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By Greg Dowling, Jun Ge, George Shannon, Shufeng Yang, Yongfeng Chen, Lifeng Zhang

"Inclusions in 316L stainless steel ingots poured using two different upgate designs – a traditional upgate and a swirl upgate - were investigated using SEM and ASPEX automated inclusion analysis. The main inclusions were high SiO2 inclusions, MnS inclusions and SiO2-Al2O3-CaO inclusions. More inclusions were detected at the top of the ingot than other places in vertical direction, and more inclusions were at the edge of the ingot than other place in the radial direction. With swirling upgate there were more K- and Na- bearing inclusions than that with the traditional upgate indicating possible more serious flux entrainment with the swirl upgate.IntroductionIngot casting still is very important for production of special steel grades including high carbon chromium bearing steel, thick plate, seamless tube, forgings, bars, and wire rods [1] . During the bottom teeming process, molten steel enters the trumpet and passes through the spider into the runners. Molten steel then enters the ingot mold through an upgate near the end of the runner. In the early stages of filling a mold, a mold flux bag hung in the mold were burnt and the mold flux will cover the top of the rising steel to protect the steel from being reoxidized, acting as well as act as a thermal insulator. So far, some efforts on studying inclusions characteristics in the ingot have been reported. A review paper on the control of inclusions during steel ingot casting was published by Zhang et al. [2] Zhang also studied Inclusions in bottom-teemed ingots of plain carbon steel and found that the >20µm inclusions originated from either the entrainment of mold flux of the reoxidation during teeming process. [3] The results of Nagendra and Du showed that there were more inclusions in the centre part of the ingot [4]. Eriksson et al reported that the composition of inclusions was more complex in the mold samples in comparison to the ladle samples, and more inclusions in the mold were found than in ladle because of the reaction between the mold flux and the molten steel [5]. It was reported that SiO2-CaO-Al2O3 inclusions originating from mold powder with reoxidation product Al2O3 as a part, and there were more inclusions close to the side wall than the center of the ingot in the radial direction. [6]. A more recent investigation showed that four main types of inclusions in runner samples were classified: oxides, sulfides, complex and carbon-nitrides. [7] The flow pattern in the mold during filling has been found to be an important factor regarding inclusions in the ingot. In the early stages offilling a mold, steel enters the mold through the entry nozzle at a high velocity. The effect of the resulting turbulence on the meniscus can lead to the entrainment of mold flux. Efforts have been paid over the years to find methods to reduce the velocity of the molten steel entering the mold, such as using opening angle of the inlet nozzle [8], using swirl blade at the runner [9], using a divergent nozzle combined with a swirling flow generated in the nozzle [10-11]."

Jan 1, 2012

By Dai Yongnian

"The feasibility to vacuum distillation of a crude metal or an alloy was discussed. The equilibrium relationship between vapor phase and liquid phase in A-B system - - - - - PA/PB =BAa*/b has been derived. The separation coefficient, BA = rAPA/(rBPB) is a judgment criterion. By calculation PA/PB, the equilibrium composition diagram of vapor phase and liquid phase was drawn. By use of the equation derived by M. Olette, the relationship among the volatilization amounts of various impurities in a crude metal (yi) was further solved. 1-(X/100)= C =(1-Y1/100)1/02i . From yi value obtained in practice, 2i, Pi and then can be calcu-lated. The correct volatilization order of various impurities was obtained. These results can be applied to determine the practical conditions (temperture, vacuum degree, type of distilla¬tion furnace, times of distillation and control of product composition) in distillation of a crude metal or an alloy.INTRODUCTIONRefining and separation of various impurities from nonferrous crude metals by vacuum distillation have many the advantages of high metal recovery, impurities recovered in metallic state, flowsheet simplified, good enviromental protection, low operation costs and in complex equipment. So in recent years this method has been adopted widely.Vacuum distillation has also been studied and used in separation of various elements from non-ferrous alloys and the area of its application is being extended rapidly.At this situation, some problems have been put up: What kind of impurities can be removed from crude metals? What kind of alloys can be separated by vacuum distillation? In present paper, attemps have been made to answer these problems and combine with practical results to analyse some valuable data obtained from testwork on vacuum distillation of crude tin and Pb-Sn alloy."

