Search Documents

By Hiroshi Maeta, Takao Kino, Hirota Osono, Kikuo Matsusaka, Azusa Shida

"Prior to refine an ultra-high purity material, it is necessary to estimate the surface cleanness of a base material. In this report, the cleaning method of a surface for refining of an ultra-high purity aluminum has been studied. Aluminum sample of 99.999% purity was p9lished mechanically and electrically and washed with various solvents. Surface composition and a depth profile near the surface were examined. Based on the experimental results, surface structure of an ultra-high purity aluminum was discussed.IntroductionRecently, studies on high purity metals have become of interest, and we have reported .various properties of an ultra- high purity aluminum1- 2)In order to purify a metal, it is necessary to clean a work area and to make vacuous as possible. So, we are studying the purification of aluminum by an ultra-high vacuum refining system and a zone refining system set up in a clean room with cleanliness class of 1000.Now, in order to avoid a mixing of impurities into the refining metal, a surface cleanness of a base metal is very important factor. The purity of the base aluminum used our work is 99.999%, but the surface state of the base aluminum is not clear. Aims in this work .are to investigate the surface state and to obtain the cleaning method of the base aluminum.Experimental procedureSamples used in this work were 99.9% (3N), 99.99%(4N) and 99.999% (SN) aluminum produced industrially and 99.9999% (6N) aluminum purified by us."

Jan 1, 2000

By Yan Fu, Chuanlin Fan, Xiujing Zhai, Yongfeng Chang, Binchuan Li

"The mechanism of the selective chlorination of nickel and cobalt in reduced limonitic laterite was investigated. Reduced ores were obtained from the reduction roasting of a limonitic nickel laterite. The thermal decomposition of related chlorides and the selective chlorination of the reduced ore were carefully studied using Differential Thermal analysis - Thermogravimetry (DTA-TG), X-Ray Diffraction and chemical leaching methods. In the temperature range of 300 - 500 °C, aluminum chloride hexahydrate was chosen as chloride agent. During the selective chlorination, reduced ore was partly chlorinated by hydrogen chloride generated from the thermal decomposition of chloride agent. Then the oxydrolysis of ferrous chloride re-generated hydrogen chloride was used to further the chlorination. Finally, iron was mostly rejected as hematite, while nickel and cobalt were selectively chlorinated. More than 91 %Ni , 90%Co and about 4%Fe in the chlorinated ore was extracted using a water leaching method.IntroductionLimonitic nickel laterite is an important nickel reserve, which is rich in iron in the form of goethite and has low contents of magnesium, aluminum, silicon, and other elements. Goethite is the main nickel-bearing mineral in the laterite [1]. Nickel is generally present in goethite in three modes: (a) associated with amorphous or poorly crystalline goethite, (b) weakly adsorbed to the crystalline goethite surface, and ( c) as lattice substituents [2]. In addition, cobalt in limonite was found to be associated with a manganese phase rich also in nickel [3]. These results indicate that the extractions of nickel and cobalt are highly dependent upon the degree of the decomposition of the nickel, cobalt-bearing minerals.For the selective extraction of nickel and cobalt from limonitic laterite, the ore is usually processed by hydrometallurgical methods, including high pressure acid leaching (HPAL) [4] or reductive roasting - ammonia leaching (Caron process). However, there are still some disadvantages in these processes, such as the expense of autoclaves and scaling problems in HP AL [ 4, 5], and relatively low overall metal recovery, large energy and reagent requirements for the Caron process."

Jan 1, 2011

The purpose of this study was to investigate the immobilization as a host for metallic pollutants (Cr, Cu, Pb, and Zn) by ettringite phase. Ettringite phase is produced through hydration reaction of calcium aluminate with gypsum. From the XRD patterns, it is known that the distance between spaces in 010 planes in ettringite crystal increase with an increase of ionic radius of heavy metal except Pb; no big difference is shown. For this reason, the d-value of 010 planes in ettringite crystal increased with the substitution of Cr, Cu and Zn having a big Al ironic radius. But in case of Pb, because the substitution occurred at calcium site, it does not influence to increase d-value of 010 planes.

