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By Toshiaki Nakai, Kunihiko Takeda, Kimio Imaizumi, Hiroaki Shirasaka

"The new type of nano-porous silica particle was considered to be constructed by the spinodal decomposition-type process which was found to have narrower pores than those of conventional porous silica prepared from boron silicate or ""Shirasu"" balloon. Nano-porous silica particles were fabricated by the calcination of silica gel mixed with well-dispersed complex salts composed of phosphorous and molybdenum compounds. Both silica and inorganic salts were not perfectly dissolved in the suspension solution. After removing of the water, the silica-inorganic salts complex was volatized and successively calcinated at a temperature ranging from 650 °C to 800 °C. Then, the inorganic salts were removed by dissolving in hot water. Other inorganic salts such as potassium halides were also found to be effective as a pore-size controller.IntroductionControl of structure has an important role in the field of industry as well as in the separation and purification technology for metals and organic syntheses. Many studies on the control of material structures have been reported regarding porous materials with pores ranging from nanometer to micrometer scale. 1 ) One example is zeolite as a naturally yielded porous inorganic material. Various types of synthetic zeolites have been studied as ""molecular sieve"" materials with ordinary pore-size of less than one nanometer. In 1992, crystalline meso-porous material with a large surface area named MCM-41 was synthesized through the use of template synthesis. 2) In direct relation to our study, amorphous borate glass having 4 to 100 nm of fine pores known as Corning glass 3l or SiO2-Al2OrB2O 3-CaO porous glass having large pore dispersity ranging from 4 to 10,000 nm have been reported. 4 ) S) 6 ) Some examples of several reported studies are as follows: phase-separated porous glass consisting of B2OrAl2O3-ZrO2-RO-R2O complex oxide 7 ) glass with finer pore induced from hydrolysis of silane alkoxide, porous material attained by condensation polymerization through the use of sol-gel process 8), alumina meso-porous material 9 ) 10), silica-zirconia material 11), carbon porous material 12), etc.."

Jan 1, 2000

By A. M. Alfantazi, M. Boissoneault, D. B. Dreisinger, J. Synnott

Acid mist generation is a major concern in zinc, copper and nickel electrowinning industries and there is a strong environmental drive to control its emission into the work environment. Foaming reagents are typically added to the electrolyte to alleviate this problem. In zinc electrowinning, Licorice and Saponin are examples of foaming reagents used for this purpose. In order for the foaming reagent to be effective, its foaming behavior must be determined. In this work, a test procedure was developed to study the foaming characteristics of various surfactants for use as foaming agents to control acid mist in aqueous metal electrowinning. This new test was termed as "mini-flotation test" and it was used to study the foaming behavior of a large number of reagents in an industrial zinc sulfate electrolyte under simulated zinc electrowinning conditions (gas sparging). In addition, the influence of important process parameters such as current density, electrolyte temperature, reagent addition level and sulfuric acid concentration on the foaming characteristics of the electrolyte for each surfactant were investigated. The results of this study have identified the most important factors that influence foam formation, growth and stability. This method could be used as a process control for reagent addition in the cellhouse by generating a calibration curve for the optimum electrolyte conditions.

Jan 1, 1997

By Pertti Koukkari, Nagendra Tripathi, Karri Penttilä, Justin Salminen

A computational fluid dynamic model for a novel flash ironmaking process based on the direct gaseous reduction of iron oxide concentrates is presented. The model solves the threedimensional governing equations including both gas-phase and gas-solid reaction kinetics. The turbulence-chemistry interaction in the gas-phase is modeled by the eddy dissipation concept incorporating chemical kinetics. The particle cloud model is used to track the particle phase in a Lagrangian framework. A nucleation and growth kinetics rate expression is adopted to calculate the reduction rate of magnetite concentrate particles. Benchmark experiments reported in the literature for a nonreacting swirling gas jet and a nonpremixed hydrogen jet flame were simulated for validation. The model predictions showed good agreement with measurements in terms of gas velocity, gas temperature and species concentrations. The relevance of the computational model for the analysis of a bench reactor operation and the design of an industrialpilot plant is discussed.

