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By S. Neogy, M. Gupta, D. Srivastava, V. Kain, S. Roychowdhury, R. C. Prasad, G. K. Dey

"Austenitic stainless steels are an important material of construction for Boiling Water Reactors (BWR). These stainless steels are amenable to strengthening by strain hardening. Various deformation modes at different test temperatures and strain become active. In the present investigation type 304LN stainless steel was used in the annealed and strain hardened condition. Thin foils were prepared from gauge section for transmission electron microscope (TEM) investigation after tensile testing at room temperature and at 288°C. TEM investigation reveals that twinning is the major mode of deformation for the tests done at room temperature while dislocation cross-slip is the major mode of deformation at higher temperature. Stacking faults were also observed to a limited extent. The extent of twinning was much higher for the tests done using the rolled material. The formation of martensite in the stainless steel due to straining was investigated by the analysis of selected area diffraction patterns.IntroductionAustenitic stainless steels (type 300 series) are an important material of construction in Boiling Water Reactors (BWR). These stainless steels cannot be heat treated but can be strengthened by cold working [1]. Nitrogen alloying of these stainless steels result in high strain hardening rates and higher strength without any loss in toughness [1]. Stress Corrosion Cracking (SCC) in BWR of these types of stainless steels have been attributed to surface strain hardening and strain hardening ofregions adjacent to constrained weldment [2].The test temperature [3, 4], prestrain [5] and nitrogen level [5] has been reported to affect the deformation mechanism during tensile testing. Byun et al. [3] have reported the formation of martensite, dislocations, stacking faults and twinning during tensile deformation, the extent of each depending on the test temperature. Strain localisation has been reported to occur during tensile deformation in irradiated stainless steels [ 6]. The behaviour of rolled material during tensile testing is similar to that of irradiated material to a large extent [3]. Austenitic stainless steels are low stacking fault energy (SFE) materials in which various types of microstructures have been reported to form during tensile deformation and the strain is also highly heterogeneous in nature in these stainless steels which aides SCC in BWR environment to a large extent [7]. During cold working of austenitic stainless steels second order twinning has also been reported [8]. Knowledge about the deformation mechanisms operative in the strain hardened austenitic stainless steels during tensile testing at different temperatures is essential to understand the material deformation behavior and the present study aims at enhancing the existing understanding."

Jan 1, 2011

By M. W. Kennedy

Prediction of the thermal duties of copper coolers in freeze lined furnaces is challenging. Where copper coolers are immersed in liquid slag the heat transfer is often defined by a natural convection cell immediately adjacent to the wall, in the absence of other factors producing forced convection. Slag coolers are typically not fully immersed, slag temperature, liquidus and superheat can vary, and bath levels may change significantly with batch tapping, leading to substantial variations in radiation heat fluxes. Radiation heat transfer is discussed with reference to the non-obvious impact of slag liquidus on radiation losses in the exposed cooler sections. Reference is made to literature and the results of analytical and FEM models.

By N. Tsuchida

Sumitomo Metal Mining Co. Ltd. (SMMC) is currently developing the flowsheet to treat stockpiled limonite, a type of laterite ore, at Rio Tuba on southern Palawan Island, Philippines. The new plant will be commissioned at the end of 2004. Rio Tuba Nickel Mining Corporation (RTNMC) has been mining saprolite since 1977, and the limonite ore located above the saprolite ore body has been stockpiled separately according to nickel and magnesium content. Ore from these stockpiles will be blended and used for the operation. The annual production of nickel will be 10,000 metric tons for the next twenty years. The proposed process consists of ore preparation, high pressure acid leach (HPAL), counter- current decantation wash, impurity removal and sulfide precipitation. Precipitated mixed sulfide will be processed to electrolytic nickel by the Matte Chlorine Leach Electrowinning (MCLE) process at Niihama, Japan. SMMC has established new technologies during the process development, such as zinc removal and sulfide precipitation. Applying this technology, preferential removal of zinc can be achieved by hydrogen sulfide gas with negligible loss of nickel. Precipitation of nickel by hydrogen sulfide gas is carried out at low temperature. Slow kinetics is selected for control of the particle size of the precipitated mixed sulfide. Keywords: HPAL, Zinc Removal, MS Production