Jan 1, 2006

By Aly M. Abdel-Rehim

The present work deals with a study of the mechanical activation of processing of Egyptian monazite by its simultaneous ball-milling and pressure leaching in order to improve the recovery of thorium and lanthanides from monazite. Experiments of simultaneous ball-milling and alkaline leaching of monazite contrary to autoclave leaching were carried out in stainless steel ball-mills of cylindrical shape under different conditions of temperature, pressure, time and alkali amount and strength. The ball-mills were heated and mechanically rotated in an electric furnace by means of roll mechanism. The effective rotation speed was fixed at 130 rpm in all tests. The charge of steel balls of different diameters was equivalent to 45% of the total mill volume. Monazite was charged in ball-mill without preliminary grinding. It is found that high rate of monazite leaching by ball-milling leaching method is achieved at lower temperature, shorter time and lower expense of alkali than in autoclaves. The results obtained show that complete recovery of thorium and lanthanides from monazite (99.8%) by simultaneous ball milling and alkaline leaching is attained at 140°C within 2 h. It is concluded that processing of monazite by its simultaneous ball-milling and leaching is mechanically activated and accelerated as a result of grinding action of steel balls that caused the continuous removal of the hydroxide product from reacting particle surfaces. This leads to the exposing of fresh and activated monazite particles surfaces to alkali leach solution and consequently the acceleration of the reaction of monazite processing.

Jan 1, 2006

By Mao Chen, Baojun Zhao, Zhixiang Cui, Leonel Contreras

Viscosity is one of the important physiochemical properties of metallurgical slags which is important for slag tapping, metal loss in slag, freeze lining and fluid dynamics. High temperature viscosity measurements are time- and cost-consuming and the number of experiments is limited. Viscosity model is an effective way to predict the viscosities of the complex slags at high temperature. However, a reliable viscosity model can only be developed on the base of accurate experimental data. A unique high-temperature viscosity measurement apparatus developed at The University of Queensland enabled accurate viscosity data to be measured for the “FeO”-SiO2-CaO-MgO-Al2O3 system in equilibrium with Fe. An accurate viscosity model has been developed based on Eyring’s theory and extensive viscosity measurements. The viscosities of copper smelting, converting and cleaning slags over a wide range of compositions and temperatures can be predicted and applied in the process control.

Jan 1, 2016

By Chen Zhang

Polycrystalline Ti-rich NiTi thin films have been deposited from a single NiTi target using a DC magnetron sputtering system. Free standing film was obtained by using a single crystal silicon substrate. Thickness ofthe thin films is controlled at around 12 pm. In this investigation, the effect of deposition temperature on the microstructure and transformation temperatures of the thin films is studied. Influence of post heat treatment temperatures on the properties of the thin films is also investigated. Transformation temperatures of the thin films are determined by differential scanning calorimetry (DSC). The surface microstructure of the thin films is studied using a scanning electron microscope (SEM), and the crystallinity is determined using x-ray diffractometry. It is found that the thin film deposited on a hot substrate is crystalline even when the substrate temperature is as low as 300°C, while the normal crystallization temperature for an amorphous thin film is around 500°C. The microstructure of the film deposited on a hot substrate shows a very fine grain size. The grain size increases with increasing substrate temperature during deposition. The effect of post deposition heat treatment on grain size is minimal.

Jan 1, 1999

By I. A. Ibrahim

Ilmenite, in its natural form, is an inactive mineral from which the selective removal of iron is rather difficult. The reactivity of ilmenite. so that it can be leached with dilute hydrochloric acid, can be enhanced by chemical reduction in solution using a suitable metal as a reducing agent. The present paper aims at the evaluation of an Egyptian ilmenite ore for the production of synthetic rutile by direct leaching with hydrochloric acid in presence of iron powder. In this process, the titanium and iron contents are dissolved; meanwhile, the dissolved titanium is hydrolyzed and re-precipitated leaving mainly iron in solution. Leaching conditions were optimized to obtain less iron in the final solid product. Addition of sufficient amount of iron powder during leaching reduces the dissolved Fe3+ to Fe2+ and reduces the dissolved Ti4+ to Ti3+. The creation of Ti3+ in solution is assumed to have a role in dissolving the ferric iron and hence increasing the reactivity of the ilmenite ore. Synthetic rutile of about 90% TiO2 and 0.77% Fe2O3 was obtained from ore with a grain size 100% passing 200 mesh and a 5-hour leach time with 20% HCl at boiling temperature (110°C) and 0.11 g iron powder / g ore.