Jan 1, 1988

By R. W. Harnmack

Hydrogen sulfide generated by the anaerobic respiration of sulfate-reducing bacteria was used to treat pH 2.2 water from the abandoned Rio Tinto copper mine in Nevada. The untreated water contained 550 mg/L Fe, 140 mg/L Al, 90 mg/L Cu, 80 mg/L Mn, 60 mg/L Zn, 4 mg/L Co, and 2 mg/L Ni. The bench-scale treatment system examined consisted of a bioreactor for H2S generation and three precipitator/clarifier units for metal sulfide precipitation and recovery. The treatment system reduced the concentrations of all metals except Mn to less than 0.1 mg/L. Manganese concentrations were reduced by 96 percent to 3.3 mg/L. A CUS/SO concentrate (33 pct Cu) and a ZnS/5° concentrate (28 pct Zn) were produced that may be suitable for metal recovery at existing smelters

Jan 1, 1994

By Gaballah I.

Elimination of arsenic, mercury and zinc from synthetic solutions containing H;\A.sD4. HgCI2 and ZnCI2 using modified barks was investigated. The pH range was varied from ?1 to 10. The initial concentrations of individual element were 10,100 and 1000 ppm. More than 99 % of mercury and 65 % of zinc cations were removed by the modified bark .. In this case, the modified bark reacts as a cation exchanger leading to the release of ' two protons for every HgII or ZnII fixed by this material. About 30 % of arsenic was eliminated from the solution. This 'low efficiency could be attributed to? the presence of arsenic ,as. anion. Decontamination of a treated industrial effluent containing 4 ppm of ion? metals was performed on a pilot plant scale by the modified bll(k. More than 70'% of these ion metals were eliminated.

Jan 1, 1995

By H. Conrad, K. Jung

"The effect of an external electric field E=5(+) kV/cm applied during the solution heat treatment at 500°-550°C of three commercial Al-Mg-Si alloys (AA6061, AA6022 and AA61l1) on the asquenched resistivity Pw and hardness H.,NULL, w was investigated. It was found that the field gave a significant increase in Pw and in Hv,w, for AA6022 and AA6111, but had no clear effect on AA6061. Thermodynamic analysis gave that the effect of the field on AA6022 and AA6111 was to reduce both the enthalpy ?H, and entropy ?H, of solution. Considering the chemical composition of the three alloys it appears that the influence of the field may depend on the amount of Cu plus excess Si present in the alloy.IntroductionKlypin and Soloviev [1, 2] were the first to report that the application of an external electric field during solution heat treatment (SHT) of Al alloys gave an increase in the as-quenched resistivity and hardness. They attributed these effects of the field to an increase in solubility of the alloying constituents during the SHT. More recently Liu and coworkers [3, 4] also reported an increase in the as-quenched resistivity of Al-Li alloys with application of an electric field during SHT. Further, the present authors [5] found that the application of an electric field during the SHT of the commercial Al-Mg-Si alloys AA6022 and AA61i1 increased their as-quenched resistivity and hardness. Their thermodynamic analysis of the results indicated that the field decreased both the enthalpy ?H, and entropy ?S, of solution."

Jan 1, 2004

By E. Allaine

Carbochlorination kinetics of pure MoO3, Nb2O5, Ta2O5 and V2O5, by Cl2+CO+N2 gas mixtures was investigated between 380 and 1000 °C. Standard free energy of carhochlorination reactions and phase stability diagrams of these refractory metal compounds were calculated. The influence of total gas flow rate, temperature, reactants partial pressures on the reactivity of these oxides were investigated. The apparent activation energies were found to be about 83, 75, 110 and 100 kJ/mole below 650°C for MoO3, Nb2O5, Ta2O5 and V2O5, respectively. Above this temperature, the Arrhenius plots exhibit a rate anomaly attributed to thermal decomposition of COCl2 and/or structural changes of these refractory metal oxides. The apparent reaction order of carbochlorination of these oxides with respect to Cl2+CO was determined. For these refractory metal oxides, the reaction rate was maximum for a Cl2/CO ratio of about 1 in the chlorinating gas mixture. Results of carbochlorination of these oxides are compared and discussed.