Jan 1, 2014

A simulation of a capper concentrate smelter was built with a capacity of 450,000 tons per year. The system's components to simulate were three : a Reverbetory furnace, a Wiente ' s modified converter ( TMC ) and two cranes. The system was classified as dynamic, stochastic and discrete. In the simulation language choice it was concluded that the most advantageous one was GPSS/H. The model verification was done through the interactive Debugger that the language has and the statistical validation was done through the result variables of sane activities, that as a whole characterize the system (charged matte and charged concentrate to the TMC, skimming white metal and skimning slag). The validation was done comparing the simulation results of these variables with the ones obtained for those variables in a specific month in the smelter. The comparison consisted in a difference of means test and in all cases the equality was accepted with a 95% of confidence. The animation tool was PROOF, a general purpose animator, that is used after processing the simulation.

Jan 1, 1994

By Batric Pesic

The interactions of mineral-pyrite with T. ferrooxidans were studied by using a cyclic voltametry technique. The interactions with bacteria were examined during the entire growth stage of bacteria (fermentation), The pyrite ?surface invariably drastically changed ' its. properties at the second day of fermentation. Beyond two .. days of fermentation, the cyclic voltamograms were insensitive to convective diffusion produced by stirring. The product layer was examined by SEM,. X-ray diffraction and chemical analysis. The SEM study revealed that bacteria populated the pyrite surface at an extremely high density levels. The high density of bacteria, and the solid reaction products formed on the pyrite surface created conditions for pore diffusion which explained why the CVs became .insensitive to convective diffusion in solution (stirring). The x-r:ay diffraction study confirmed jarosite as a product layer. A mechanism of T. ferrooxidans cells serving as nucleation sites for jiarosite formation is proposed.

Jan 1, 1991

By S. Sugiyama, M. Kiuchi

"New metal working processes, such as the mashy-state mixing, mashy-state forging, mashy-state rolling and mashy-state extrusion are developed and applied to manufacture the so-called particle reinforced metals, fiber reinforced metals, particle reinforced cladding metals and so forth. These metal-ceramics composites are made of metal sheets, metal powders, ceramics particles and ceramics fibers. The mashy-state processes are also used to work those composites into bars, wires, tubes, plates, sheets, machine parts and other products. The working conditions necessary to manufacture sound composite products are clarified and the mechanical properties of the products are investigated. Through the investigation, it becomes clear that the mashy-state processes are useful and effective to manufacture metal-ceramics composites. It is al so known that these processes may be applied in various ways to development of new metal matrix compounds. IntroductionThe so-called metal-ceramics composites and processes to manufacture them are now being widely investigated in order to comply with increasing demands for new materials with novel and excellent mechanical properties and functions. The metal-ceramics composites are expected to have superior characteristics with respect to the elastic modulus, hardness, anti-wear resistance, high temperature strength and other mechanical properties to those of conventional metallic materials.The present authors ha v e been investigating into new metal working processes which are based upon the characteristics of metals and their alloys in the mashy-state. In the mashy-state, the metal (or alloy) includes both of the solid and liquid components. According to the fact that the partial melting takes place and the liquid component usually exists at grain boundaries, the metal in the mashy-state has quite different mechanical properties from those of the metal in the solid-state. Because of that the bonding force among grains is very weak due to the partial melting occurred at grain boundaries, the mashy metal has distinctively low flow-stress and high deformability. The mashy metal splits into grains or particles and sticks to others very easily. It is so soft as to be stirred up just like a lump of sherbet, but it is sufficiently viscous to be mixed up with other materials, such as ceramics particles and ceramics short-cut fibers."

