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By T. Kamata, S. Takemoto, H. Takeuchi, M. Takayanagi, Y. Akahori, I. Jimbo

"A cooperative research work on the silver recycling process is underway between Matsuda Sangyo Co., Ltd. and Tokai University in Japan. Silver wastes treated here are mainly from photograph industries where the concentration of minor element is steadily increasing in the recent years. The waste materials are concentrated and the impurities are removed by evaporation and slagging. In this paper, the industrial practice of wastes treatment is introduced and the result of the laboratory studies on the removal of antimony and tin from the binary and ternary alloys will be discussed. Characteristics in the behavior of antimony and tin during the process are also discussed with the observation of practical operation.1. IntroductionPrecious metals such as gold and silver primarily come from mining practice and the byproduct in copper smelting. However, the recycled amount of these precious metals have been increased 1 along with the environmental restriction and the widely accepted idea of saving resources on the earth in the recent years.· Though the recycle process of precious metals are comparatively simple from other metals refining, the process has been getting more complicated as wastes treatment has to deal with more impurity elements which are intentionally added to the products. Among these additives, antimony is used in the film materials in the photography industries to suppress its inflammability. Tin is another concern ,that is also coming from photography wastes; These minor elements have become problematic during the recycle.The removal of these minor elements has been in operation at Matsuda through a traditional oxidation refinement process using a reverberatory furnace. However, the complexity of the charge makes the recycle process more tedious and troublesome. In order to investigate the minor element behavior in the complicated materials system during the silver recycling processes, a cooperative research work is undertaken between Matsuda Sangyo Co., Ltd. and Takai University in Japan. Silver wastes treated here are mainly discharged from photograph industries where the minor element contents such as antimony, tin and bismuth in those wastes are steadily increasing in the recent years. The liquid wastes containing silver are concentrated and then treated pyrometallurgically with solid wastes from other sources, where the impurities are removed ·by evaporation and slagging. The purpose of this study is to investigate detailed behavior of impurity elements in the silver. containing systems."

Jan 1, 2000

By T. Iriyama, Y. Fujita, R. Omatsuzawa, T. Nishio, N. Okochi

Sm-Fe-N hard magnetic materials are good candidates for high performance bonded magnets. Rapid-quenching method should be highly favorable for the fabrication of isotropic magnet powder with high coercivity. We report here the magnetic properties of Sm-Fe-N powders produced by a few kinds of rapid-quenching processes. Sm2Fe17 powders were prepared by gas-atomization (GA), rotating-disk atomization (RDA), or melt-spinning (MS) method. The Sm2Fe17 GA powder had dendritic solidification structure, while the RDA powder had micro crystalline structure with size of 3-5 µm. Coercivities (HcI) of their nitrides were 56 (for GA) and 217 ka/m (for RDA). The H cI of nitrided Sm2Fe17 MS powder with wheel velocity (V5) of 5-20 m/s, which had also microcrystalline structure, was 53 to 509 Wm. These coercivity values are not sufficient for bonded magnet applications. From the study of additive effects, it was found that C, C-Si, C-Ga, or C-Al addition decreased the crystal size of quenched Sm2Fe17 powder. Consequently, high coercivity was obtained; the HcI of nitrided Sm2Fe1C1Si1 MS powder with V5 of 10 m/s was 898 kA/m, and 708 kA/m for the nitrided Sm2Fe15C1Si1 RDA powder. The compression-molded bonded magnet made from Sm2Fe18Si0.1Nx MS powder showed a high (BH)max of 82.7 kJ/m3.