Jan 1, 1995

By Bin Xu, Qian Li, Yong-bin Yang, Tao Jiang, Jian-jun Hu

It could significantly increase the leaching rate of refractory gold concentrate containing sulfur and arsenic by roasting pretreatment with adding certain amount of sodium sulfate, and the mechanism of that was systematically researched with DSC, XRD and SEM in this paper. Results indicated that the mechanism of Na2SO4 on double refractory gold concentrate at roasting pretreatment can be summed up in the following three aspects：Firstly, Na2SO4 can react with SO2 and SO3 which is produced by the oxidation of sulfides and generate Na2S2O7(l), which plays buffer effect on sulfides exothermic oxidation, avoiding the secondary-encapsulated of gold. Secondly, the liquid phase of Na2S2O7 can cover mineral particles' surface that possesses a sintering effect, it leads to internal cracks of the particles. Finally, mineral particles will gather with sodium sulfate particles as the center that can improve the permeability of the layer.

Jan 1, 2015

By Masaki Imamura

A novel hydrometallurgical process for copper concentrate treatment has been developed by Niihama Research Laboratories of Sumitomo Metal Mining Co., Ltd. The process has numerous advantages with respect to the operational and environmental aspects. For example, copper is leached effectively from chalcopyrite concentrates by chlorine gas under atmospheric pressure. The copper in the leach solution is then separated from iron and silver by solvent extraction and undergoes electrowinning for its recovery as a highly pure copper metal; this does not require any further purification. Moreover, iron metal can be produced from the purified raffinate by electrowinning without generating a large volume of goethite or hematite, which are solid wastes generated due to iron rejection in common hydrometallurgical processes. This process can also realize the efficient recovery of precious metals. The results of batch testing and continuous-operation testing are presented in this paper.

Jan 1, 2006

By Victor Bredykhin

The reasons of formation low quality cathode deposits and conditions of the anode passivation in electrorefining of copper silver alloys with increased (more then 5%) silver content in electrolyte, g/l: Cu - 40; H2SO4-50; 150 and 250; T= 401C have been investigated. As it is shown, increased acidity, anodic current density and silver content in anodes favor passivation. The assumption is made that the ingress of silver on cathodeis the most probable reason of growing dendrites on cathode. We have determined that addition of ethylene carbonic acid to electrolyte in the amount of 3,5 ÷ 10 ml/l suppresses the dendrite formation.

Jan 1, 2006

By K. Murayama, M. Kawakami, T. Takenaka, S. Yokoyama

"Cokes play an important role of spacer in blast furnace. However, they degenerate during Boudouard reaction. Blast furnace cokes are reacted with pure C02 at I 072 to 1673 K. Reaction rate was obtained by the weight change of spherical specimen. The specimen after reaction was examined by microscopic observation. The reaction rate increased with temperature and was expressed by two Arrhenius type lines. The activation energy was 126 KJ/mol at higher temperature than 13 73 K and 202 KJ/mol at lower temperature range. At the higher temperature range, the reaction proceeded from the surface leaving unreacted core, whereas homogeneously whole inside at lower temperature. The porosity increased from the center to surface at higher temperature, whereas it was almost constant at lower temperature.IntroductionThe cokes have the function of fuel, reductant and spacer to keep gas and liquid flow in the blast furnace. Thus, the reaction mechanism of coke with several gas and the strength after the reaction should be important factor to control the blast furnace operation. The reaction mechanism of coke with C02 has been studied extensively. The rate equations were derived by Gadsby[ I], Ergun[2] and Turkdogan and Vinters[3]. They were compared and discussed by Kobayashi and Omori [ 4]. Effect of crystallization degree on the reaction rate was examined by Kashiwaya and Ishii[5]. Catalytic enhancement effect of ash componets have been clarified by Kashiwaya et. al. [6]. Although degradation of coke in blast furnace has been examined recently[7], however, the degradation of coke after the reaction with C02 has not been well clarified yet. In the present work, the metallurgical coke specimen was heated in N2 and C02 and the reaction mechanism and degradation behavior after the reaction was investigated."