Jan 1, 2003

By Nagahiro Saito, Takashi Nishimura, Takamichi Ichikawa, Akio Fuwa

"Yttria-stabilized zircohia (YSZ) has high potential to be used as solid-oxide fuel cell (SOFC) electrolyte. However, the high efficiency of SOFC has not been yet achieved due to the high internal resistance of bulk electrolyte. The resistance becomes lower with the decrease in the electrolyte thickness. Thus, the decrease in electrolyte thickness leads to lower internal resistance. . The aim of this study is as follows: (a) to prepare the thin films of YSZ by inductively-coupled RF plasma-enhanced metal organic chemical vapor deposition (PEMOCVD) process using Zr(t-OC4H9)4,Y(DPMh and oxygeil, and (b) to reveal the relationship between the structural characterizations and the process parameters.1. IntroductionYttia-stabilized zirconia (YSZ) has, been widely used as not only heat-resistant materials but also the components in automotive oxygen sensors, electrolytes of solid-oxide fuel cell (SOFC)(1)(2) and the buffer layers for the high-temperature superconductor because of its low thermal conductivity, good mechanical properties and high ionic conductivity. However, it is said that the internal resistance of the bulk electrolyte is too high to be appropriate as a solid electrolyte for high-efficient SOFC. The authors believe that the thin YSZ electrolyte can give a high performance to characteristics SOFC, since the internal resistance becomes lower with the decrease of electrolyte thickness. Thus the process technology to prepare YSZ thin films is desirable and must be established.In recent years, the YSZ thin films have been reported by chemical vapor deposition (CVD), thermal CVD using metal chlorides (MC) of ZrCl4 and YC(3)(4), thermal CVD using metal organic compounds (MO)(5)(10) Zr(t-OC4H9)4 and Y(C11H19O2)(11) and plasma-enhanced (PE) CVD using MO. Here, these methods are called MCCVD, MOCVD and PEMOCVD. MCCVD has two disadvantages; a large quantity of chlorinated impurities in deposited films and high processing temperature (> 1273K). This high processing temperature leads to damage of substrates in particular, so the application of this technology is limited. On the other hands, the processing temperature by MOCVD becomes and is lower. Unfortunately, the accurate vapor pressures of these metal organic compounds have not been, known so: that it is difficult to control the composition and the film thickness by MOCVD method well. Moreover, the large amount of carbonic compounds in the films prepared by MOCVD method is produced. However, plasma-effect has been reported to decrease large amount of the carbonic impurities by PEMOCVD. However, PEMOCVD has many reaction parameters in plasma processing; the geometry of experimental apparatus, radio frequency, electronic power input and so on. Thus, the general understanding about the relationship among reaction parameters, the composition and crystal structure of thin deposit film by this method has not yet been established."

Jan 1, 2000

By Michal Rzyman, Nakamura Takashi, Shibata Etsuro, Grabda Mariusz, Oleszek-Kudlak Sylwia

"Thermodynamic considerations indicate that heavy metal oxides should easily react with HBr, the main gaseous product from the thermal decomposition of tetrabromobisphenol A (TBBPA), forming low boiling point metallic bromides suitable for volatile separation. Mechanisms and kinetics of the bromination reactions must be well recognized prior to developing of a new treatment for the simultaneous recycling of plastic waste containing brominated flame retardants (BFRs) and metal oxides (printed circuit boards, automotive shredder residue, plating sludge, metallurgical dusts). In this work, a differential scanning calorimeter and laboratory-scale furnace were used to investigate the possibility and conditions of the bromination of ZnO by product of thermal decomposition of TBBPA. The formed solid, condensed and gaseous products were analyzed by X-ray diffraction analysis, electron probe microanalysis, inductively coupled plasma analysis, ion chromatography and gas chromatography coupled with mass spectrometry. Introduction Tetrabromobisphenol A (TBBPA) is the largest volume brominated flame retardant (BFR) in production today and is used in more than 70% of the world’s electronic and electric (E&E) appliances [1]. The growth in the production of E&E products and the fact they become obsolete so quickly cause significant problems in the safe disposal and recycling of the electrical and electric waste (E-waste) and other BFR-containing waste [2]. Among various treatment processes, thermal methods are most useful since they allow the recycling and recovery of both the organic and inorganic fractions of the waste. However, incineration of the BFR-containing wastes results in the emission of hazardous organobromine compounds, while the main portion of bromine released from decomposed BFRs is present in flue gas as hydrogen bromide (HBr) [3]. HBr, which is known to damage incineration systems, seems to be a very effective bromination agent for many metallic oxides present in waste. The concept of this study is to take advantage this of its property."