Jan 1, 2000

By Chris T. Vild

"ABSTRACT NOT AVAILABLEPRESENTATION SUMMARYIntroductionToday, light gauge aluminum scrap is melted in sidewell furnaces using natural gas reverberatory burners. The scrap is introduced into the sidewell adjacent to the combustion chamber through a submerged archway. Super-heated metal is then pumped into the sidewell where it aids in melting the scrap. From the sidewell, the flow is returned to the combustion chamber through a second submerged archway at some lower temperature. Normally, the burners are set at a designed high fire level and the scrap is introduced at a rate to attempt to mat.ch the burner input. A thermocouple in the bath is programmed to throttle back the burners to low fire if a high temperature limit is exceeded.Jn many cases the thermal efficiencies of these furnaces can be very low. With inadequate circulation, air and natural gas furnaces run at a dismal 18% thermal efficiency. If a circulation system· is added, the efficiency can jump to 28%. For a $100 million lb/yr recycling facility, and natural gas prices reaching $4.50 per million Btu, fuel cost at 18% efficiency can reach $1 million per year. A 10% increase in thermal efficiency saves $350,000 a year in fuel costs.With an increase in thermal efficiency, furnace utilization also increases. A 10% increase in thermal efficiency would result in a 20 million Btu furnace producing 12,000 lb/hr up from 8,000 lb/hr or 35 million lb more produced per year. This is a 33% increase in output.Most current furnace development has focused on burner technology using oxy-fuel, regenerative burners, etc. However, thermal efficiency is also largely effected by the molten metal circulation rate and how well the scrap is mixed into the superheated metal. Therefore, the flow dynamics should be optimized first, before installing of more thermal power.Jn an effort to understand the effect of these variables, a series of computer models were made and the critical factors studied with the goal of demonstrating an increase in thermal efficiency and production. Large-scale graphical representations of these models will be presented."

Jan 1, 2000

By R. A. Spitz, R. Leiby, M. Bricker

Electrochemistry plays a significant role in minimizing wastes at East Penn's secondary lead smelter. East Penn has been recovering spent battery acid for reuse in new batteries since 1992. East Penn also produces a fertilizer feedstock from sulfur dioxide in the smelter stack gases. The success of these processes is, in large part, due to the installation of electrochemical cells. The cells in the acid recovery plant allow the waste from this process to be concentrated into less that 10% of the original spent acid. The cells in the fertilizer plant treat the solution to remove dissolved metals prior to sale to fertilizer manufacturers.

Jan 1, 2000

By A. V. Tarasov, S. D. Klushin

493 The most common method for minimizing the copper content of residual slag in the process of autogenous smelting of sulfide raw materials is treatment of molten slag in an electric furnace, with optional addition of solid reducing agents, such as coke, and/or sulfiding agents such as pyrite. A drawback of this technique is the fact that the final slag produced still contains 0.5% or more Cu. We have tested a method for treating molten slag obtained as a result of autogenous smelting by a gaseous mixture of sulfur dioxide and methane at a ratio of. SC:SO2 = 0.75 :1.0 in the presence of oxygen. Interaction reaction within the SO2-O2-CRi system proceeded at a high rate at 1373 to 1573 K to form reducing and sulfiding agents: H2S, S, COS, CO, CO2, H2, H2O. The gas mixture requirement was about 100 to 150 Nm3 per 1 tonne of slag. A decrease in the ferric iron concentration (Fe3+) from 10-15% down to 2-3% resulted in lower solubility of copper in slag, and agitation of the melt with gas stream accelerated. the separation of the sulfide phase and slag. Removal of copper from slag was performed in a pilot unit within the second V anyukov furnace zone where slag arrived with a copper content of 0.8-1.3%. The temperature of molten slag was maintained within 1523 to 1573 K. The copper content of the final slag was at a level of0.12 to 0.14%. The matte sent to converting was a mixture of bottom matte from the smelting zone and the slag treatment zone. It had a copper content of about 50 to 55%. Process gases from both furnace zones were combined and sent to the acid plant for sulfur recovery. This process was offered for commercial use at two copper smelters in Russia and CIS.

