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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 R. Padilla, M. C. Ruiz, R. Villa

"Bismuth is an impurity in copper minerals where it occurs mainly as the mineral bismuthinite (Bi2S3). In smelting of copper minerals, most of the bismuth reports to the white metal, as a result, a substantial amount of bismuth accompanies the copper to the electrorefined cathodes. Thus understanding the behavior of Bi2S3 at high temperatures is crucial to eliminate bismuth before electrorefining. In this paper, some experimental data on the decomposition/volatilization of bismuthinite in nitrogen- oxygen atmospheres is discussed. The results indicated that in nitrogen atmosphere, bismuth volatilization occurs through a fast decomposition of bismuthinite to metallic bismuth and sulfur with subsequent volatilization of bismuth in the range 850-1100 °C. Similarly, in the presence of oxygen, bismuthinite decomposes to bismuth too, followed by oxidation to the non-volatile bismuth trioxide at temperatures higher than 750 °C. Both, temperature and partial pressure of oxygen affect significantly the bismuth volatilization and the oxidation rates.IntroductionCopper sulfide minerals are the major source for the production of metallic copper by pyrometallurgical processes, which are the dominant processes in the production of copper by selectively oxidizing the sulfide sulfur to SO2 and the accompanying iron in the concentrates to iron oxide, which can be conveniently removed as a stable slag.Generally, copper concentrates contain some deleterious minor elements such as arsenic, antimony, bismuth and lead, which are present as sulfides. These elements depending on their concentration may originate problems in the copper smelting processes and they can ultimately lead to a final copper product with unacceptable high levels of impurities.During the treatment of these copper concentrates by smelting, the impurities generally distribute themselves in the condensed and gas phases and they are eliminated mainly through the gas phase [1-3]. Thus, smelter off gases contains substantial amounts of volatilized impurity elements. For example, in the case of bismuth, the estimated distribution of bismuth in flash furnace smelting [2] was 15 % in the matte, 5 % in the slag and 80 % in the gas phase, and recently, for Outokumpu flash smelting Davenport [3] reported the distribution of bismuth as 30-75% in matte, 5-30% in slag and 15 -65 % in the off gas."

Jan 1, 2011

By Jerry L. Smith

Industry on a whole has not been very receptive to government prodding to implement waste minimization programs. Waste minimization has the appearance of substantial benefits, however, there are underlying difficulties and suspicions that need to be addressed before industry will support pollution prevention initiatives. They can be summarized as follows: - Human behavior resists change, uncertainty, and unknowns. - New waste minimization techniques are difficult to find and research. - Calculating the true cost of present waste practices as well as new techniques being considered is difficult and time consuming. - Getting a consensus opinion of all the individuals affected on the course or technique to be employed in a pollution prevention program. New software products have addressed many of the problems associated with implementing pollution prevention programs: They contain research on a large number of pollution prevention techniques and case studies; they generally are accessed by EPA ID number, chemical name, or synonym; and some programs have the option to print a comprehensive written user-specific pollution prevention program.

Jan 1, 1994

By Heimo Thalhammer

During the refining of lead, copper or other metals the furnaces used in the process · often produce waste gases. This paper illustrates how these waste gases can be successfully treated and destroyed by CTP 2-bed or multi-bed compact systems, modified for the additional reduction of dioxins and furans. The CTP regenerative thermal oxidizer also destroys voes (organic compounds and odours) using ceramic blocks as a heat exchanging media. The raw gas is forced through the ceramic beds where it is heated up to the oxidation temperature level. The voes, dioxins and furans are destroyed in the combustion chamber, subsequently generating water, eo2 and heat. The hot purified gas heats up a second ceramic bed, which is used to preheat the raw gas after the valves have been switched. This process does not produce any secondary waste such as contaminated water, polluted air or any other products that have to be disposed of.

Jan 1, 2000

By Lin Yang, Yuanbo Zhang, Zhuoxuan Li, Guanghui Li, Jinghua Zeng, Tao Jiang

A technique has been proposed for recovering iron from hematite-rich diasporic-type bauxite ore in this study. Direct reduction roasting followed by low intensity wet magnetic separation process was carried out. The parameters including reduction temperature and time, sodium salts, grinding conditions and magnetic field intensity for separation of iron were determined. The optimum process parameters as follows: roasting temperature of 1050 oC, time of 60 min, sodium salts involving sodium sulfate, borax, sodium carbonate with dosages of 10 wt%, 2 wt%, 35 wt% respectively, and magnetic field intensity of 1000 Gs with fineness of pulp reached 92.75% passing -0.074mm. Under the optimal conditions, an iron concentrate containing 88.17% total iron grade and iron recovery of 92.51% was obtained, 4.55% total iron grade in tailings. This novel technique provide a potential route for utilizing hematiterich diasporic bauxite ore, recovering iron resource firstly, and extracting alumina from magnetic separation tailings further.