Jan 1, 2008

By Stein Tore Johansen

Some ferro-silicon furnaces have heat-recovery equipment. Here, the recovery of electric energy from the off-gases can be increased by increasing the off-gas temperature. This is easily done by reducing the amount of air which usually is mixed into the?off?gas to cool the gas mixture. If the off-gas becomes too hot problems with severe fouling or clogging of the gas channels close to the furnace is observed. The result is irregular stops to clean the off-gas channels. The paper focuses on the nature of the clogging phenomena and some of the ways to avoid clogging. A detailed experimental study was carried out at the Elkem Thamshavn Plant. Theoretical studies were performed to understand the particle deposition, turbulent multiphase fluid flow and off gas combustion in the off-gas channels. The study has resulted in reduced clogging.

Jan 1, 1992

By Stein Tore Johansen

Some ferro-silicon fumaces have heat-recovery equipment. Here, the recovery of electric energy from the off-gases can be increased by increasing the off-gas temperature. This is easily done by reducing the amount of air which usually is mixed into the off-gas to cool the gas mixture. If the off-gas becomes too hot problems with severe fouling or clogging of the gas channels? close to the fumace is observed~ The result is irregular stops to clean the off-gas channels. The paper focuses on the nature? of the clogging phenomena and some of the ways to avoid clogging. A detailed experimental study was carried out at the Elkem Thamshavn Plant. Theoretical studies were performed to understand the particle deposition, turbulent multiphase fluid flow and off gas combustion in the off-gas channels. The study has resulted in reduced clogging.

Jan 1, 1992

By Bradford C. Wesstrom, Omar Araujo

"Impurities from an electrolytic refinery are typically extracted from the electrolyte utilizing conventional electrowinning cells. These cells are arranged in series with cascading solution flow and are commonly referred to as liberator cells. The Freeport McMoRan Copper & Gold El Paso Refinery has optimized the removal of arsenic in cascading liberator cells by utilizing two separate feed solutions. The primary feed solution is recycled liberator electrolyte and the secondary feed solution is ""neat"" tank house electrolyte. The secondary feed solution is added based on the voltage response across the individual cells utilizing independent variable frequency drive (VFD) pumps. When the voltage across a cell changes, a signal is sent to the VFD pump to maintain a cell voltage of 1.98 volts. By maintaining this voltage the copper content in each cell exits at 2-4 grams per liter. This safely optimizes the arsenic removal as copper arsenides on the liberator cathodes.IntroductionDuring the electrolytic refining of copper, impurities from the copper anode report both to the bottom of the electrolytic refining cell as slimes and to the electrolyte. The impurities which enter the electrolyte are arsenic, antimony, bismuth and nickel. The impurities that report to the electrolyte during the electrolysis process gradually increase. As these impurities increase, they are incorporated into the refined copper cathode. There are many processes that have been used to remove these impurities from refinery electrolytes. Some of them are listed as follows: solvent extraction, ion exchange, hydrogen sulfide reduction, bioreactor, adsorption onto a low - solubility metal-oxide hydrate, adsorption onto activated carbon and EMEW cells. The conventional process used by the copper refining industry for controlling the level of impurities in electrolyte involves multistage electrolytic cascading liberator cells. In these cascading liberator cells copper, arsenic, antimony and bismuth are removed as various mixed deposits from the electrolyte. Removal of these impurities is achieved through an increase in voltage resulting from the depletion of copper in the electrolyte through electrowinning. With this higher voltage, the Group Vb elements, arsenic, antimony and bismuth are deposited on the copper cathode and report as slimes to the bottom of the cells. Nickel is removed in a subsequent process."

Jan 1, 2012

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

"Mixing phenomena in a bottom blown air-stirred one-seventh water model of CLU (Creusot-Loire Uddeholm) reactor was studie9-using three different configurations of straight circular nozzles fitted axially at the bottom of the vessel. The mixing time has been determined by pH measurements at various gas flow rates, bath heights and nozzle orientations in the presence and in the absence of a second phase.Experimental results reveal that the mixing time decreases with increasing gas flow rate. For a given gas flow rate the mixing time increases non-linearly with increasing bath height. Off-center configuration gives slightly lower mixing times as compared to center configuration. It is found that the contribution of buoyancy to the total stirring energy density is very small, but its contribution increases with increasing bath height. In the presence of an upper oil layer, the mixing time increases significantly for all configurations.IntroductionIn high temperature metallurgical melts mixing is carried out by injection of a gas either from top or bottom of the vessel in order to accelerate the rates of chemical reactions and to promote bath homogenization. When a gas is injected into a liquid through a submerged lance, porous plug or nozzle, the gas, rising as a two phase plume to the surface, imparts momentum to the surrounding liquid and causes gross circulation in the bath which promotes mixing."