Jan 1, 2000

By Keiji Okumura, Hong Lan, Masamichi Sano

"Magnesium has been well known as one of the excellent agent of desulfurization, deoxidation, etc. in iron- and steelmaking because of its high reactivity. Since its production is energy nitensive, the price is very high. Thus magnesium has not widely been used as an agent in metal refining ·processes. In the present work, reduction of magnesia by carbon and aluminum is examined. Because the reaction is very sensitive to temperature, non-isothermal technique is applied to investigate the reaction kinetics. The effects of heating rate .and reaction interface area on the reaction kinetics .are studied. .A kinetic model is proposed based on the experimental results.IntroductionFor the metal refining processes, the production of high purity metal has been one of the most important research subject. In order to produce the high purity metal, the amount of the refining agent and the consumed energy is increasing. Therefore, if the future earth environment is taken into consideration, the further efficient and energy saving processes are required. Generally, Cao slag has mainly been used for desulfurization of molten iron as a desulfurization agent. However, environmental problems, such as recycling of disposal slags, are still unsolved. On the other hand, the deoxidation of molten steel is mainly performed by addition of aluminum. Therefore, the alumina inclusions· remain in. molten steel and the great efforts have been made to the removal of the inclusions. The affinity of magnesium with sulfur and oxygen is strong, and magnesium is well known as a powerful desulfurization and deoxidation agent. However, magnesium has been seldom used for the steel' refining process. The following reasons are considered. Generally, magnesium is expensive. And at iron- and steelmaking temperatures, the refining efficiency becomes low due to its abruptly .evaporation."

Jan 1, 2000

By R. J. Wesely

In recent years the trend in copper smelting has been to expand existing smelters to increase their throughput. New smelters under consideration are large, typically in excess of 200,000 tons per year of copper. Despite this trend to larger smelters there are a number of conditions where a much smaller smelter can be economically viable. This paper examines these conditions and outlines the process concepts for a small smelter treating from 20,000 to 100,000 tons per year of copper.

Jan 1, 2000

By Banqiu Wu, Ramana G. Reddy, Robin D. Rogers

Experimental studies on aluminum recycling via electrolysis in ionic liquids were carried out at the temperature of 105°C. Impure aluminum was dissolved at the anode and pure aluminum was deposited on a copper cathode. The products were characterized using an optical microscope, micro-image analyzer, X-ray diffraction, emission spectrometer, and atomic absorption analyzer. The electrorefining process with a current density of 310 - 730 AJm2, and current efficiency of about 99% was obtained. Impurities such as Si, Cu, Zn, Fe, Mg, Cr, Ni, Mn and Pb were removed as anode residue. Impure aluminum was purified from 79.8wt% to 99.9wt%. At a cell voltage of 1 volt, the energy consumption of about 3 kWh/kg-Al was obtained. The process has advantages of low energy consumption and low pollutant emissions, compared with the current industrial refining process.

Jan 1, 2000

By Keizo Uematsu, Kumiko Sanda, Nozomu Uchida

"Full understanding of mechanical properties is the most important assignment in ceramics. Establishment of defects-property relationship is crucial for fulfilling the assignment. This study reports detailed characteristics of defects and their relevance to the mechanical properties for alumina ceramics made through a typical industrial processing. Novel characterization methods were applied to evaluate their defects. A very simple direct correlation was successfully found between defects and properties in ceramics. This result is a great epoch in the field of ceramics. IntroductionThe ceramic materials are used in refractoriness, corrosion resistant materials and structural materials. The low fracture toughness and scatter of strength are very important problems in ceramics. The toughness of ceramics is lower than metal and polymer materials, and the allowed defect size is small. Very small internal defects (pore, crack, huge particle) can be a fracture origin in the brittle fracture. The characteristics of defects such as size, distribution and shape change markedly by process condition, which cause the scatter of strength. This study conducts quantitative evaluation and direct observation of the sizes, shape and a number of internal defects with a light microscope, and discusses the relationship for mechanical properties and defect sizes"