Jan 1, 1988

By Vadim J. Jabotinski

Electron beam processing is potentially very attractive for the high temperature treatment of hazardous materials. The very high power efficiency of the electron beam energy source (80- 90% of the power from the electric power line is converted to useable energy) is one of the positive features of this technique. This paper will consider advanced electron beam concepts for solid, liquid, and gaseous waste treatment such as stabilization of radioactive solid and liquid hazardous streams. Fundamental aspects and applications including an analysis of the economic potential of electron beam processing of waste treatment will be presented.

Jan 1, 2000

By Bohumir Jelinek, Sergio Felicelli, Mohsen Eshraghi

"We present a parallel lattice Boltzmann - cellular automaton model of the two-dimensional dendritic growth during solidification of binary alloys. The model incorporates effects of solute and energy transport under melt convection. The parallel performance of the algorithm is assessed. A loss in the parallel efficiency is observed when multiple computational cores per processor are utilized. Excellent strong scaling up to thousands of computing cores is obtained across the nodes of a computer cluster, along with the near-perfect weak scaling up to forty thousand cores. The presented solidification model shows a good scalability up to centimeter size domains, including millions of dendrites.IntroductionLattice Boltzmann method (LBM) is an attractive numerical technique for solving fluid dynamics problems. Its advantages are simple formulation and locality, with locality facilitating parallel implementation. In the present model, interface kinetic is driven by the difference between local actual and local equilibrium liquid composition [1]. The cellular automaton (CA) technique is deployed to track the solid-liquid interface [2]. A serial version of the present LBM-CA model with a small number of dendrites was validated against theoretical and experimental results in the previous publications [3, 4]. In this work, it is the first time that simulations with millions of dendrites were performed, something not possible with the computationally much more costly phasefield method [5].This research effort examines a technique for simulations of millions of dendrites in centimeter size domains, including thermal, convection, and solute redistribution effects. Nearly ideal scaling properties of the model are demonstrated. This extensively large landmark was achieved because of• the CA technique being two orders of magnitude faster than alternative, phase-field methods [5]• highly parallelizable LBM method, convenient for simulations of flow within complex and time dependent boundaries• availability of the powerful NSF Extreme Science and Engineering Discovery Environment (XSEDE) supercomputing resources"

Jan 1, 2013

By Amy Nelson

In the electrolytic production of zinc, cobalt is removed from the zinc electrolyte by cementation with zinc dust prior to electrowinning. Although the thermodynamics for this reaction are favourable, kinetic barriers to cobalt reduction render the method almost useless in practice unless activators such as copper and antimony or arsenic are added. There is a large body of work studying the effect of these additives, yet the mechanism by which they act is still poorly understood. Even when the target conditions are met, zinc dust consumption is excessively high: satisfactory operation requires up to 300 times the stoichiometric amount of zinc dust. The objective of this work is three-fold: (1) to examine the effects of activators and elucidate the characteristics that make a good activator; (2) to identify new additives that could lead to a more efficient purification process; and (3) to test the new additives with synthetic and real electrolyte solutions. The present paper gives a status report on this project.

Jan 1, 1998

By E. Anelli

Based on experimental continuous cooling transformation (CCT) diagrams, an artificial neural network has been trained to predict the amount of microsturctural constituents and hardness resulting from and controlled cooling at rates from 150 to 0.015 K/s. It can be applied to quenching and normalizing processes of low-alloy steels with 0.05-0.30 C% and 0.4-2.0% Mn -with possible microalloying additions. Examples of the good predictive capabilities about 15 Vickers standard deviation for hardness and a few percent for volume fraction of phases) are reported' Keywords: Austenite decomposition, low. And medium-carbon steels, artificial neural networks