Jan 1, 2000

By F. M. Wang, J. P. Lin, G. Y. Tang, H. C. Zhou, Y. F. Liang, F. Ye

"Fe-6.5%Si alloy is a very excellent soft magnetic material compared with conventional Si steel (Si content ~ 3.5%), especially in high frequencies with reduced iron losses and noises. But it is hard to be fabricated due to its brittleness at room temperature. Dynamic electropulsing is applied to the cold rolled Fe-6.5%Si sheet during tensile deformation. Mechanical and microstructural properties are investigated with different electropulsing and strain rate. It is found that the yield stress decreases and the elongation increases dramatically with the application of dynamic electropulsing. It is indicated that the work hardening could be reduced with the dynamic electropulsing during deformation, which provides a promising way to fabricate this alloy sheet much easier.Introduction Fe-6.5%Si (weight percent, same as below) alloy has more excellent soft magnetic properties compared with conventional silicon steel (Si content ~ 3.5%), such as higher resistivity, higher permeability, near zero magnetostriction, etc. and exhibits much lower core losses and noises [1]. However, Fe-6.5%Si is very brittle at room temperature and hard to be fabricated in strip by conventional hot-cold rolling process [2]. This lack of low-temperature ductility has been generally attributed to structural ordering ofB2 and D03 phases [3]. Several methods have been developed to avoid its brittleness, such as chemical vapor deposition (CVD) [4], rapid quenching [5, 6], dipping and diffusion [7, 8], direct powder rolling (DPR) [9], etc. However, hot-cold rolling method is still of interest for industrial applications. In our previous work, this alloy can be cold rolled after certain thermomechanical process and heat treatment [10-13]. The cold rolled sheet exhibits some extent of ductility [11]. However, side cracks are common for the rolled sheet, it is very necessary to improve the ductility of this alloy by other technical applications."

Jan 1, 2012

By Kimio Itagaki

"As a contribution to understand the smelting of copper or nickel matte by blowing oxygen or oxygen-enriched air, the phase equilibrium and the distribution of minor elements between the iron-silicate based slag and the Cu2S-FeS or Ni3S2-FeS matte at 1573K were investigated in a magnesia crucible under controlled partial pressures of SO2 at 0.1, 0.5 and 1.atm. At a given matte grade, the solubility of copper in the slag was found to be independent of p5O2 while that of nickel was dependent on pSO2 and these behaviors were analysed thermodynainically based on a concept of oxidic and sulfidic dissolution of the components in the slag. When the matte grade was specified, the distribution ratios of X, defined as (wt pct X in slag)/(wt pct X in matte}, for As, Sb and Bi increased with increasing p5O2 while that for Ag was constant against p5O2.IntroductionA combination of intensive reactors with the use of oxygen or oxygen-.enriched air as the blowing gas has provided a number of improved copper and nickel smelting processes such as INCO-Flash, Outokumpu-Flash, Mitsubishi-Continuous and IBRC (top blown rotary converter) processes. Phase equilibrium and thermodynamic studies for the slag and the copper matte or the nickel matte under high partial pressure of SO2 are of practical importance for evaluating the behaviours of the related components in the oxygen-smelting.A series of experimental studies have been already conducted in a limited range of conditions for Pso2 around 0.1 atm, which corresponds to the smelting with air-Stowing [1-5]. However, there remain very few data on the phase equilibrium in the matteslag systems under higher partial pressures of SO2. Tavera and Davenport studied the phase equilibrium between the copper matte and fayalite slag phases under the partial pressure of SO2 controlled at 0.1 - 1 atrn but without controlling the partial pressures of sulfur and oxygen [6]. A potential diagram for the Cu-Fe-S-O-SiO2 system at 1523 - 1573K suggests that the partial pressure of S2 equilibrated with the matte and the fayalite slag with saturated SiO2 under the high SO2 pressure is considerably high at 10-4 - 10-2 atrn [7]. This condition must require controlling of p52 as well as Pso2, in the equilibrium experiments, otherwise, the equilibrium condition may be hardly attained due to the continuous flushing of sulfur from the system."

Jan 1, 2000

By W. Dresler

Design details of a 100 kVA DC electric-arc reduction furnace are described. The furnace is equipped with a 610 mm (24 inch) diameter graphite crucible hearth. A 76 mm (3 inch) diameter top graphite electrode is used as a cathode. The current passes through the bottom of the crucible and is carried to a bottom plate (the anode) by conductive magnesia carbon bricks. The furnace can be operated up to a maximum of 120 V, 1800 A, and presently 100 kW. The start-up operating experiences and metallurgical results of one reduction test with a Montana chromite containing 38% Cr2O3 are discussed.