Jan 1, 2004

By Oscar Perales Perez, Atsuo Kasuya, Kazuyuki Tohji, Yoshiaki Umetsu

"The removal of iron and various heavy-metal ions by their incorporation into stable ferrite-type precipitates at 25°C is a promising alternative to clean up large volumes of polluted aqueous effluents. Our research work investigated the conditions to produce magnetite and various M-bearing ferrites (where M: Zn, Cu, Co, Ni, Cd, etc.) directly from aqueous solutions at 25°C by simultaneous control of the oxidizing conditions and pH. The formation of the solids was followed by monit9ring the oxidation-reduction potential (ORP) and rate of proton release during the aerial oxidation of the suspensions at constant pH (contact stage). Only mildly oxidizing conditions, represented by ORP values between -110 mV and -150 mV and a moderate oxidation rate of Fe(II) species were conducive to well-crystallized ferrites at ambient temperature.' It was also found that increasing the Fe/M mole ratio in starting· solutions enhanced the stability ·of the M-bearing ferrites at ambient temperature. When the formation of the ferrite was incomplete, aging of the sludges in their mother liquors at 25°C promoted the crystallinity of the precipitates. The mentioned conditions ·favored the suitable progress of the ferrite-forming reaction involving the oxidation of Fe(II) entities, subsequent hydrolysis of produced Fe(III) species and dehydration of the intermediate:· Furthermore,· the ferrite formation at· low temperature permits the elimination of iron and co-existing heavy metal ions to sufficiently low concentration.In tum, the characterization of the precipitates evidenced their magnetic nature (room-temperature saturation magnetization above 60 emu/g) as well as the effective incorporation of target metal ions into the ferrite structure."

Jan 1, 2000

By José Brant, Douglas Torres, Rogério Navarro, Rodrigo Souza, Eduardo Brocchi

The steelmaking process requires the input of ferro-alloys to implement the adjustment of some elements composition in the final product. In the particular case of stainless steel production, the high carbon FeCr alloy stands out as one important precursor. However in the production of this material a certain quantity of fine powder with remarkable chromium and carbon content is also generated, which, in turn, could be processed through alkaline roasting in order to selectively recovery this element in a subsequent aqueous route. In the present work, this process is investigated, using excess of NaOH as oxidizing agent, and H2O2 for precipitating chromium as Cr(OH)3, which is next calcinated to Cr2O3. According to the results, the global achieved recovery has shown to be around 98%, suggesting that the proposed route can be seen as a potential process for chromium oxide production from the mentioned fine powder.

Jan 1, 2015

By E. Fockedey

he destruction of free cyanide on a Co3O4 doped carbon felt was studied. The experiments were done with an eiectrochemical filter press cell on dilute alkaline solutions containing 250 mg/l NaCN. No chloride ions were added to the solutions. The cobalt oxide protects the felt against corrosion and has a catalytic effect on the degradation of the cyanide. This kind of electrode allows working with current density as high as 1200 Aim without any visible degradation of the felt. The most interesting results were obtained with a current density of 400 Aim' at which the cyanide concentration can be lowered to 5 mg/l with a current efficiency of more than 70 % and a specific energy consumption of about 10 kWh/ kg CN.

Jan 1, 1998

By Takao Mori

Novel rare earth boron icosahedral compounds are investigated as potential high temperature thermoelectric materials. REB50-type compounds and REB22C2N compounds were synthesized and the thermoelectric properties measured. Seebeck coefficients in excess of 200 V/K are observed at temperatures above 1000 K for the REB50-type compounds. Strikingly, n-type behavior was observed for REB22C2N. Up to now, non-doped B12 icosahedral compounds have all been p-type. The discovery of an n-type compound is extremely important in terms of the potential development of this class of compounds as viable thermoelectric materials. Low thermal conductivities of < 0.03 W/cm/K at room temperature was observed for these rare earth boron cluster compounds.

