspended solids in the decant water, a new process was developed to provide a consistent dredged sludge for delivery to the press. This paper discusses modifications made to a conventional dredging and dewatering process to improve production rates and dewatering capabilities. These modifications are applicable to any project where efficient solids dewatering is required and where returning decant water must be visually free of suspended solids.

Jan 1, 1996

By James E. McNulty

Today's energy era is the beginning of a transition from the Petroleum Age to a future age of renewable fuel resources. Fuels for the transition era will come from unconventional sources and conversion technology. Affecting the practicability of transition technologies are attitudes of the public, capital requirements and availability, patterns of fuels utilization, producibility of fuels and the actions of governments. Primary energy sources to replace deficiencies of oil and gas and provide growth in the period of transition will be coal, oil shale, nuclear energy and peat.

Jan 1, 1981

By Zachery Zanetell

Flotation circuit performance has become increasingly more challenging due to the complexity of available ore sources. To optimize value mineral recovery, the mineralogical composition of the ore should be evaluated and understood. Utilizing a variety of mineralogical and analytical tools, flotation processing challenges can be overcome and potential limitations understood. In this paper, several case studies will be discussed in terms of the value that has been provided through the use of mineralogical analysis to optimize flotation performance.

By Mark C. Bronson

The feasibility of several pyrochemical approaches-for separating non-radioactive constituents from ICPP HLW calcine were examined. The removal of aluminum as AICI3 from aluminia calcine was successfully demonstrated. The examination of pyrochemical processes to remove non-radioactive constituents, primarily aluminium, zirconium, calcium and fluorine, from zirconia calcine showed that fluorine removal was required in order to chlorinate the calcine. A molten calcium chloride wash, a calcium reduction, and. a sulfuric acid treatment were examined as possible zirconia calcine pretreatment options for fluorine removal. Fluorine removal from simulated ICPP zirconia calcine was demonstrated by both a CaCl2 wash method and a sulfuric acid treatment method. X-ray fluorescence analysis indicated that greater than 97% of the fluorine can be removed by either method. Fluorine removal by a calcium reduction using an alloying agent, zinc, or a calcium reduction using, a filtration separation were also demonstrated, but the efficiencies of fluorine removal were considerably less ranging from 50 to 90%. Regeneration of CaCl2 from the salt and oxide residues of the CaCl2 wash experiments was also demonstrated 'by an aqueous dissolution method. From the salt residue, 85% or more of the CaCl2 was recovered and contained little if any CaF2 or CaO. From the oxide residue close to 100% of the CaC12 was recovered. Because of the overall success of the CaCI2 wash, it was determined to be the preferred fluorine removal process. The sulfuric acid treatment to remove fluorine is effective, but the proposed overall flowsheet has not' been adequately demonstrated.

Jan 1, 1995

By Ajit Kumar Jaiswal

"Electric Arc Furnace (EAF) being a power-intensive equipment, EAF based industries are highly dependent on scarce electric energy. This is the reason Government of India is highly concerned about this and laid emphasis on the conservation of electric energy.This paper highlights factors contributing to reduction in specific electric energy consumption in EAF and suggests measures not only for power saving, but also for productivity improvement. To name a few, these are proper sealing of furnace, introduction of oxy-fuel burners, foamy slag practice, increased usage of hot metal/DRI, post-combustion of CO gas for preheating of scrap, improved selection & design criteria of electrics, power demand management, and process automation. Few cases also have been cited, where the above measures have helped in reaping significant benefits.IntroductionFor a long time, Government of India had focused on increase in energy supply, in particular, through electricity generation. Now the emphasis of Government of India has shifted from electricity generation to its conservation for following two reasons:??Power plants have become very cost-intensive??By saving energy, more of it can be delivered at lower cost to the consumersPower generating units, transmission & distribution agencies as well as consumers all have roles to play in the area of energy conservation. By energy conservation, we mean curtailing energy requirement by reducing energy wastages and taking up measures to improve energy efficiency of electric equipment/appliances. In almost all cases, this would be economically beneficial.India’s cost-effective energy conservation potential has been estimated by the Planning Commission at 23 per cent of total commercial energy generated ?1?. A national movement for energy conservation can significantly reduce the need for fresh investment in energy supply systems in coming years. It is imperative that we make all-out effort to realize this potential. Whether a household or a factory, a small shop or a large commercial building, a farmer or an office worker, every user can and must make this effort for his own benefit and for the nation’s benefit as well."