Jan 1, 1994

By Tiejun Chun, Jian Pan, Deqing Zhu, Vinicius Mendes

"Fine manganese fines are characterized by large amount and low price compared to lump manganese ores. However, fine manganese must be agglomerated as EAF (electric arc furnace) feed. In this paper, high quality fired pellets were produced by simulating grate-kiln process to supply the feed for EAF from some imported manganese ore fines containing high combined water. Manganese ore fines assaying 44.47wt%Mn, 5.89wt%Fe, 12.09%LOI and with 72.7wt% ranging between 0.5mm and 8mm, are pretreated up to the particle size of 84.7wt% passing 0.074mm by HPGR (high press grinding roller) twice in open circuit. The finely ground manganese fines were mixed with 1.2wt% bentonite, balled at 15% moisture for 7min in disc pelletizer. The drop numbers, compressive strength and thermal shock temperature of green balls reach 11 times/0.5m, 11 N/pellet and 360oC, respectively. After the green balls drying in the oven, the dry pellets were preheated at 1050oC for 12 min and then fired at 1300oC for 12 min in electric tube furnace. The compressive strength of fired pellets reaches 2621 N/pellet. Therefore, these pellets are high quality burden for blast furnace or EAF due to high mechanical strength and high Mn grade of 49.11wt% and low detrimental elements.IntroductionManganese, mainly using as deoxidizing agent, desulfurization agent and alloying elements, is widely used in the steel company. With the rapid development of iron and steel industry in China, domestic manganese ores cannot meet the requirement, resulting large quantities manganese ores import to China [1-4]. Compared to lump manganese ores, fine manganese ores containing high combined water are characterized by large amount and low price. However, they must be agglomerated as EAF (electric arc furnace) feed. There are three ways to agglomerate the manganese fine ores, sintering, briquetting and pelletizing [5-6]. Compared to the other two methods, pelletizing technology possesses the following superiorities, such as uniform size distribution of product, stabilizing chemical composition of product and lower energy consumption in producing. Therefore, pelletizing is a superior way to treat the fine manganese ores [7]. The systematic research of producing manganese oxide pellets by fine manganese ores containing high combined water was studied in this paper."

Jan 1, 2011

By G. O. Onyedika, M. U. Obidiegwu, G. C. Onuegbu

The effect of kolanut (KN) filler and compatibilizer (maleic anhydride) contents on the transport of toluene through low density polyethylene (LDPE) and low density polyethylene composite were studied at the temperatures 40, 60 and 80 °C.The kolanut powder used was ground to 25 μm particle size. In preparation of composite 0–5 wt% of kolanut powder and 0–2.5 wt% of the compatibilizer were mixed with 200 g of low density polyethylene in an injection moulding machine. The injected polyethylene and polyethylene/kolanut composites (LDPE/KN) were taken for sorption test. The sorption data obtained for low density polyethylene and kolanut powder filled low density polyethylene at the different temperature investigated were expressed as the molar percentage uptake (% Qt) of toluene per gram of the kola nut composites. Results show that the uptake of toluene at the five filler content (0–5 wt%) generally increased with increase in sorption temperature but decreased with increase in compatibilizer and filler contents. This can be seen at 80 °C and 0, 1, 1.5 and 2.5 wt% of compatibilizer respectively. The molar percentage uptake of toluene at 1 wt% of filler yielded the following values; 8.6789, 8.4768, 8.3476 and 8.2679 respectively. At 2 wt% it yielded 8.6224, 8.1333, 7.9525 and 7.9042 respectively, at 3 wt% it gave 8.4336, 7.9450,7.8900 and 7.7823 respectively, at 4 wt% it yielded 8.0263,7.9614,7.8218 and 7.6800 respectively and at 5 wt% it gave 7.9635, 7.8630, 7.6256 and 7.5013 respectively.