Jan 1, 2006

By Versiane Albis Leão

This work aims at the selection of an appropriate eluant for cyanide recycling using ion exchange resins. Based on a literature review as well as on experimental results, the elution of resins loaded with copper and minor amounts of iron and nickel is discussed. The resins Imac HP 555s, Amberlite IRA 900 (Rohm&Hass) and Purolite A860S (Purolite Co) were eluted using either NaCI, zinc and nickel cyanides, hydrochloric acid, sulfuric acid or acid thiourea solutions. The results indicate that saline solutions are effective only with polyacrylic resins (Purolite A860S), failing to desorb the metals, specially the nickel cyanocomplex, loaded on polystyrene-based resins. Cyanide solutions of both zinc and nickel are capable of eluting over 90% of the loaded metals. In contact with pure acid&apos; solutions, iron precipitates onto the resin beads, as Cu(II) ferrous cyanideCu2Fe(CN)6.xH20. Thiourea is able to elute all the three metal cyanocomplexes owing to the increased solubility of copper cyanocomplexes in the presence of this complexing agent. The results demonstrate that a universal eluant is not available and the selection of the most appropriate resin-elution procedure should be based on the specific features of the system under consideration

Jan 1, 1998

By Dinesh Goyal

Industrial fly ash from (electro static precipitator) was mixed with soil at different levels on v/v basis for raising of pulpwood tree species. In field trials conducted on degraded soils increase in the plant growth of Eucalyptus tereticornis, Acacia auriculiformis and Casuarina equisetifolia by 10 %, was observed during the initial six months after plantation at 18-24% (v/v) fly ash concentration which was at par with chemical fertilizer treatment. Level of As, Se and Mo in flyash was 6.2, 3.6 and 4.0 ppm respectively. The radioactivity analyses 40K, soil and 28 fly ash showed that the activity levels of gamma emitting radionuclides K, Ra, Ac were within the permissible limits and mixing of fly ash with soil at tested concentration would have no deleterious effects. Available Co, Cr, Ni and Cd in rhizospheric soils were below detection limit. Fly ash at 10-20 % level (v/v) was also found to be a good potting mix material in forestry nurseries in terms of improving biomass production by 20 %, when tested in nursery seedlings of Eucalyptus tereticornis. Nursery addition of fly ash in soil decreased soil dehydrogenase activity and the soil bacterial population was negatively affected. These results indicate that use of fly ash in forestry sector involving nursery and plantations as a soil amendment agent upto 10-20 % v/v is a gainful utilisation of fly ash.

Jan 1, 2002

By Donghai Li, Cheng Pan, Xuewei Lv, Mei Liu, Enguang Guo

"Phosphorite is the main raw material for the production of phosphorus in chemical industry. More attentions have been drawn to the phosphorite concentrate beneficiated from low-grade phosphorite due to the decrease of high-grade phosphorite. For another, the agglomeration process is necessary for the phosphorite concentrate after beneficiation process. The mineralogy and sintering process of the phosphorite from Leshan, China were studied in this work. The result shows that the main phases in the phosphorite are fluorapatite (Ca3(P04)3F), hydroxylapatite (Cas(P04)3(0H)), quartz (Si02) and dolomite (CaMg(C03)2). The yield of the sinter increases with increasing the carbon dosage to 7%, and then decreases when it continuously increases. Similar regularities were found for the strength and the content of P20s of the sinter. The best strength of the sinter as well as its P205 content were discovered when the carbon dosage is 7%. Fluorapatite ((Ca5(P04)3)F) is the main phase in the sinter while fuggerite (Ca2MgSiz01) is the main binder phase.IntroductionPhosphorus is an important foundation industrial raw material of national defense industry, food industry and chemical industry, where it is used to produce red phosphorus, phosphonium hydroxide, phosphorus pentasulfide and phosphoric anhydride[l-2]."