Jan 1, 2000

By James C. Foley, David K. Rehbein

"In-situ characterizations of green state part density and sintering state have long been desired in the powder metal community. Recent ·advances in non-contact electromagnetic acoustic transducer (EMAT) technology have enabled in-situ evaluations of the acoustic attenuation and velocity as sintering proceeds. Pure aluminum (99.999%) and aluminum alloy powders were prepared with high-pressure gas atomization (HPGA). The powders were pressed in a uniaxial die and examined with acoustic waves for changes in velocity and attenuation during sintering. The changes in acoustic properties were correlated with sample microstructures and mechanical properties. Evolution of the acoustic echo train during sintering is shown to provide information on the state of sintering as well as having the potential for detection of interior flaws.IntroductionThe versatility of powder metalallurgy (PIM) technology in the manufacture of complex shapes has enabled an increasing amount of wrought and casting production capacity to be converted to PIM technology. However, ultrasonic inspection of green components produced using PIM techniques remains a challenge and is not generally practiced [1]. Inspection of PIM components in the green state is highly desirable, because the green part can be reclaimed with only accepted components being subjected to further costly processing. Another potential benefit is characterization and greater understanding of the sintering process itself. An increased scientific understanding of the sintering process enables intelligent process control, greater reliability of the production process and a lower rate of rejection of the finished product. In order to realize these potential benefits, it is necessary therefore that accept/reject criterion be based on real time nondestructive evaluation of the green-state components and the sintering process.Most current nondestructive inspection techniques suffer from their inability to perform inspections below the near-surface region with the exception of X-ray and to some extent pulsed eddy current [2]. X-ray inspection requires extensive shielding of production personnel and expensive film and film processing. While development of pulsed eddy current techniques have lessened the impact of the well-known skin effect, the depth of penetration of the induced eddy currents remains somewhat of an issue [2]."

Jan 1, 2000

By Taiping Lou

The coarsening process of precipitates in non-equilibrium systems was studied, and then a physical model of coarsening was proposed. The coarsening process of CaO'TiO2 in MgO-TiO2-Al2O3-SiO2-CaO-CaF system was investigated. It is shown that the coarsening process by the model predicting is agreed with the experimental results.

Jan 1, 2000

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 Masayuki Kudoh, Kiyotaka Matsuura

"Molten aluminum and nickel cast onto a steel block exothermically react and produce molten nickel monoaluminide, NiAI, which is simultaneously joined to the steel. The heat of the exothermic reaction is transferred to the steel block, and steel near the surface of the block is melted. The depth of the melted steel increases with both the initial temperature of the steel block and the thickness of the produced NiAI. Iron from the melted steel dissolves in the molten NiAI, and an intermetallic compound of NiAI-Fe pseudo-binary system is produced. During solidification of the intermetallic compound, it is strongly joined to the steel. The Ni.Al-Fe intermetallic compound has an excellent resistance to oxidation and corrosion.IntroductionAn intermetallic compound of nickel monoaluminide, NiAl, offers many advantages over conventional superalloys, such as higher melting temperature, lower density, greater specific modulus and higher thermal conductivity [1]. NiAl also exhibits excellent high-temperature oxidation resistance when doped with zirconium or hafnium, and excellent high-temperature corrosion resistance when doped with chromium or yttrium, that are superior to existing high temperature alloys or coating materials [1-4]. On the other hand, NiAI is significantly brittle at temperatures below 600 K [5-7], which is the most sigriificant disadvantage of NiAI. A possible way to overcome the disadvantage and to utilize NiAl as an environmental-resisting high-temperature structural material may be joining of NiAl to a ductile material."