Jan 1, 2003

By K. E. Gonsalves, G. M. Chow

"Nanostructured powders (particle diameter of 1 - 100 nm) have uses in electronic, magnetic, structural, thermal applications as well as advanced processing of materials. Among many methods of making nanostructured powders, chemical routes offer many attractive features such as feasibility of cost-effective bulk quantity production, design of chemistry at the molecular scale, and chemical homogeneity of the powders. In this talk, two systems of chemically synthesized nanocomposite powders are presented, namely, granular magnetic materials of Fe-Cu and Co-Cu, and thermal-structural materials of AIN-BN. Synthesis and processing, characterization and properties of these materials are discussed.IntroductionNanostructured powders (particle diameter of 1 - 100 nm) are attractive materials because of many useful properties (e.g. catalytic, optical, magnetic etc.) and processing advantages (e.g. lower sintering temperature) [1]. There are many methods of making nanostructured powders, for example, physical and chemical vapor deposition, mechanical attrition, and solution chemistry [1, 2]. A common method of making composite powders involves the grinding, mixing and blending of constituents powders, but it has the limitation of inhomogeneous mixing. Chemical routes have many useful features. Using solution chemistry, precursors can be molecularly tailored and homogeneously mixed at the molecular level. The chemical approach may result in better properties of the final product. Compared to vapor-phase fabrication techniques, chemical routes are more cost-effective in producing large quantity of material. In addition, control of particle size, size distribution and stabilization of the nanoscale particles against agglomeration can be more effectively manipulated via solution chemistry.In this paper, we present an overview of some of our work in nanocomposite powders prepared by solution chemistry. Metallic systems of FeCu and Co-Cu, and ceramic system of AIN-BN are discussed. The powders were characterized using x-ray diffraction (XRD) , scanning electron microscopy (SEM), conventional and high resolution transmission electron microscopy (TEM, HRTEM), vibrating sample magnetometry (VSM), inductively coupled plasmaatomic emission spectroscopy (ICP-AES)."

Jan 1, 1994

By Jiang Fan, Wang Haigang

"The three-dimensional complex multiphase turbulent flow in U-beam separators was simulated using the Reynolds stress equation models (RSM). To account for the effect of the stochastic characteristic of the instantaneous gas velocity on the particles, the improved Lagrangian stochastic model based on the Reynolds stress model for gas phase was adopted, which attributed to the successful prediction of the turbulence anisotropy and particle crossing trajectories effects. The interaction between the particles was also considered using the HardSphere model. To treat the particle-wall collision, the influence of the roughness of the wall on the motion of the solid particles was taken into consideration by imposing random collision angles. The result from this study not only shows the dynamic characteristics of the multiphase flow- in the separators, but also gives the relationship among the efficiency, structure and pressure losses of the separator.IntroductionCirculating fluidized bed (CFB) combustion is one of the most promising clean coal techniques. A main feature of CFB boilers is the un-delayed recycle of solid, coal and sorbant particulate, in an external loop. Separator, which is required to separate the solid particle from the flue-gas leaving the reactor of CFB, plays an importance role in the external solids recycle loop. It affects the combustion of CFB system greatly. Presently cyclone is the most commonly used as separators for CFB system and other chemical industrial processes. It provides high level of separation for CFB system for fine particles. However it suffers from some inherent disadvantages. It's volume and size is huge. Moreover, it is difficult to design and install when the CFB workload rises. The application of U-beam separators instead of hot cyclone separators in CFB boilers has many advantages. Publications indicate proposals or successful use of Ubeam separators in Swedenr11, USA 21, Russia r3land China [4]• But it is not possible to find results in the literature of detailed investigations of this new. type of separators or recommendations on the choice and calculation of an optimal design. For this reason, numerical simulation for the three-dimensional gas-particle two-phase flows with several rows of vertical U-beam elements, local in the chess order and blocking a way of outgoing from a CFB boilers dusted gases was carried out in this study."

