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By Jilai Xue, Jun Zhu, Yongqiang Liu

"Up-grading silicon feedstock by removing B and metal impurities can improve process efficiency and lower production cost in metallurgical processing for solar cells production. Hydrometallurgical study has been carried out in laboratory through alternative treatments of the metallurgical grade (MG) silicon (-200 mesh) by using hydrogen peroxide, hydrofluoric acid (4 mol/L) and NH4Cl-NH4 F (30:5) solution. The experiments were usually performed under mechanical agitation at 70 ? for 5 h. ICP-AES analysis showed that B content in MG silicon after the hydrometallurgical treatment has reduced by 92.4 %, and Fe, Al, and Ca contents by 98.8 %, 98.0 % and 81 %, respectively. Kinetics of these processes was also studied for better understanding of the effects of silicon powder size, acid concentration, leaching and oxidizing time on the processing chemistry.IntroductionAs one of the most clean and promising new energy, solar energy is used more and more in many countries all over the world, especially in United States, Japan and European Union. Most of industrialized states have made their national photovoltaic plans, which have stimulated further increase in use of solar energy. Photovoltaic Industry is at a high growth rate about 30 % [1-2]. For silicon solar cells to remain the mainstay for the photovoltaic industry it is necessary to develop a low-cost solar grade silicon feedstock [3]. At the same time, the availability of the currently M-G silicon from the semiconductor industries becomes limited [4]. With the advantages of low cost and low energy consumption, metallurgical routes to product solar–grade silicon get more attention [5]. These routes mainly include pickling, slagging, vacuum processing and directional solidification, etc [6]. Among them the most important processing step is the directional solidification, but it still can not satisfy the industrial demand for removing B. Removing B from Si remains as one of the most difficult and important processes in making M-G silicon [7]."

Jan 1, 2012

By J. W. Lyman

Nickel-metal hydride (Ni-MH) battery electrodes have been developed as a substitute for cadmium-containing negative electrodes. Use of Ni-MH electrodes offers enhanced electrochemical properties in many instances as well as reduced environmental toxicity. Rechargeable batteries using Ni-MH electrodes are also strong candidates for electric vehicles. During the production and secondary reclamation of these battery types, recycling procedures will be needed to prevent environmental impact caused by these wastes as well as to recover the value inherent in the scrap. The U.S. Bureau of Mines (USBM) is investigating hydrometallurgical technology that separates and recovers purified metallic components from Ni-MH battery scrap of two types, AB, and AB,. An investigation of acid dissolution and metal recovery techniques has determined several processing alternatives that may be used to promote the successful recycling of much of the battery fabrication scrap and eventual secondary scrap. Although recovery techniques have been identified in principal, their applicability to mixed battery waste stream and economic attractiveness remain to be demonstrated.

Jan 1, 1995

By M. I. Kalashnikova

Gipronickel Institute has developed the technology of treatment of difficult to concentrate sulphide Pb-Zn concentrates (Zn-19,9%, Pb-8,4%, Cu-0,34%, Fe-8,8%, Ba-6,8%, S-18,7%, Ag-106 g/tonne). The technology consists of pressure leaching, impurity removal from leaching solution, electrowinning and Pb-Ag containing cake treatment. Despite low zinc content in initial concen-trate the technology allows production of solution which is suitable, after standard procedure of impurity removal, for electrowinning with production of zinc grade SHG. Comparing to the standard technologies the flowsheet developed provides the lesser expenses per zinc unit because of decreasing of liquid to solid ratio at pressure leaching stage. The initial concentrate is characterized along with low content of principal metals by high con-tent of barite, which makes flotation of pressure leaching residue more difficult. That is why in this case the hydrometallurgical treatment was chosen. At optimal parameters of chloride leach-ing found during laboratory experiments the principal components extraction was 99.5% for Pb and up to 92% for Ag.