Jan 1, 2015

By John J. Dunkley

Recent years have seen the increased use of hydrometallurgy in the smelting and refining of metals. However this is often used as a final refining step, following an initial pyrometallurgical smelting process. Huge amounts of material are produced as melts which have to be cast, comminuted, and taken up into solution or leached. A common method is to granulate the melt and then grind it. In the case of metallic melts this can be difficult or unfeasible due to the ductility of the granulated particles. Water atomisation is capable of replacing the granulation and grinding stages with a single process step that can process in excess of 30tlhour of melt into particles as fine as 50 microns. Applications in operation in Co, Cu, Ni, Ag, Au, Pt and Rh refining are discussed together with potential applications in copper smelting.

Jan 1, 2003

By Qingchun Yu, Baoqiang Xu, Yongnian Dai, Bin Yang, Fulong Zhu

"In this paper, the mechanism of the carbothermic reduction-chlorination process to extract aluminum from alumina in vacuum was investigated. The carbon monoxide (CO) content of the gas, phases of the reduction slag, surface morphology of the reduction slag and the product aluminum were measured by means of gas chromatography (GC), XRD, and SEM. The experimental results indicated that the content of CO in the gas decreased, but Al4C3 increased with time at 1773K during the carbothermic reduction process of alumina. AlCl(g) and graphite (C) were produced by the reaction between Al4C3 and AlCh(g) at 1773K, and then aluminum beads generated after the decomposition of AlCl(g). It implied the mechanism of alumina carbothermic reduction-chlorination process in vacuum involves three steps as follows: the carbothermic reduction of A}z03 to produce Al4C3, the chlorination of Al4C3 by AlCh(g) to produce AlCl(g), and the decomposition of AlCl(g) to produce Al(l).IntroductionAluminum is the basic raw material for many industries [1], and it is used extensively because of various excellent properties such as light weight, good malleability, high strength, excellent thermal conduction, high corrosion resistance and so on [2]. Industrial production of aluminum currently includes refining alumina and electrolytic aluminum processes. However, its development has been effected by some factors such as high energy consumption and heavy environmental burdens [3]. In the past several decades, there had been numerous attempts to produce aluminum by new methods. Extracting aluminum from alumina or bauxite directly by carbothermic reduction-chlorination process had been studied [ 4-6]. Although the alumina carbothermic reduction process [7~9] had been studied, the mechanism of the carbothermic reduction-chlorination process had not been systematically elucidated.In order to investigate the mechanism of the carbothermic reduction-chlorination process in vacuum, GC, XRD and SEM techniques will be used to determine the CO content and to characterize the surface morphology and composition of the slags at various temperatures."

Jan 1, 2011

By J. E. Sallee

An experimental study has been conducted on the level of arsenic contamination in samples of zinc oxide when the zinc oxide is contacted with gas mixtures containing As4O6(g). This contamination has been determined as a function of A4O6 saturation pressure, temperature, zinc oxide sample surface area, impurities, and oxygen level in the gas mixture. The results indicated a rather clean separation can be achieved between condensed zinc oxide and gaseous arsenic oxide as long as attention is given to temperature control, and the final zinc oxide surface area. For a 300°C operation temperature and an AqOg saturation pressure of 0.38 TORR (or 0.05% As406 by volume), the contamination level is expected to be approximately 100 ppm. This suggests that arsenical dusts can be treated in the HRD flame reactor process and a reasonable purity zinc oxideproduct produced. The results also show no evidence of zinc arsenite or zinc arsenate formation.

Jan 1, 1994

By Ralph H. Nafziger

The feasibility of smelting a Ni-Co-Cr-bearing laterite ore from southern Oregon was evaluated by the Bureau of Mines. The objective was to prepare a master alloy for subsequent stainless steel production. A mixture of the ore with suitable reductants and fluxes was smelted in a 50-lb-capacity single-phase ac electric furnace under sub- merged arc conditions. The smelting tests produced a metal in which most of the nickel was concentrated. High-chromium recoveries required an excess of carbon. The resulting metal alloys contain sufficient nickel for some stainless steels. Ferrochromium additions would be required to attain suitable chromium levels. This research was conducted under the Oregon Metals Initiative in cooperation with Walter B. Freeman.