Jan 1, 2000

By Wade L. Karlsen

"Revision surgery to replace joints in the human body requires materials that are strong, long-lasting, and biocompatible. Metallic implants made of cobalt-chromium-molybdenum alloys are already popular because of their proven corrosion and wear resistance properties, but there is an on-going effort to economically improve their performance. Alloying with inert nitrogen can enhance the mechanical properties of the alloy, enhance its corrosion resistance, and elevate the temperature at which the metallic implants can be thermally treated, without increasing the threat to the human body. The current work has produced a high-nitrogen Co-Cr-Mo alloy through HIP consolidation of metal powders that have undergone nitriding in a mechanically fluidized bed. The already fine microstructure of the powders combined with the increased nitrogen content resulted in significant property gains in the consolidated materials.IntroductionMetallic implants made of cobalt-chromium-molybdenum alloys are already popular because of their proven corrosion and wear resistance properties, but there is an ongoing effort to improve their performance. Research on a Stellite 21 cobalt-chromiummolybdenum alloy has shown that nitrogen alloying can be desirable from several standpoints [l]. Firstly, it has indicated that nitrogen can enhance the mechanical properties of the alloy, which could allow more demanding implant designs. The same work also demonstrated that nitrogen can elevate the temperature at which the metallic implants can be thermally treated, which is desirable in situations in which surface textures are to be sintered to the implant to enhance its fixation properties. Finally, that research work discovered that, not only does nitrogen not harm the corrosion resistance of the cobalt-chromium-molybdenum alloys, but it may in fact enhance it. Combining this with the fact that small amounts of nitrogen are not considered a threat to the human body, makes nitrogen alloying an attractive alternative for enhancing the properties of Co-Cr-Mo."

Jan 1, 2000

By T. Goda, H. Kiuchi, M. Iguchi

"IntroductionThe utilization of silver in the electronic industry has been increasing in recent years. It is desirable that valuable metals are recovered from the used scraps of these industrial goods. Condensor chips, for example, contain silver, palladium, and Ag-Pd alloy. The dissolution behavior of silver was studied assuming that scraps such as used condensor chips in which Ag-Pd paste is used are subjected to wet treatment.ExperimentalIn this study the powder, granules, and flakes of silver were used in these nitric acid leaching experiments. The nitric acid solution was agitated in a glass reactor with a magnetic stirrer and heated to the required temperature. The experiment was started by putting the silver sample in the solution. After the leaching, the solution was filtered and the concentration of silver in the filtrate was analyzed by ICP.ResultsIn dilute nitric acid of less than 5 N, silver powder dissolved easily with increase in the concentration of nitric acid and temperature. However, the more intensive the stirring of the solution was, the lower the dissolution quantity became. Fig. 1"

Jan 1, 2000

By Jaroslav Horskoý, Miroslav Raudenský, Bogdan Filipic, Božidar Sader

This paper describes main elements and practical use of the computational system for automated setting of optimized casting conditions in the continuous casting of steel. The system consists of the heat transfer model of the process, empirical metallurgical criteria, and optimization algorithm. The physical model of the, strand temperature distribution relies on the classical Bennon-Incropera mixture continuum formulation for the convective-diffusive heat transport. Fluid flow effects are considered through enhanced thermal conductivity of the liquid phase. The model is solved by the operator-splitting Crank-Nicolson finite volume version of the Voller-Swaminathan scheme. The solution procedure is coupled with the IDS solidification analysis package. Boundary conditions for the strand cooling rely on combination of the generic and plant-specific mold, spray, and roll heat transfer coefficients ' by coping the effects of the casting speed, casting temperature, casting powder, mold oscillation mode, steel grade, water or air-mist spray type, running water, trapped water on the rolls, and radiation. The caster safety and productivity and the quality of the strand are related to nine empirical metallurgical criteria. The criteria ensure the caster safety and economy as well limit the internal, longitudinal, and transversal surface cracking possibility. The problem of finding optimum casting parameter values is stated as a minimization problem based on the analytical form of the cooling criteria evaluated from the steady-state temperature distribution of the strand. To solve the optimization problem, a genetic algorithm is employed. The algorithm explores process parameters settings heuristically by applying the principles of biological evolution. It starts with a random set of solutions and iteratively improves them through selection and variation. Solutions are evaluated by running the heat transfer model of the process and extracting the values of the empirical metallurgical criteria.