Jan 1, 2004

By Ehsan Vahidi, Fereshteh Rashchi, Amirhossein Shahnazi

"The pig iron from steel manufacturing plants contains a high concentration of vanadium-bearing materials smelted with iron ore. During the oxidation process of the molten pig iron with oxygen lances, vanadium transfers to the slag. In this research, recovery of vanadium from LD (Linz-Donawitz) converter slag of steelmaking plant was investigated. The leaching residue was characterized by XRD and XRF techniques. The maximum vanadium recovery was achieved at optimum leaching conditions of 70 °C, S/L: 1/15, sodium hydroxide concentration: 3 M and leaching time: 150 minutes. The dissolution rate increased with rising sodium hydroxide concentration and temperature and decreasing particle size. The experimental data are treated graphically to explain the kinetics of the vanadium recovery process using shrinking core model (SCM). As a result, the controlling regimes in the SCM were analyzed separately using liquid film diffusion control, solid product diffusion control, and reaction control mechanisms.IntroductionVanadium is commercially important as a constituent of several alloys and catalysts. Nowadays, vanadium is mostly recovered as a by-product from secondary sources or from industrial waste streams such as titaniferrous magnetite, fly ash, spent catalysts, and petroleum coke. Steelmaking operations are specifically concerned by this problem due to the production of a huge quantity of by-products [1]. These by-products, including LD converter slag, sludge, fly ash, spent catalyst, ash, and alloyed scrap, contain a notable amount of heavy metals which may cause environmental problems. Solvent extraction is one of the techniques being increasingly used for the recovery of vanadium [2]. Apart from vanadium ore, secondary resources such as titanmagnetite, ilmenite and slag from the ferrous industry are a major source of supply. The pig iron from steel manufacturing contains a majority of vanadium-bearing materials smelted with iron ore. In a heat resistant shaking ladle the molten pig iron is oxidized with oxygen lances, causing the vanadium to be transferred to the slag. Normally, the vanadium in LD converter steel slag (coming from Linz-Donawitz steelmaking process) is ca. 5% as vanadium pentoxide (V2O5). This slag is the world's principal raw material for vanadium production [3, 4]. Moskalyk and Alfantazi [4] reported that a roast-leach process is used in South Africa for the production of vanadium oxides from magnetite ores while some of the slag was converted to ferrovanadium. A portion of the slag was exported to Europe for the production of vanadium oxide. The researchers mentioned that alkaline roasting was the main process at that time employed to extract vanadium pentoxide from vanadium slags."

Jan 1, 2012

By J. W. A. Morris

To investigate the use of centrifugal fields in fused salt electrowinning cells, a high temperature rig has been designed, constructed and commissioned. Initially, the cell has been applied to the fused salt electrowinning of zinc. Current efficiencies of 93% have been obtained for inter electrode gaps as small as 8mm for 70mm diameter electrodes rotating at 100rpm. The construction of a semi-rigorous physical model has shown the potential exists to extend the use of centrifugal fields to the electrowinning of light metals.

Jan 1, 1994

By Gökhan Demirci, Ishak Karakaya

"Energy consumption in electrolytic magnesium cells is well above the theoretical values. However, the mechanism of the back reaction, the main cause of the current losses, has not been fully understood yet. Magnesium dissolution into the melt is generally regarded as the limiting step for the back reaction. Accordingly, present cell designs are made with priority given to fast magnesium removal from the cell. However, experimental data and modeling results in this study indicate that the limiting step for the back reaction between magnesium and chlorine is the chlorine dissolution into the electrolyte when physical contact between electrolysis products was eliminated. Effects of chlorine bubbles on the current efficiency and the cell potential were investigated. Results show that the extent of back reaction is proportional to the chlorine surface area in contact with the electrolyte per unit time, and the cell potential increases with the amount of chlorine bubbles inside the electrolyte.1. IntroductionMagnesium is less dense than the electrolyte in electrolytic magnesium production. Therefore, both electrode products, magnesium and the chlorine gas, move upwards inside the molten salt electrolyte during electrolysis. The upward motion of electrode products promotes the most important current loss mechanism, the ""back reaction"". Separation of the highly reactive species; liquid magnesium and the chlorine gas in the cell, to prevent their recombination is one of the main concerns in cell designs. The employment of large inter-electrode distance or a separation wall in early cell designs; decreased the extent of recombination, but increased the cell voltage and energy consumption. Recent cell designs, on the other hand, make use of lifting action of chlorine gas [1,2] by utilizing smaller inter electrode distances to separate the magnesium and chlorine gas faster. Although energy consumption was reduced, but more physical interactions between electrode products make electrolytic magnesium cells still highly inefficient when energy consumptions are compared with the theoretical values. Today, the most efficient industrial cells utilizing high purity feed operate at 10.5-11.5 kWh kg-1 Mg [3-5] and it is considerably higher than the theoretically attainable value of about 6.0 kWh kg-1 [6]. This large gap demonstrates the necessity of more research on physics and chemistry of magnesium cell electrolysis."