Jan 1, 2009

By K. Yarnaguchi

In the Mitsubishi Continuous Copper Converting Furnace, calcium femte slag is used. Due to its extremely high basicity, the improvement of corrosion resistance of the refractory lining is in need. In order to clarify the corrosion mechanism and to search for a new corrosion resistant material, first, the surface snuctures of bricks corroded in molten slags were observed by EPMA. Second, the dissolution behaviors of sintered MgO-based pellets containing various oxide additives were examined. It was found that the formation and the dissolution of magnesiofemte at the surface of the bricks play an important role in their corrosion and an addition of NiO, Mn02, or Ti02 to MgO is effective in stabilizing the magnesio-femte and improving the corrosion resistance of MgO.

Jan 1, 1994

By Masahiro Yoshimura, Sergiy Korablov

"Hydi-othermal corrosion ofTiN, TlAlN and CrN PVD films (3 µm thick) deposited on SUS-304 substrate was studied in 100MPa water in 20-950°C temperature range up , to 750h. The beginning temperature of their reaction was determined as 200°c for TiN and TiAlN and 500°C for CrN films, which are quite low in comparison with that of air oxidation of those powders. Very thin oxide scales. of TinO; n-I homologous series phases were formed above 300°C. TiO2 anatare. is observed for TIN and TiAlN films at 400°C. The· feature of hydrothermal corrosion of CrN films seems to be CrNxOy phase formation.Distinguishable weight changes were observed at higher temperature than 700°C for TiN, 750°C for· TiAlN and 800°C for CrN respectively. Hydrothermal corrosion kinetics .was constructed to calculate the activation energy of hydrothermal corrosions. On the base of obtained data, hydrothermal corrosion resistance was as follows: TiN – TiAlN - CrN. Facetted oxide crystals were formed at higher temperature than 500°C for TiN, TiAlN and 850°C forCrN.IntroductionThe metallic nitride (TiN; TiAlN, CrN) PVD films have high hardness, strength and wear resistance. Therefore these films are widely used in industry for wear resistij.nce application such as cutting tools and die molds. Their performances depend on not only the mechanical properties but also corrosion resistance of coated films. High temperature oxidation of metalliq nitride and nitride films was well studied [1-5]. However there are no reliable data concerning the .corrosion resistance of coated nitride materials. In high-temperature and high-pressure water. There are a few reports on hydrothermal corrosion of nitride films [6,7]. The increase of corrosion resistance of CVD films was observed in following succession TiC - TiCNO - TiCN - TiN at 300-680°C temperature interval and I 00 MPa pressure water according to data of the first report. Kawana et al. [7] have reported about excellent corrosion resistance of CrN films under 290°C and 8, 6 MPa water during I 000 h in the circulating type experimental loop. The films thickness was about 7-10 µm in both cases. However it remains unclear the chemical state of the surface species and especially in-depth distribution, oxide scale thickness and its growth, and defects formation in the oxide film."

Jan 1, 2000

By M. Kawakami

In relation to the designing of a new-type blast furnace, the reaction of carbonaceous materials with CO2 is expected to occur at as low temperature as possible. In order to get a highly reaetive carbonaceous material at low temperature, the reaction kinetics was investigated by measuring such quantities as the reaction rate from weight loss, the amount of CO adsorption and specific surface area by BET method. The reaction rates were large in the order of the Bintyo char, metallurgical coke, graphite and glassy carbon. If the rate was converted to the rate per unit area, however, those of the Bintyo char was smaller than that of graphite. Thus, it is suggested that the rate of the Bintyo char is influenced by the pore diffusion of CO2. The rate had a positive relation with the amount of CO adsorption, showing that the rate determining step would be the desorption of CO from the active side on the surface. The rate independent of surface area was derived, combining all the obtained data.

Jan 1, 2003

By B. C. Jena

In a chromite smelting process for the production of high-carbon ferrochromium, the slag composition profoundly affects operating conditions and the economic performance of the process. For a Canadian chromite concentrate, optimum slag composition and operating temperature were determined by process simulation with a computer model, which is based on parameters, such as the minimisation of slag volume, liquidus temperature, electrical energy consumption and chromium losses. Chromium recoveries are identified for slag compositions spanning wide concentration ranges within the quaternary system MgO-AI2O3- SiO2-CaO. The simulated data are compared with the experimental results.