Jan 1, 2013

By Batric Pesic

Solvent extraction of nickel and cobalt from the real leach solutions was studied by using a novel extraction system. The extraction system was a mixture of 2,6-bis-[5-n-nonylpyrazol-3¬y]] pyridine (BNPP) and dinonylnaphthalene sulfonic acid (DNSSA). The BNPP represents a novel molecule, which was designed and synthesized in our laboratory. Real solutions for the study were prepared by leaching of two different cobalt-nickel bearing concentrates, cobaltite [CoAsS] concentrate from Blackbird Mine, Idaho, and siegenite [(Ni,Co)3S4] concentrate from Missouri Lead-Belt. The major strength of the system was the selectivity of extraction toward nickel and cobalt from iron containing solutions. Other metals such as Mn, Mg, Ca, Al and As were not extracted. Due to the irreversibility of copper extraction, its removal from solution was required prior to the extraction of nickel and cobalt. Zinc was not as strongly extracted (i.e. its stripping was readily achieved) as was copper . Flowsheets for the recovery of nickel and cobalt were also developed.

Jan 1, 1997

By Guy L. Fredrickson

A modified transpiration reactor was used to measure the composition of the equilibrium gas phase formed above compounds in the Hg-O-S system at high temperatures (600 to 900K). A thermodynamic database {(AGo°f AH°t. AS°t)} for-HgO, HgS, HgSO4, Hg2SO4, HgSO4?HgO, and HgSO4?2HgO was developed based on the experimental results. Prior to this study, only estimated data were available in the literature for the sulfates and oxysulfates at temperatures above 298K. A series of vapor pressure&apos; stability diagrams were constructed from 473 to 973K with isobars of Hg(g), HgO(g), S2(g), and SO3(g). These diagrams were found to be significantly different than those available previously and do provide insight to the phase relations of importance during the thermal processing of Hg-containing wastes. The thermodynamic results were used to conduct a series of Gibbs energy minimization calculations for a thermal processor&apos; afterburner system for the treatment of HgS-containing wastes. The retention of Hg in the discharge calcine was examined as a function of temperature and excess air. Hg was found to report to the calcine as HgSO4, Hg2SO4, or HgSO4 HgO depending on the process conditions, and Hg retention occurs at temperatures as high as 930K. The precipitation of Hg-containing phases from cooled afterburner discharge gas starts at approximately 900K and the cooling of the gas an additional 30K (to 870K) results in over 50% of the Hg being preCipitated as HgS04?HgO. It was also determined that for small amounts of Hg present in sulfide concentrates during roasting, the Hg will be retained as HgSO4 or HgSO4?HgO at temperatures as high as 870K.

Jan 1, 1996

By Hong Liang-shi

Olivine lithium iron phosphate (LiFePO4) is considered as one of the most promising materials for lithium-ion secondary batteries because of its high theoretical capacity, low cost, good safety, benign environment and good cycle performance. In this paper, carbon-free and/or carbon-coated olivine lithium iron phosphate composite ultrafine powders were successfully synthesized from aqueous precursor solutions of (NH4)2Fe(SO4)2?6H2O, H3PO4 and LiOH?H2O by co-precipitation method. The obtained LiFePO4 or LiFePO4/C powders were characterized by X-ray diffraction (XRD) and scanning electron microscope (SEM). Their electrochemical performance was investigated in terms of cycling behavior. As confirmed by X-ray diffraction and scanning electron microscope, the material obtained by co-precipitation within the temperature range of 60ºC to 100ºC and then followed by moderate heat treatment are a single-phase olivine LiFePO4with the particle size of about 300nm. An improved carbon-coated olivine LiFePO4/C material was prepared by adding conductive carbon materials, such as glucose, activated carbon and acetylene black, into the precursor. The carbon dispersed in the materials increases the electronic conductivity of LiFePO4/C composite, and consequently, leads to high rechargeable capacity of the material. The carbon-coated material with carbon amount of 7.64%wt obtained from glucose has the first discharge capacity of 150.3mAh/g at the rate of 0.1C and 129.3mAh/g at the rate of 1.0C, respectively. After cycled for 50 times, the capacity retention rate is 95.13% at the rate of 1.0C in the voltage range of 2.5 to 4.3 V vs. Li/Li+.