Jan 1, 2011

By S. Saptharishi

Selenium, which is a 6A group element of the periodic table, constitutes about 7x10-5 % of the earth?s crust. Even though selenium is a dispersed element with respect to its commercial exploitation, it is capable of forming number of minerals and nearly forty selenium minerals have been identified, out of which the copper ores are the richest sources of selenium. Electronics industries and glass industries are the major consumers of selenium, while pharma grade selenium used as micronutrient for humans and animals. Various methods have been developed to recover selenium as a by-product from copper anode slime during copper refining. Selenium being amphoteric in nature, it is soluble in both acid and alkali. While acid roast process is widely used, considerable work has been carried out in Russia for recovering selenium through alkali route. This paper enlightens the process developed at Central Research and Development Laboratory, for recovering selenium from decopperised slime through alkali pressure leaching. The decopperised slime is pressure leached with alkali under oxidizing conditions by which almost all the selenium present is converted to alkali selenate, which is easily separable from the rest of the decopperised slime. The solution so obtained is neutralized, during which, most of the impurities are precipitated out. Then selenium is precipitated in its elemental form upon purging sulphur-di-oxide under warm acidic medium. The purity of the selenium obtained by this process is higher than that of the selenium from acid roast process. Moreover selenium can be crystallized as sodium selenate and it can be marketed. The acidic content of the effluent is recovered and it is recycled back to the process. The sodium content of the effluent is converted into high purity sodium sulphate, which is marketable. The hazardous waste containing arsenic is precipitated as its sulphide and can be disposed off as landfill.

Jan 1, 2006

By Yang Tian-zu

The separation of precious metals from base metals containing in gold-antimony alloys by selective chlorination leaching under controlling potential was studied in this work. The effects of the consumption of hydrogen peroxide, the concentration of hydrochloric acid, the concentration of sulfuric acid, leaching temperature, leaching time and the liquid-solid ratio in hydrochloric acid system on the leaching efficiencies of the base metals have been investigated. The optimal leaching conditions of the gold-antimony alloys are as follows: hydrochloric acid concentration 4.0mol?L-1, sulfuric acid concentration 1.2mol?L-1, liquid-solid ratio L:S=7.5:1, the leaching temperature 80 0C, leaching time 2h, and the oxidation potential of the leaching system 400±20mV( vs SCE).The leaching efficiencies of copper, nickel and antimony are more than 99% and the gold leaching efficiency is about 0.042% under the above leaching conditions. The base metals containing in the gold-antimony alloy are separated from the precious metals thoroughly.

Jan 1, 2006

By W. K. Tolley

The Bureau of Mines is investigating hydrometallurgical processing techniques to recycle metals from semiconductors and other advanced materials. Cadmium and tellurium were recovered from CdTe scrap produced in the manufacture of infrared optic devices. Sulfation, ferric chloride leaching, and oxygen-pressure leaching have been tested. Cadmium dissolution was achieved using oxygen-pressure leaching in dilute sulfuric acid. However, no satisfactory scheme for dissolution of the higher valued tellurium has been devised. Leaching the ground CdTe for 75 min at 110°C in 1.1M H2S0, under 120 psig 0, yielded 99.5% Cd extraction. Tellurium remained in the leach residue as TeO, and elemental tellurium; residual cadmium was less than 0.5%. The cadmium in the leach liquor was purified of coextracted metals such as gallium and iron by adjusting the pH. The cadmium was recovered as cadmium sulfate crystals by evaporating the solution. Recovery of by product metals, notably gallium, is possible.