Mar 1, 2017

By N. Bazzanella

The hydrogen desorption kinetics of pure and Nb-doped magnesium hydride film samples was investigated by using a Sievert-type apparatus. The overall activation energy and the reaction order controlling desorption are (141±5) kJ mol-1H and n 4 for Mg hydride and (51±5) kJ mol-1H and n 1 for Nb-doped (5% at) Mg hydride indicating that, in the doped sample, hydrogen desorption is controlled by the H migration in transformed h-Mg layers. Structural analysis performed by X-Ray Diffraction (XRD) and Extended X-Ray Absorption Fine Structure spectroscopy (EXAFS) show that the catalytic effect of the Nb dopant is connected with the formation of NbH0.89 nanoclusters dispersed in the Mg hydride matrix. It is suggested that the catalysis process is also connected to the presence of Mg-Nb hydride interfaces where the transfer of H atoms preferentially occurs by connecting h-Mg grains and by the role of the MgH2-NbH0.89 interface as preferential site for the dissociation of the hydride phase.

Jan 1, 2006

By M. L. Apel

A conceptual approach to the bioremediation of uranium mill tailings (UMT) is presented., This approach focuses on, biosorption to remediate the. effluent solution and bioleaching remediate the. solid fraction. Comparative biosorption studies were performed with synthetic single metal solutions using a commercially available biopolymer. The maximum rate of metal sorption by calcium alginate was found to be 5.43, 6,39, 6.48, and 9.74 mg dm-3 min-1 for U022*, Ba2+, Cd2+ and Zn2+, respectively. Activation energy (AEa) for barium uptake by calcium alginate beads was determined to be 11.5 kJ, indicating a diffusion controlled reaction mechanism. Thermodynamic values (AG+ AH+ and ASt) of the metal-alginate activated complex, as reported in the literature, were found to be in agreement with those calculated from this research. Results show that this biopolymer can be effectively applied in the removal of select metals prevalent in uranium mill tailing effluents and associated waste streams.

Jan 1, 1991

By Fatma Arslan

The lateritic nickel ore sample subjected to this experimental study was taken from Çalda ore deposit (Turkey) and contains 1.43% Ni and 0.105% Co. Mineralogical investigations showed that the ore sample contains asbolane, chromite, limonite, hematite, goethite, lepidocrocite, magnetite, serpentine, and clay type minerals together with chalcedon, quartz, calcite, and chlorite. In the acidic leaching experiments, the effects of temperature, acid (H2SO4) concentration, and leaching time on nickel leaching recoveries were investigated. Leaching recovery versus time curves showed a parabolic trend and increasing the temperature shifted that curves to the higher values. The dissolution of nickel from lateritic ore can be explained by a shrinking core model and the apparent activation energy was found as 47.34 kJ/mol in the range given by the literature. The highest Ni and Co leaching efficiencies as 90.2% and 96.8% respectively were obtained at 80°C temperature, 200 g/L H2SO4 concentration, and 8 hours of leaching time.

Jan 1, 2006

By J. E. Dutrizac

The behaviour of the lanthanide elements during the precipitation of sodium and potassium jarosites at 98oC from sulphate media was systematically investigated. The lower atomic weight lanthanide elements (La to Gd) are characterized by the limited solubility of their alkali-lanthanide sulphates, such as NaNd(SO4)2?H2O, which commonly contaminate the jarosite precipitates. Hence, single phase jarosite-type compounds were precipitated only from solutions containing <0.4 g/L of the La to Sm lanthanides. The sulphates of the heavier atomic weight lanthanide elements (Tb to Lu) have significantly higher solubilities such that solutions containing up to 10 g/L of the individual lanthanides could be investigated without the precipitation of alkali-lanthanide sulphate species. Even at the highest lanthanide concentrations, however, none of the jarosite precipitates incorporated more than 0.3 wt% of any of the lanthanide elements. Comparable levels of lanthanide incorporation were noted in both Na-jarosite and K-jarosite. Although the mass of the jarosite precipitate increased with increasing ferric sulphate concentration or with increasing pH, the extent of lanthanide incorporation was not significantly affected. Clearly, the trivalent lanthanide elements do not substitute extensively for trivalent iron in the jarosite structure. This behaviour likely reflects the significantly lower hydrolyzability and larger size of the trivalent lanthanide ions relative to ferric ions.

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