Jan 1, 1993

By M. Bhattacharya, A. Dutta, P. Barat

"Pinning of dislocations at nanosized obstacles like precipitates, voids and bubbles, is a crucial mechanism in the context of phenomena like hardening and creep. The interaction between such an obstacle and a dislocation is often explored at fundamental level by means of analytical tools, atomistic simulations and finite element methods. Nevertheless, such studies fail to predict the effect on the overall plasticity on account of insufficient information about the underlying statistics of this process comprising a large number of dislocations and obstacles in a system. Here we propose a new statistical approach, where the statistics of pinning at idealized spherical obstacles is explored by taking into account the generalized size distribution of the obstacle along with the dislocation density within a three-dimensional framework. The application of this approach has been demonstrated for dislocation pinning at nanovoids in neutron irradiated type 316-stainless steel.IntroductionPresence of nanoscale obstacles like precipitates, voids and bubbles play a crucial role in determining the deformation behavior of a crystalline solid on account of the interactions between the line defects and such localized obstacles. In the context of the glide motion of dislocations, the obstacles can offer resistance to a moving dislocation, thereby causing a hardening effect [l-3]. In some other cases, inclusions like voids and bubbles can affect the rate of dislocation climb through diffusive [4] and non-diffusive [5] mechanisms. Over the last few decades, numerous studies have been performed to gain an insight of the dislocation-obstacle interactions at a fundamental level. These include the interactions responsible for the hardening effect, in addition to those pertaining to the non-conservative motion of dislocations.Although the elementary mechanisms of the various dislocation-obstacle interactions have been vastly explored and understood by means of analytical theory and numerical simulations, it remains difficult to quantitatively understand their effects on the macroscopic deformation behavior. This is due to the fact that their influence on the gross plastic deformation of a bulk sample would be the collective outcome of a large ensemble of such interactions. As a result, it becomes infeasible to predict the bulk deformation behavior of a material until the statistics of pinning of the dislocations at the localized obstacles is available. In the context of precipitate hardening, some well known attempts to extract the pinning-statistics were made by Friedel-Fleischer [6] and Mott [7] by analytical means, which were later tested through simplified 2-dimensional in-silica modeling [8]."

Jan 1, 2014

By Jingwei Lou, Bing Li, Suzhen Li, Miao Shen, Jianguo Yu

"As a main impurity in primary lithium metal, magnesium is difficult to remove because of the very close relative volatility of the two metals. Electrochemical refining provides a possibility to completely remove Mg in the LiCl-KCl melt prior to Li reduction. MgCl2 reduction processes in LiCl-KCl- MgCl2 melt were investigated by cyclic voltammetry (CV), square wave voltammetry (SWV), chronoamperometry and chronopotentiometry. Then potentiostatic electrolysis was carried out and Mg (II) ion was reduced onto a liquid lead cathode from the LiCl-KCl-MgCl2 melt at the Mg deposition potential. The results show that Mg ( II ) is reduced in one step with two-electron transfer. The reduction potential of Mg ( II ) was well defined. The reduction of Mg( II) results in Li ( I ) underpotential deposition at 0.2V more negative potential than that of Mg( II) reduction. Therefore, in order to prevent Li ( I ) from codeposition with Mg, accurately controlling Mg ( II) reduction potential during the potentiostatic electrolysis was necessary. Ninety three to 99 % removal rate of MgCl2 was achieved after 8-12 h electrolysis when liquid lead was used as cathode.IntroductionMetallic Li has been widely used in batteries, light weight alloys and in fusion reactors because of its excellent properties. Currently, the only way in industry to produce metallic Li is by electrowinning from molten LiCl-KCl at about 450 °C [l-5]. LiCl-KCl is the only electrolyte used, because they presents a lower eutectic temperature and KCl shows a slightly higher theoretical decomposition voltage than LiCl, as shown in Table l .The produced metallic Li generally contains 1-2 wt% impurities including Na, K, Al, Ca, Mg, Si, etc. [6l, which are derived from the corresponding metal chloride compounds or metal oxide compounds existing in the LiCl and/or KCl raw materials. These impurities have to be removed by subsequent vacuum distillation at high temperatures to meet the requirements for metal Li purity in the final products. Separation of Mg from Li by vacuum distillation is difficult because their relative volatilities are very close, as shown in Table 2."