Jan 1, 1994

By Ronald K. Riddle

The processing of lateritic ores in rotary drying and preheating/pre-reduction systems has historically been plagued by problems associated with significant dust generation. These problems include handling issues, kiln capacity limitations, negative impacts on furnace stability, a reduction in nickel recovery and higher operating costs. The dust is formed in the rotary devices during heating and tumbling due to the following three mechanisms: (I) mechanical dccrepitation of the ore as a result of tumbling and attrition, (2) thermal decrepitation during rapid vaporization of internal free and bound water, and the (3) loss of free moisture which functions as a binder. This paper investigates the causes of dust formation, provides methods to reduce dust carryover from the rotary devices, and finally offers methods to recover the dust in the existing pyrometallurgical process. Keywords: Laterite, Drying, Rotary, Dust

Jan 1, 2004

By J. Schmidl

In non-ferrous metallurgy the service life of refractory materials typically ranges from several weeks up to three years or more and is strongly dependent on operating conditions. To support our customers with the most viable refractory solution for their needs RHI Magnesita follows a structured approach of thermo-chemical calculations, experimental evaluation from lab scale up to industrial field tests and post-mortem analysis of used refractory materials. This paper will give an overview of the RHI Magnesita refractory selection process and the most recent developments of the experimental setup for the so called HF-IF test. This is a dynamic corrosion test that allows to determine fundamental properties of different refractory material types under process conditions subjected with respective customers process materials. The HF-IF experimental procedure is an excellent tool to simulate refractory wear in industrial processes, diminishing risks associated with plant trials and support decision making to choose the optimal refractory solution for the customer.

By Cheng Fang, Zhou Lie-xing, Peng Jin-hui, Guo Sheng-hui

This article discusses the behavior of temperature and microwave thermo gravimetric analysis characteristic of ammonium paratungstate in a microwave field. Experimental results show that when 12g of material is place in a microwave with 900W of power, paratungstate’s temperature rises at 70°C/min. This results in paratungstate’s temperature being 980°C after 14 minutes. Compared with thermo gravimetric analysis characteristic, former two-step process of paratungstate microwave calcined completed ahead of schedule, after two-step process reaction is more intense,Paratungstate warming is more rapidly, the reaction time is much shorter; According to XRD and SEM, the product is high purity, the crystal particle size is uniform, and the grain size is fine.

Jan 1, 2015

By Min Xiaobo

As for treatment of zinc-containing wastewater, traditional SRB (Sulfate Reducing Bacteria) process was used, however, there exist two defects, like toxicity of heavy metal ions and high effluent COD (Chemical Oxygen Demand) value. In this study, a new technique, called ISIS process (Immobilized SRB sludge beads with Inner cohesive carbon Source), in which SRB sludge is embedded in carrier of PVA (Polyvinyl Alcohol) with carbon source that adsorbed on certain material, is put forward for the first time to overcome the two defects existing in traditional SRB process. Furthermore, it has been shown that compared to traditional SRB process, ISIS process increases average zinc removal rate up 30%, average sulfate reduction rate up20%, and decrease average effluent COD value to meet discharge standards. If activated carbon is selected for carbon source adsorption and fixing material, and PVA for immobilization material, the zinc removal rate can reach above 98% under the conditions of 35 and pH 6. Meanwhile, the mechanism of zinc removal has been determinated according to the results from SEM (Scanning Electronic Microscope) and XRD (X-Ray Diffraction).

Jan 1, 2006

By Y. W. Miao

Along the south-west coast of Taiwan is about 550,000 metric tons of heavy sand deposit containing about 10 % black monazite. The Institute has developed a separation process to recover the individual rare earths and the developed process has been commercialized by a local private company. The decomposition of the local black monazite by sodium hydroxide through hydrothermal and fusion methods has been investigated. In the hydrothermal process 4.5 wt. % of aqueous alkali solution was used in an autoclave. In the fusion process, caustic soda (9.8% NaOH) was employed in am open cylindrical reactor. The same product of hydrous rare earth oxides were obtained and then dissolved by hydrochloric acid and the p-H adjusted in order to separate the thorium from the rare earths. After filtration, the filtrate contained rare earth chloride and the cake contained mainly the silica and thorium hydroxide. Both methods give a yield of 90 % with respect to the rare earths recovery. A detailed description of operation and comparison of the two methods are given.

Jan 1, 1989

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 R. G. Reddy

The oxidation kinetics of A13Ti intermetallics have been studied at the temperature range of 850°C to 100O0C in pure dry oxygen. The oxygen diffusion rates were investigated using TGA method. Parabolic rate constants were calculated. The oxidation scales were analyzed using SEM, EDS and X-ray diffraction. A continuous A120, scales with a little TiO2(rutile) were formed on the intermetallic surface. The A13Ti intermetallic exhibited excellent oxidation resistance among the Ti-Al base intermetallics.

Jan 1, 1997