Jan 1, 1997

By Toshiyuki Kozuka

CdTe semi-conducting materials have been expected as solar cell materials because its theoretical energy conversion ratio is very high. The actual efficiency still low, however, many research works have been done in order to improve the efficiency. And crystal orientation is one of possibilities for that. In this work, a new method using intense magnetic field for a control of texture of CdTe crystals will be proposed, where the CdTe film was electro-deposited under an intense magnetic field. CdTe is less affected by magnetic field, because of its cubic structure, but Cd or Te has hexagonal structure, which is sensitive for magnetic field. In this paper, crystal orientation of Cd or Te film, which can be utilized as basic layer for CdTe deposition, will be developed.

Jan 1, 2006

By Ravinder N. Reddy

Electrochemical capacitors are charge storage devices. They bridge the gap between dielectric capacitors and batteries in terms of energy and power density. Electrochemical capacitors are classified into two types, electrochemical double layer capacitors (EDLCs) and capacitors based on pseudocapacitance. In EDLC, charge is stored at the interface between electrode and electrolyte. Carbon is considered to be prime electrode material for EDLCs due to its many favorable characteristics. In this study carbon materials are derived from thermal decomposition of catechol- formaldehyde polymers and are studied as electrode material for electrochemical double layer capacitors. Carbon electrode surface is characterized using NOVA 1200 gas sorption analyzer. It is also characterized using XRD and SEM. Carbon electrodewaselectrochemically characterized using cyclic voltammetry (CV). A highest capacitance of 110 F/g was observed in 30 wt% H2SO4.

Jan 1, 2006

By G. T. Lapidus, O. J. Solis-Marcial

"The oxidative dissolution of copper from refractory minerals, such as chalcopynte, represents a technological challenge that has occupied hydrometallurgists for more than half a century. Innumerable processes have been suggested, but the majority operates at high temperatures or employs corrosive media. The origin of this refractory nature is the formation of passivating phases of iron(III) or copper. One option is to add non-corrosive ligands that complex these metal ions, thereby facilitating their dissolution. In the present work, the effect of acetone in sulfuric acid solutions was studied. The initial experiments were on chalcopynte carbon paste electrodes using cyclic voltammetry, where greater reactivity was observed. Later, leaching tests with hydrogen peroxide, cupric sulfate and ozone and, as oxidants, were performed. High extractions were achieved in three hours at 50°C. The solid residues contained the iron in the form of Fe203 and FeOOH.IntroductionChalcopyrite is the most important mineral of polysulfide copper ores [1] and accounts for approximately 70% of the world's copper reserves [2]. Currently, the copper present in chalcopyrite is extracted mainly by pyrometallurgical processes, which generate environmental concerns because of the formation of SO2 gas and submicron particulates [3]. The development of a less aggressive hydrometallurgical process for the extraction of copper would constitute a possible solution to these problems. For that reason, studies of the dissolution behavior of chalcopyrite are of great technological importance [4], However, the proposed oxidative leaching routes for chalcopyrite, generally at high pressures and temperatures, have not been implemented on an industrial scale, because of the elevated costs required to equal the high copper extractions obtained in thermal processes. These extreme leaching conditions are required because of the refractory nature of chalcopyrite. Passivation has been used to explain this phenomenon, although researchers have disagreed on the composition of the layer, which is various have assumed to be sulfur, copper sulfides, and iron-bearing jarosites or hydroxides [5]. If the latter compounds are the cause, an alternative solution would be the use of polar organic solvents in the oxidative leach to decrease the formation of the passivating iron layer. In this work, the influence of acetone on the oxidative leaching of a chalcopyrite concentrate at room conditions is explored."