Jan 1, 2006

By Dirk Verhulst, V. I. Lakshmanan

Why Chloride Hydrometallurgy?The most available, cheapest and best known reagent for treating ores and other raw materials for the metallurgical industry is sulfuric acid. Hydrochloric acid is second in line. What often happens is that a process is developed on the basis of sulfuric acid, and that at some point the question arises: wouldn't hydrochloric acid do this better?Considering hydrochloric acid immediately opens a very interesting field of research. To summarize a few comments from another paper presented at this symposium [1]: chlorides are far more soluble than sulfates (with a few interesting exceptions); the hydrogen ion activity is greater in chloride than in comparable sulfate solutions; higher oxidative conditions are possible; regeneration is more straightforward; more diversity is possible and better conditions for the separation of species can be found for solvent extraction and ion exchange; sulfur in the ore can be separated as elemental S; higher metal concentrations in solution and more flexibility in the chosen oxidation state means significantly lower energy costs.Also, the volatility of many chlorides at higher temperature allows further separation without the need to go to a different system. Chlorides also form molten salts with a low melting point, providing another means of separation and purification in the same chloride medium.

Jan 1, 2011

By Yavuz Ali Topkaya, Aydin Rusen

"In this study, zinc and lead recovery from zinc plant leach residue obtained from Çinkur using hydrometallurgical methods have been investigated by laboratory scale experiments. Considering more than one million tons leach residue (LR) rich in Zn (12.43%) and Pb (15.51%) in the stockyard and environmentally hazardous, it is essentially necessary to process Çinkur LR. Zinc and lead have been recovered in two main stages. As a first step, Çinkur LR was releached by using hot sulphuric acid for zinc recovery. About 72 % Zn was recovered by using 150 g/l H2SO4 at 95 oC in 2 hours with a pulp density of 200 g/l. Secondly, for lead recovery brine (NaCl) leaching tests were performed on the secondary Çinkur LR obtained after acid leaching process. In brine leaching while lead recoveries up to 95 % could be attained at a low pulp density, the maximum recovery obtained was 84.9 % at a high pulp density (200 g/l) with 300 g/l NaCl concentration in 10 minutes at 95 oC. Introduction Zinc and lead have been known and used by humans since ancient times and also they are important nonferrous metals [1]. Zinc and lead have different properties thus they are used in various application areas, ranging from automobiles to construction, from batteries to textile. Zinc and lead deposits are widely distributed in the Earth’s crust. The principal ore mineral for zinc is zinc sulfide, Sphalerite (ZnS), and lead sulphide, Galena (PbS), is the main source of lead in the world [2].Although zinc is generally produced from sulphidic ores (ZnS) or concentrates by Roast – Leach – Electrowinning (RLE) in the world, in Turkey, zinc production is based on zinc carbonate ores (ZnCO3), and at the Çinkur plant zinc was produced from zinc carbonate from its establishment to 1997 due to high reserves of zinc carbonate in that region. Çinkur is the only plant in Turkey that produces Zn from primary ore containing ZnCO3 by Waelz – Leach - Electrowinning route [3]. However, due to depletion of local high grade ores, oxidized ore concentrates were imported from Iran after 1997, until this plant was shut down. Therefore, there are two different leach residues (LR) which are Turkish LR (TLR) and Iranian LR (ILR) in Çinkur stockpiles. It has been estimated that the total amount of leach residue is more than one million tons of which the major part is Turkish leach residue (TLR)."

Jan 1, 2008

By Joon H. Jang

At a selected pH, hydrothermal oxidation of chalcopyrite was carried out under controlled F+,, at elevated pressures and temperatures (172-200°C) by balancing the rate of oxygen injection against the rate of consumption. Chalcopyrite was converted to covellite (CuS) and digenite (CU1.8S) with rejection of iron and sulfur to the solution. Covellite forms in the first stage, followed by nucleation and growth of digenite in the second stage. The effects of rapid and slow injection of stoichiometric quantities of oxygen are compared. Both the covellite and digenite form a porous layer occupying the same volume as the original chalcopyrite grain. An electrochemical kinetic model is presented to correlate the observed results.