Jan 1, 2006

By H. Bai, B. G. Thomas

"A three-dimensional finite difference model has been developed to study the liquid steel-argon bubble two-phase turbulent flow in continuous casting tundish nozzles. Experiments have been performed on a 0.4-scale water model to verify the computational model by comparing its prediction with velocity measurements using PIV (Particle Image Velocimetry) technology. The computational model was developed using CFX and then employed to investigate the effects of various casting process variables. A fast, simple inverse model to quantify relationships between those process variables was developed, based on interpolation of the numerical model results, using Bernoulli's Equation and advanced multivariable curve fitting methods. Predictions using this model compare well with plant measurements. The model has been applied to present trends and observations on the relationship between casting speed, tundish depth, slide gate opening, and argon gas injection rate. The results can also be used to predict .the theoretical steel flow rate through the nozzle, so that clogging conditions can be identified in the plant.IntroductionTundish nozzle geometry is one of the few variables that are both very influential on the casting process and relatively inexpensive to change. Designing an effective nozzle requires quantitative knowledge of the relationship between nozzle geometry and other process variables on the influential characteristics of the flow exiting the nozzle. This relationship depends on the flow pattern within the nozzle components. Most previous modeling studies of flow in the nozzle have focused on single-phase flow [1-4]. Argon injection into nozzle is an efficient and widely employed method to reduce nozzle clogging, even though the real working mechanism(s) are still not fully understood [5]. Argon injection may greatly affect the flow pattern in the nozzle, and subsequently in the mold. Therefore, two-phase flow modeling is needed to improve understanding of fluid flow in the nozzle."

Jan 1, 2000

By S. Fitzel

The Betts process for electrorefining of lead has been in operation since 1902 in the Trail Operations Metallurgical complex. The Betts process allows production of high purity lead in a single electrochemical step. Process improvements and plant expansions have taken place over the many decades of operation of this process which has proven to be robust, flexible, and capable of successfully treating a large range of anode bullion compositions. This paper reviews the history of the Betts lead electrorefining process, the innovations and quick industrial adoption of new discoveries that took place at the end of the nineteenth century. The process was first implemented in Trail Operations and integrated very well with metallurgical needs then and now.

By J. E. Dutrizac

A mineralogical study of a weak acid leach residue from the Clarksville zinc plant of Savage Zinc Inc. was carried out. The study focused on Pb and Cd as these elements most significantly impact on the environmentally acceptable disposal of the residue. The residue consists of major amounts of bassanite, zinc ferrite and various Zn-Pb-Fe-Cd silicate species. Also present are lesser quantities of PbSO4, sphalerite, Fe2O3 quartz, Mn-Pb-Fe oxides, SrS04, (Pb,Sr)SO4 iron gel-silica gel, jarosite and Ti oxide. The principal Cd carriers are the zinc ferrite, which contains up to 9.00% Cd and likely accounts for -45% of the total Cd content of the residue, and the various silicate species which contain up to 6.97% Cd and account for about 45 % of the total Cd. The sphalerite is a minor Cd carrier containing an average of 0.35 % Cd and accounting for -5 % of the total Cd; the other carriers contribute only trace amounts to the total Cd content. The major Pb carriers are PbS04, Pb-bearing silicates and Mn-Pb-Fe oxides. Minor proportions of the total 1.09% Pb content of the residue are carried by SrS04 and (pb,Sr)S04&apos; Trace Ph carriers include the iron gel-silica gel, Fe-Zn-AI oxide and bassanite. The residue after the toxicity characteristic leaching procedure (TCLP) is mineralogically very similar to the initial weak acid leach residue; the amounts of calcium sulphate are approximately the same in the two products. The principal Cd and Pb carriers are also the same as those noted in the initial residue, except that some dissolution and reprecipitation of Pb-Sr sulphate takes place. That the residue fails the TCLP test is likely a consequence of the superficial dissolution of Pb and Cd from species such as PbS04 or Zn-Pb-Fe-Cd silicate.