Jan 1, 2012

By Qinghai Pang

"With the increasing proportion of bituminous coal in blend coal, the safety of blend coal during pulverization and transportation is gradually being paid more and more attention. Therefore, the explosivity of bituminous pulverized coal (PC) with different volatile content from 25 to 38% was studied by measuring the combustion flame length after its injection into a glass pipe with the heat source installed in the center. The results indicated that high volatile content bituminous PC is apt to have higher explosivity. By blending different bituminous PC with 10% anthracite, the explosivity of bituminous PC showed a positive correlation with the proportion –OH radical. However, different bituminous PC seemed to have the same explosivity when the addition of anthracite increased to 20%. With the further increasing proportion of anthracite to 30%, the explosivity of bituminous PC with high –OH proportion became negligible while a weak explosivity of high –CH3 proportion bituminous PC still remained.IntroductionWith the increasing iron ore prices and decreasing steel prices, it has become critical for iron and steel enterprises to control the cost in ironmaking and steelmaking process. Blast furnaces (BF) are the main consumer in ironmaking process, which occupies 70% fuel consumption of total steelmaking process [1]. In this circumstance, any means necessary is taken by BF operators to lower the cost of iron in production. Coke and iron ore are the main expense in this process, who takes up a very high proportion in total cost. Pulverized coal injection (PCI) is the most efficient way to reduce coke ratio, which replace coke with relatively cheaper PC.At present, most of BF is injected with blend coal in the consideration of decent combustion property and quantity of heat. Simultaneously, bituminite and anthracite blending is an effective method to obtain blend coals with required composition and performance, such as volatile and ash content, etc. Nevertheless, a very huge gap was found between the price of bituminous coal and anthracite in some regions of China, in which the price of bituminite can be just 70% of the price of anthracite. Thus, iron enterprises in these regions attempt to possibly amplify the proportion of bituminite in blend coal. Increasing proportion of bituminite results in higher volatile content in blend coal, by which the safety of blend coal during pulverization or transportation was deteriorated.Relatively, coals with higher volatile content usually possess stronger explosivity, which means that volatile and explosivity may related to some extent. However, the relationship between volatile and explosivity is not of certainty for some PC with high volatile content around 40% was found to be inexplosive in comparison to the coals with lower volatile content. With the increasing proportion of bituminous coal in blend coal, investigations on the factors of PC explosivity have become more and more important. Therefore, bituminous coals with different volatile content were selected. The explosivity of blend coal and its relationship between volatile content and functionality was investigated in this research."

Jan 1, 2014

By Jin-tao Gao

In order to recover Ti resource from titanium bearing blast furnace slag, a new technology to separate perovskite phase from CaO-TiO2-SiO2-Al2O3-MgO system by supergravity is researched. In the condition of gravity coefficient of 750g, treatment temperature of 1305°C and time of 20min, the significant layers appear in samples which are obtained by means of centrifugal treatment. Along the direction of the supergravity, the volume fraction of perovskite phase increases gradually, and the equivalent diameters of perovskite phase crystals increases with the area approaching to the bottom of the sample. It is indicated that TiO2 is enriched in the bottom of sample as concentrate with a recovery ratio of 74.05% by supergravity treatment.

Jan 1, 2014

By Noboru Masuko, Sachiko Ono

"The structure and composition of anodic films formed on aluminum in a borate solution have been investigated by using TEM and SIMS with respect to the effect of current density and electrolyte temperature. The film is composed of a boron-containing outer layer and a boron-free inner layer with disc-like crystals present at the interface. The thickness of the film formed at constant current density up to an identical voltage, decreases with increasing current density. The thickness increases remarkably with elevated temperature. The transport number of Al3+ estimated from the thickness ratio .of the cuter to the inner layers is 0.4 when the film is formed at the current density of 20 Am-2 at 60°C. It increases slightly with increasing current density and decreases significantly with increasing temperature. Content of boron in the outer layer increases 1.5 times when current density .increases 10 times. These changes in film structure and composition with electrolysis conditions must have a significant role in the determination of electric properties of anodic alumina films as a capacitor material.IntroductionThe growth of anodic alumina film in ·a neutral electrolyte proceeds at both film/electrolyte and film/substrate interfaces giving a duplex structure. The oxide layer formed at the former interface includes electrolyte anions while a-pure alumina layer is formed at the latter interface. The thickness ratios of each layer respectively represent transport numbers of Al3+ and 0 2 - (1). The film thickness and the incorporated anion content as well as transport numbers of both ions must affect the dielectric properties of the film as a capacitor material. However, the correlation between film structure and electrolytic conditions is not fully understood (2). For the further clarification of anodic film growth mechanism, more detailed characterization of anodic films in relation to electrolytic conditions is advantageous. In the present paper, therefore, the effect of current density and electrolyte temperature on the microstructure and composition of anodic barrier films formed in a neutral borate solution was studied. The films were characterized by direct observation using transmission electron microscopy (TEM) and depth profiles of constituent elements obtained by secondary ion mass spectroscopy (SIMS)."

Jan 1, 2000