Jan 1, 1993

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 Ryo Sasai, Takeshi Itakura, Haruki Imaizumi, Hideaki Itoh

"Emission of industrial wastewater containing harmful oxoanions is one of the serious problems on account of its toxicity and the environmental pollution, especially caused by boric, phosphinic, arsenic and antimonic species. In this study, we developed a novel treatment technique of such polluted-water by hydrothermal mineralization. The treatment is “Geomimetic” method for precipitating oxoanions in aqueous media as natural ore resources by using hydrothermal treatment with calcium salts mineralizer. The treatment made it possible not only to detoxify the polluted-water, but also to recover the calcium minerals such as Ca2B2O5·H2O, Ca5(AsO4)3(OH), etc. Concentration of each ion in treated-water was lower than that of effluent standard in Japan. Moreover, the residual concentration of each ion was independent of the initial concentration, but it depends only on the solubility of the formed mineral under hydrothermal condition. Therefore, the hydrothermal treatment could be recommended as one of the treatment techniques of polluted-water.IntroductionVarious oxoanions such as boron and arsenic oxo-anions have high toxicity against human health and the environment. They are important resources, however, for plating or advanced material manufacturing industries[1-3], from which the wastewater containing these oxoanions is generated every day. An appropriate treatment is often required for industrial wastewaters to attain national effluent standards of Japan (NESJ, B: 10 mg/dm3, As: 0.1 mg/dm3). On the other hand, there is no production of arsenic and boric resources in Japan, and they are expected to be recycled. Therefore, the establishment of a system for the removal and recycling of arsenic and boron from wastewaters is of global significance.Several methods to remove them from aqueous media have been already reported by using adsorption[4], electro-coagulation[5], membrane separation[6-8] and biological techniques[9]. However, these methods have the following problems because of their stability in water. (1) Removal yield is low, especially for tri-valent arsenite ion (AsIIIO3 3-) and borate ion. (2) The applicable concentration range is narrow. In addition, the used adsorbents or collected residues after treatments are sill hazardous wastes, so that they must be treated by a proper method. But, it is very difficult to convert them to recyclable resources at most industrial plants. These problems are caused by the difficulty to recover these oxoanions as stable solid precipitates with low solubility in water. The establishment of recycling system of these hazardous compounds will be one of the world-important issues, especially, in Japan, which is poor in natural resources. On the other hand, compounds that contain high arsenic concentrations and are insoluble in water, are often found in natural minerals, for example, as haidinglite (Ca(AsO3OH)·(H2O) or Johnbaumite (Ca5(AsO4)3(OH)). This fact suggests that nature has an ability to produce insoluble As-bearing minerals. Similar phenomena can be found in case of boron, antimony, etc."

Jan 1, 2008

By V. Yahorava

Mintek has developed a non-destructive Resin-in-Leach method for the recovery of Rare Earth Elements (REE) from phosphogypsum (PG) waste dumps. However, PG from different sources was found to be highly variable in terms of REE recovery and physical properties. Development of a pre-treatment process was initiated to improve the robustness of the current REE recovery process in order to render it effective for any type of PG. Extensive research into the mineralogy of REE associations with PG revealed that the majority of REE are trapped inside phosphogypsum clusters which inhibits their recovery. Hydrothermal treatment of PG-containing slurry was found to result in re-crystallisation of gypsum with the release of REE phases encapsulated in it. This process was tested on various PG samples and subsequent REE recoveries improved from 5 to 80%. This approach carries a large potential for unlocking value associated with gypsum dumps worldwide.

By Yan Zeng

Lithium metal silicates (Li2MSiO4, M = Fe or Mn) composed of abundant and non-toxic elements are important cathode materials for Li-ion batteries (LIB). In contrast to solid-state or sol-gel methods, hydrothermal synthesis conducted in pressure reactors is a favorable processing route as it provides the potential for scalable production and is environmentally benign. However, the key is to control the precipitation reaction to obtain powders with desired properties to meet battery specifications. Through a systematic study, we have found that Li2MSiO4 with tunable size from 300 nm to 1.5 μm can be produced by adjusting precursor concentrations, temperature, and reaction time. Under optimum conditions, high purity Li2MSiO4 with minimum defects were successfully produced and examined as an LIB cathode. The use of complexing agents promoted the formation of unique hollow particles via the self-assembling of elongated crystals. A four-step formation mechanism is proposed based on extensive characterizations with XRD, HR-TEM, SEM, and Mössbauer spectroscopy.