Jan 1, 2011

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 David Cocke

Study of surface and subsurface interfacial chemistry of metallic and similar systems has its enormous technological importance. Copper, for example, is a common component of many alloys and bulk amorphous systems. It is being increasingly studied today because of its use for electronic interconnect systems where processing is done below 200 ºC. Since several types of copper oxides exist, and the degree of their formation is dependent on temperature, perhaps characterization by EDS-SEM depth profiling and EIS might delineate one type of oxide from another. In this paper, we described our work on transformation of copper oxides with temperature ranging from 70 to 350 °C and their characterization by SEM, EDS, and XRD. We also showed the use of the phase angle portion of the impedance as a means to identify the predominant structure and the transition through Cu3O2 between the predominant stable CuO and Cu2O.

Jan 1, 2009

By W. K. Connor, O&apos

The Bureau of Mines has conducted beneficiation, carbothermic reduction, and leaching tests of Mn oxide ores as part of its evaluation of the Mn and Co resources of the West- Central Arkansas District. The major Mn oxides in the ore include cryptomelane, psilomelane, pyrolusite, and lithiophorite. Cobalt is contained within the Mn oxides. Nonbeneficiated ore was reduced at 800' C with coal and leached in ammonium sulfate and ammonium carbonate leach liquors. Ore concentrates were calcined at 600" C prior to reduction under the same conditions as the raw ore. Head analyses reported up to 21 ptt Mn and 0.11 pct Co. Extractions of 70 to 90 pct Mn and 40 to 60 pct Co were achieved.

Jan 1, 1992

By Richard B. Stein

Bechtel's BEMSIM computer program is a useful tool for solvent extraction-electrowinning plant design optimization. Its power (up to 90 stream components, 240 process streams, 180 process steps) has been applied to investigate floweheet configurations in order to perform basic engineering, sizing of plant equipment and to optimize performance of commercial-size copper plants. Flowsheet variations presented include series, parallel and series-parallel extraction stages, while heat balances simulate operations in summer and extreme winter conditions. The BEMSIM program has also been applied to nickel-cobalt, gold and manganese extraction.

Jan 1, 1993

By Aert Driessen

Australia has large resources of rare earths -- 4.35 Mt of contained rare-earth oxides (REO) in the demonstrated category and 1.69 Kt in the inferred category. Australia's demonstrated REO resources are contained in about equal proportions in placer deposits, which also host Australia's titanium and zircon resources, and in hard-rock deposits. The largest single deposit of rare earths, at Mount Weld in Western Australia, is contained in regolith overlying a carbonatite pipe. It has a demonstrated resource of 1.73 Mt of contained REO and yttrium oxide. The largest demonstrated resources of REOs in placer deposits are in the Murray Bash, southeastern Australia -- a total of 1.90 Mt of contained RE0 in six deposits. However, the REO-bearing minerals (monazite and xenotime) are of secondary importance and their recovery will be determined by the market for titanium dioxide and zircon. The Murray Basin and other pre-Pleistocene basins offer the greatest potential for discovering more REO resources. Australia produces about 7000 t/year of REO in monazite and xenotime nearly all from Western Australia, as by-product of mineral-sand mining; monazite production is about 12 000 t/year (6600 t REO) and intermittent xenotime production is about 50 t/year (25 t REO). About 8000 t/year of monazite containing about 4400 t REO is not recovered separately, or is lost in tailings, as is an unknown but smaller amount of xenotime.

Jan 1, 1992

By Neng-Wen Yu, Miao Wang, Ji-He Wei

The mass transfer characteristic between powder particles and liquid steel in the RH-PTB (Powder Top Blowing) refining has been investigated in a water model of 1/5 scale for a 90t RH degasser. The sodium chloride powder with analytical purity has been used as the flux for blowing. The mass transfer coefficient of the liquid side has been determined under the conditions of RH-PTB process. The influences of the main technological and structural parameters on the mass transfer rate have been examined. The results indicated that under the conditions of the present work, the mass transfer coefficient on the liquid side increases with raising the lifting gas blowing rate, inner diameter of the up-snorkel, circulation rate of the liquid and particle size of powder flux. And it decreases with an increase in the inner diameter of the down-snorkel. It is in the range of (l.36-7.30) x 10·4 mis, the appropriate dimensionless relationships have been obtained as follows:

Jan 1, 2000

By Satoshi Yamashita, Noboru Masuko

"Newly prepared bipolar membrane is promising to become a key material of an electrolyser for a production process of strong reducing solvent. This research is basic research for using bipolar membranes as electrolysers of reducing agents, Cr(II), TI(III) and V (II) on the laboratory scale. In this report, a bipolar membrane was tried with an electrolyser, reducing chromic chloride to chromous chloride. An analysis of mass balance demonstrates advantages of it over the former electrolyser equipped with an anion and/or. cation exchange membrane. The effects of current density and concentration of Cr(lll) on the reduction rate of Cr(II) and the current efficiency were examined No deterioration of the bipolar membrane resulted from the electrolytic reduction of Cr(III). IntroductionRecently, bipolar membrane that was the development subject for a long time in the industry of ion exchange membranes has met the stage of the practical application at last [l]. The expectation of the application to the hydrometallurgy field increases. We took up the manufacturing of the strong reducibility solvent as part of the application of bipolar membrane to hydrometallurgy technology. This laboratory has much experience in the electrolytic reduction of Cr (II) aqueous .solution such as chromous sulfateusing bipolar membrane were compared in theory to chromous chloride aqueous solution manufacturing of the strong reducibility solvent. The advantage of applying bipolar membrane by substituting ion exchange membrane is described, and the experimental result is reported."

Jan 1, 2000

By Chuan-fu Zhang

Li(Nil/3Col/3- xMnl/3)MxO2(M=Ti, Mg) cathode materials were prepared from LiOH?H2O and oxalate precursor. The physical and electrochemical properties were studied by XRD, SEM, cyclic volt-ampere (CV), AC impedance and constant current charge-discharge. The results show that crystal volume of Ti4+ or Mg2+ doped sample is increasing and the electrochemical reaction resistant Rct is decreased at high rate, improving the cyclic performance and rate capability. The effect of Ti4+ doped is better than Mg2+. The sample is well crystallized and simple pure phase with a-NaFeO2 layered structure when doping quantity x=0.025. The second specific discharge capacity of Li(Nil/3Col/3- 0.025Mnl/3)Ti0.025O2 is 143.2mAh/g at 1C,128.0mAh/g at 2C in the voltage of 2.75-4.3V,and still has 140.7mAh/g and 121.7mAh/g after 20 cycles, respectively, keeping 98.25%, 95.07% capacity.

Jan 1, 2009

By Kun Wang, Xinhui Li, Huaqing Xie, Qingbo Yu, Qin Qin

"Three typical model compounds of bio-oil (ethanol, acetone and phenol) were studied in the steam reforming process for hydrogen production. In the thermodynamic analysis, the three componds showed the similar trends. The hydrogen yields increased with the increase of steam/carbon (S/C) ratios, and the temperatures of the maximum hydrogen yields moved afterward to low temperature zone. However, the hydrogen contents were just about 70%. For improving hydrogen yield, a new system for steam reforming of bio-oil with site CO2 capture was put forward. This system required the catalst with the larger granularity having greater mechanical strength and higher abrasion resistance. So, six Ni-base catalysts loaded on Al2O3 particles prepared were used and among them, Mg-Ni/Co catalyst showed the best catalytic performance. For the simulated bio-oil (the mixture of the compounds), the hydrogen yield can attain 63% with Mg-Ni/Co catalyst with the good stability and regeneration ability.IntroductionCurrently the interest in the use of hydrogen as a clean energy carrier is increasing, and the main way for producing hydrogen is steam reforming of fossil fuels, containing steam reforming of nature gas, naphtha and coal. But this way caused substantial amounts of CO2 emitted, and these sources of hydrogen which are non-renewable energy will eventually be used up [1, 2]. As a kind of renewable energy, biomass is recognized as an attractive alternative to fossil fuels, because of its neutral CO2 emissions [3]. There are mainly two thermochemical processes using biomass to produce hydrogen, gasification and flash pyrolysis followed by steam reforming (SR) of the biooil produced in the flash pryolysis process [4]. The latter was known as one of the most promising and economically viable methods for hydrogen production [5]. In the last decades, the biomass flash pyrolysis technology was adequately developed and fairly mature [6]. But the steam reforming of bio-oil is still at the research stage and yet has been leading to more and more concerns by the researchers. In their research, the catalysts were widely studied and yet mainly were powdery[7-10], and the reactors manily were fixed bed reactors[11-13], readly causing the carbon deposition and the catalyst deactivation, against the continuous running. In this paper, a new systerm was put forward and could realize continuous production of hydrogen, yet needed catalysts with the larger granularity having greater mechanical strength and higher abrasion resistance, as well as powdery CO2 sorbents which mainly calcium oxide based ones.In this paper, the thermodynamic analysis of the steam reforming processes of three typical bio-oil model compounds (ethanol, acetone, phenol) was performed, and the effect of S/C ratio and temperature on the hydrogen yield and the compositions of gaseous products were investigated. Then, a new systerm for steam reforming of bio-oil with site CO2 capture was put forward, and the catalysts with a certain granularity were prepared and studied."

Jan 1, 2014