Jan 1, 1991

By Kouji Mimura, Tamas Kekesi, Yongfu Zhu, Masahito Uchikoshi, Minoru Isshiki

"The formation and anion exchange sorption of chloro complex ions can offer a great potential to be utilized for the separation and purification of metals in aqueous solutions. Available stability data were primarily used to estimate the predominance of chloro complex species, indicating the feasibility of such separations. Anion-exchange sorption functions, describing the equilibrium distribution of a number of important elements have been determined by the batch equilibrating method in the practical HC1 concentration range. Various oxidation states were stabilized by the addition of appropriate agents. Tendencies in oxidation, complex formation and anion exchange sorption were confirmed by spectrophotometric investigations. Based on the fundamental results, anion exchange processes have been developed for the purification of iron, cobalt, copper and zinc. The efficiency of separation was assessed and the procedure optimized by the analysis of experimental elution curves. Results have demonstrated that by properly controlling the oxidation states and HC1 concentrations, practically all the impurities can be eliminated. Computer programs have been developed to estimate complex formation and redox equilibria, to screen and correct analytical data, to determine distribution coefficients and to evaluate efficiencies of separation.IntroductionBase transition metals have long been used as the staple materials in various fields of industry. In general, there has been an increasing tendency in purity requirements but recent advances have created a rapidly increasing demand for ultra-high purity metals. To give a few examples, ultra high purity copper can be used as bonding wire and interconnection in integrated circuits, or as material for superconductor stabilizing, high-field magnets, beside its use in cryogenics and ultra high vacuum technology [1]. Iron holds promises as a constituent element in the ß-FeSi2 material to be applied in new opto-electronic devices [2] and it is currently used, together with chromium and manganese, in the production of special magneto-optical materials for digital recording. The use of ultra high purity manganese and chromium in semiconductor technology is evolving. Although not considered a transition metal, zinc is also treated here because of the major significance in compound ZnSe semiconductors [3], and the possibility to purify it by the anion exchange method."

Jan 1, 2000

By Bruce W. Wessels

"Metal-organic chemical vapor deposition has been shown to be a highly versatile technique for the synthesis of complex oxides. High dielectric constant oxide thin films of SrTiO3, BaTiO3, Ba1-xSrxTiO3 and SrxBa1-xNb2O6 can be be be deposited at 800 ºC with this technique. The fluorine substituted B-diketonate precursors have been shown to be well-suited for the deposition of high quality, epitaxial thin films of these materials.IntroductionThere has been a resurgence of interest in thin film ferroelectric oxides as a result of the development of techniques to deposit high quality material. Both physical and chemical vapor deposition techniques have been realized. Of the chemical vapor deposition techniques, metal-organic chemical vapor deposition (MOCVD) has received the most interest for the deposition of ferroelectric oxide thin films. This results, in part, from the availability of a number of volatile metal-organic precursors.(l) Moreover, MOCVD offers the advantages of high growth rates, uniform coverage over large areas, conformability, abrupt interfaces and excellent epitaxial crystallinity. Of the metalorganic precursors, the B-diketonate complexes have played an important role especially in the deposition of ferroelectric oxides containing alkaline-earth metals such as BaTi03 and Ba1•XSrxTi03. For example, barium tetramethylheptanedionate Ba(thd)2 has been used in the preparation of BaTi03 by MOCVD.(2) These compounds, however, are not without their problems. Ba(dpm)2 has a relatively low volatility; and as a consequence, temperatures in excess of 180·C are required for volatilization. This leads to the necessity of a complex precursor delivery system to insure that the precursor does not condense before the reaction zone. Moreover, the Ba precursor tends to oligomerize leading to a decrease in vapor pressure as well as a problem with reproducibility. To counter these problems, novel liquid source and solid source precursor delivery systems have been developed. (3)(4)"

Jan 1, 1994