By Jose F. Hevia

This study is part of a broader project on the hydrothermal conversion of copper concentrates to metallic copper by solid state reactions in which the copper remains localized in the solid phases. The kinetics of the solid/solid hydrothermal hydrogen reduction of tenorite (CuO) and cuprite (Cu,O) to metallic copper are presented. After an induction period, the process is governed initially by a nucleation step followed by rapid solid state reduction. Nucleation promoter agents decrease the induction period and control the particle morphology. Separate nucleation and reduction rate processes have been identified. Following nucleation, reduction follows a shrinking core process.

Jan 1, 1994

By Chang Wei, Zhigan Deng, Jiqiang Liao, Minting Li, Hongsheng Xu, Yan Song, Cunxiong Li, Xingbin Li

"Abstract: Direct ?otation of oxidized zinc-lead ore is characterized by recovery of zinc and lead only around 55% and 50%, respectively. Mineralogical analysis shows that the sample used in the present study is a carbonate hosted zinc-lead ore, with a zinc and lead carbonate content that accounts for 80.14% and 75.63% of the total minerals, respectively. The carbonate hosted zinc-lead ore was hydrothermally sulfidized with elemental sufur and the experimental data indicated that under the conditions employed up to 75% zinc and 82% lead sulfidation extent were achieved. As a result of pre-sulfidation followed by flotation, the recoveries of zinc and lead into flotation concentrate were over 90%. A flotation concentrate was obtained with 52% Zn and 37% Pb from the materials which was treated by sulfidation.IntroductionSulfide ores are the primary source of zinc and lead, and they are becoming depleted; thus, metallurgical investigators are interested in using abundant oxidized zinc-lead ore reserves. The high-grade zinc-lead oxidized ore, which normally has a zinc content higher than 15%, can be disposed of by acid leaching and electrolysis. However, the low-grade ore, which has a zinc content lower than 10%, is difficult to smelt with pyrometallurgy and hydrometallurgy, and the processes are very complicated and expensive in terms of production flow and energy consumption. Therefore, making the low-grade oxidized zinc-lead ore more beneficial has become more important in recent years. Flotation is the most common process, and the primary method of recovering zinc and lead from sulfide or oxide minerals. It is well known that there is a difference between sulfurized and oxidized minerals regarding their separation by flotation. Flotation of zinc and lead oxidized minerals is extremely complex because of the similarities in the physicochemical and surface chemistry of the constituent minerals. There are no known direct-acting collectors capable of producing single metal concentrates [1-3]."

Jan 1, 2012

By Yang Hai-long, FAN Gang, LI Cun-xiong, WEI Chang, LI Min-ting, LI Xing-bin, DENG Zhi-gan

Hydrothermal sulfidation of pure cerussite with elemental sulfur has been reported in the present paper. The variables considered in the study were temperature, time, particle size and elemental sulfur fraction in the reacting mixture. Temperature was the most important factor at temperatures above 180 , PbS and PbSO4 were the only stable reaction products in the sulfidation of cerussite. The experimental data indicated that under the hydrothermal conditions with a particle size of -74+58 μm and sulfur fraction in reacting mixture of 15% at 200 °C for 120 min, and 92% of lead sulfidation rate was achieved.

Jan 1, 2016

By K. P. V. Lei

The U.S. Bureau of Mines investigated a hydrothermal sulfidation procedure to recover lead and silver from plumbojarosite. The plumbojarosite, generated during pressure-oxidative leaching of zinc concentrate in a commercial operation, contained, in percent, 25.4 pb, 18.8 Fe, 1.4 Zn, 29.5 SO,2-, 3.2 s?, 13.4 total sulfur, and 7.4 oz/ton Ag. The sulfidation was conducted in an autoclave and converted the plumbojarosite to amorphous iron oxide and liberated the lead and silver as sulfides. The best operating conditions were using 50 9 of plumbojarosite and 7 pct s? (2.04 9 S? added) in 500 mL of 2.0 mol/L NH3, 150? C, and 1 h. The sulfidation product contained, in percent, 37 Pb, 28 Fe, 6 S2-, 2 SO,2-, and 11.2 oz/st Ag. Ferric chloride leaching extracted 98 pct Pb and 97 pct Ag from the sulfidation product.