Jan 1, 1995

By C. Takano

The integrated iron and steelmaking industry generates large amounts and many types of solid dusts and sludge, at different phases of the production. Within these are: sludge of the Blast Furnace; coke fines; fine and coarse fractions from oxygen converters; sludge from water treatment at rolling mill unit; and others. In this paper the above dusts and sludge were physically and chemically characterized. The obtained results allowed defining self-reducing pellets using these materials. The high temperature behavior of the pellets were evaluated. Good results, with no decrepitation and swelling, and high yield of reduction, show that it is feasible to recycle them, as self-reducing pellets, in oxygen steelmaking converter.

Jan 1, 2001

Lead blast furnace water-jacket stability was investigated by examining samples from the Port Pirie Lead Smelter. The compositions of the phases formed in the samples were analysed using Scanning Electron Microscopy (SEM) and Electron Probe X-ray Microanalyser (EPMA). Phase equilibria analysis and thermodynamic modelling was undertaken using FactSage with latest thermodynamic database for the slag/matte/metal/speiss/solids multi-component Cu2O–PbO–ZnO– Al2O3–CaO–MgO–FeO–Fe2O3–SiO2–S major and As–Bi–Sb–Sn–Ag–Au minor elements system. Results indicated that the stability of the water-jacket steel wall without freeze-lining is influenced by formation of the complex Fe-rich speiss phase at critical As concentrations. The integrity of the furnace walls with freeze-lining is critically dependent of the stability of the oxide-based freeze-lining which is dependent on various factors including most critical one—the proportion of solids determined by the slag chemistry and fluxing. Thermodynamic modelling of the lead blast furnace operation indicated limiting thermochemical conditions for the water-jacket stability. Factors and controls critical to the water-jackets integrity are discussed.

By Djona M. Gaballah I.

Selective chlorination of unroasted and roasted spent hydrorefming catalysts was studied between 300 and 600°C using the following gas mixtures : C12+CO, C12+N2 and CI2+air. Such materials contain Co, Ni and Mo compounds supported by alumina and/ or silica. They also contain variable amounts of V compounds, C, S, etc., accumulated during the life time of the catalyst. Direct oxychlorination of the C+S rich sample allows higher extraction rates than those obtained by the carbochlorination of the same roasted one. It seems that the roasting step doesn&apos;t favor the economic metals&apos; recovery. Results of the chlorination of C+S poor spent catalysts, in the presence of CO, in the chlorinating gas mixture, or of carbon added to the sample, were comparable. Cobalt and nickel chlorides were .extracted from the chlorination residues by their dissolution with acidified water, whereas molybdenum and vanadium chlorinated compounds were recovered by selective condensation from the vapor phase. The recovery rates of valuable metals as well as the selectivity were higher for the chlorination of spent catalysts than results obtained by the hydrometallurgical processing of the same sample. Results of the scale-up of the oxychlorination of the unroasted sample confirmed those of the laboratory scale. The global recovery rates were about 88 pct of cobalt, 93 pct of molybdenum and 76 pct of vanadium. The carbochlorination was applied to the recovery of W and Ti from Denox catalyst that is a carbon and sulfur free one. Recovery rates higher than 99 pct at temperatures lower than 500 °C could be obtained. This may indicate that the chlorination process can be applied to the treatment of various industrial wastes or by-product containing transition and/or refractory metal compounds A flow - sheet for the pretreatment of these materials is proposed.

Jan 1, 1995

By James B. Pfeiffer

TETRA Technologies, Inc., has applied its HDSIM metals precipitation system to treat a waste stream containing scrubber blowdown and process water from a smelter operation. The combined stream contained cadmium, lead, selenium, arsenic and zinc, plus some iron and copper. Treatment requirements included meeting stringent mass flow limitations for specific heavy metals. The HDS ? system can reduce the arsenic from 600 ppm to less than one ppm. The process generates a dense sludge that can be reprocessed in a smelter, eliminating the liability associated with landfilling. Flow diagrams and process details are discussed.

Jan 1, 1994