Jan 1, 1990

By Norihiro Murayarna

Hydrothermal synthesis of K type zeolite was carried out by using coal fly ash as a raw material and KOH as an alkali source. The change in various physical properties of the obtained zeolite, such as the kind of zeolite crystal, cation exchange capacity, surface structure of zeolite and particle size distribution were investigated through the overall reaction of zeolitization. The reaction mechanism of K type zeolite from coal fly ash was investigated from these results in this study

Jan 1, 2002

By Guo Jun

In this study, BaTiO3 ultrafine particles surface-modified with stearic acid were synthesized by the hydrothermal method in a system of BaCl2-TiCl4-NaOH. The effects of NaOH/TiCl4 molar ratio, Ba/Ti ratio and time on structure and morphology of BaTiO3 ultrafine particles were investigated experimentally. The formation mechanism of different crystalline BaTiO3 particles was discussed, and it is considered that in a hydrothermal system, the main factors determining BaTiO3 crystalline are H+ replacement of Ba2+ causing H+ deficiency and anatase growth units involving in crystal growth, which clogs the axial channel for Ba2+ transference. By means of increasing the alkalinity of system and barium content, H+ deficiency and involvement of anatase growth units in crystal growth could be effectively controlled. The results show that when molar ratio of NaOH to TiCl4 is 9 and ratio of Ba to Ti 1.5, and time 8 hours, high purity tetragonal BaTiO3 ultrafine particles with a narrow grain-size distribution and nonpolar surface are obtained at 240oC. The particles have excellent flowability, which is ascribed that the surface polarity of barium titanium powder modified with stearic acid is changed and the interaction between the particles is weakened.

Jan 1, 2006

By Mojtaba Ahmadiantehrani

A previous study showed that up to 80% gold extraction could be obtained with 160 lbs/ton hypochlorite consumption at ambient temperature from a low grade Carlin-type carbonaceous ore. Crushing the ore to a finer size and agglomerating with cement decreases hypochlorite consumption by 60%; while, agglomeration and curing the cement-ore mixture with hypochlorite solution has no significant effect on total gold extraction. The high hypochlorite consumption is due to oxygen depletion as the solution percolates through the column, i.e., oxidation of gangue materials. These side reactions are reduced at sub-ambient temperatures resulting in a substantial further decrease in hypochlorite consumption. The optimum temperature range and additional reduction of hypochlorite consumption by introducing the reagent into the column at different elevations will be discussed.

Jan 1, 1992

By R. W. Bartlett

The extensive central Idaho black sand placer deposits are a potential source of rare earth elements, particularly the heavy rare earth elements that are not prevalent in commercial bastnasite deposits. These placers derive from the Idaho batholith. The geology, occurrence, and extent of these deposits are reviewed and the diverse mineral assemblages and complex mineral chemical compositions of these sands are described. Niobium, yttrium and thorium are also present in significant concentrations. The results of prior mining practice, including concentration and separation of the heavy minerals are reviewed. Technical approaches to extraction of rare earths from Idaho black sand concentrates are discussed.

Jan 1, 1992

By Jian Li

Corrosion resistance of materials is highly dependent on the microstructure of the specific material. Apart from general corrosion rate measurement using techniques like linear polarization and A.C. impedance, microstructural investigations are frequently needed to identify the root cause of corrosion. Advanced techniques, including scanning electron microscopy (SEM) and transmission electron microscopy (TEM), have been well integrated into routine characterization studies. Other microscopy techniques, including electron probe micro-analyzer (EPMA), Auger, X-ray photon spectroscopy (XPS) and secondary ion mass spectroscopy (SIMS), can provide detailed chemistry information on corrosion products. In recent years, focused-ion beam (FIB) microscopes have evolved into an important microstructural characterization instrument. In this study, corrosion of rebar encased in concrete was studied in great detail using advanced microscopy techniques. Corrosion product on the rebar surface was identified as ferrous oxide with relatively large crystal size. The morphology of this passive layer was thoroughly analyzed, and its formation mechanism is proposed.

Jan 1, 2009

By Peter M. DiGiacomo

In situ leaching technology requires information about how injected fluids flow in the rock in relation to the localization of the valuable minerals to be leached. In oxidative leaching of sulfide copper ores, flow channels can be determined by the observation of residual iron oxides. In contrast oxide copper ores do not leave a detectable residue after leaching. Method is developed that allows a selective labeling of the leach residue with fluorescent compounds. The fluorescent zones can be detected in corings after the leaching operation.

Jan 1, 1981