Jan 1, 2000

By Toshihide Takenaka, Takashi Matsui, Nao Murakami, Masahiro Kawakami

"Electrowinning of Ti have been investigated in a LiF-NaF-KF melt including K2TiF6 at 773-923K by applying electrochemical oxidation ofH2 gas as an anodic reaction. The cathodic behavior of titanium and the anodic behavior of H2 gas were studied by voltammetry in detail to clarify the electrolytic condition for the process. The electrowinning of Ti was carried out by potentiostatic _electrolysis. Steady electrolysis was achieved under the suitable electrolytic condition without breaking out the anode effect. Titanium metal was electrodeposited on a Ti cathode though the deposits were usually powdery. It is concluded that this process is potential if the morphology of the deposit can be improved.IntroductionTitanium has such good properties as high specific strength and high corrosion resistance. However, the availability of Ti has been limited because the price of Ti is much higher than those of other common metals, such as Fe and Al. The production process of Ti ingot from its ore is rather intricate so that the production cost is high. If the simpler process is developed, the production cost should be retrenched. Titanium metal is usually produced by the Kroll process, which consists of the electrowinning of Mg metal in molten salt and the chemical reduction of TiCl.i by Mg metal. The Kroll process is very elabrate, but not simple. Because the chemical reduction ofTiCl4 by Mg metal is highly exothermic, a considerable amount of energy is wasted.Titanium metal can be electrowon in molten salt bath in principle. A simpler and more effective process than the Kroll process may be realized by the direct electrowinning so that the electrowinning of Ti metal has been studied widely[ 1]. Some researchs progressed to a pilot plant stages [2], but the electrowinning of Ti has not been industrialized yet."

Jan 1, 2000

By Norihiko Fukatsu, Takashi Iwamoto, Noriaki Kurita, Koji Katahira, Kunihiro Koide, Teruo Ohashi

"The galvanic cell-type hydrogen sensor employing CaZro.9Ino.t03-a. as the solid electrolyte was designed for the measurement of hydrogen activities in molten copper under industrial .conditions. The sensor probe consists of the cap-shaped solid electrolyte with porous platinum electrode on the inside and alumina refractory tube. The gas mixture of the composition 4%H2-0.5%02-Ar was made to flow on the inside electrode. The hydrogen sensor probe was inserted directly into molten copper and the melt was used as the outer electrode. The effect of oxygen activity gradient to EMF was eliminated theoretically by measuring the oxygen activity in the melt simultaneously with an oxygen sensor. The high stability of output and excellent response to the change of hydrogen activity were obtained over the wide range of industrial copper melting conditions.IntroductionIn the metal casting process, hydrogen easily dissolves in molten metals from water vapor in the surrounding atmosphere. Owing to the large difference in hydrogen solubility between liquid and solid metal, dissolved hydrogen becomes a cause of the defects of blowholes in castings or ingots. It is necessary to control the hydrogen content in the molten metals [l]. Using proton-conducting ceramics as a solid electrolyte, high temperature-type hydrogen sensor can be constructed [2]. SrCe03- and BaCe03-based perovskite-type oxides exhibit appreciable proton conduction under hydrogen containing atmosphere at high temperature [3-5]. A hydrogen sensor for molten aluminum using CaZro.91no.103-a. has been developed and widely used in the ·process control in the aluminum melting industry [6,7]. The same type of hydrogen sensor has also been expected in the copper melting industry. .. However, CaZro.91no.103-a shows ·not only proton but also oxide ion conduction in the high temperature and at low oxygen activies like the copper melting· conditions. Then we studied the oxide ion conduction in CaZro.91no.103-a. iit · detail [8]. From the consideration on the EMF of the galvanic cell employing this material as electrolyte, it was shown that the unknown hydrogen activity may be precisely determined from cell potential which is corrected for the effect of oxygen potential gradient And the hydrogen sensor based in this principle was constructed and tested in laboratory-scale [9,10]. We repeated the similar tests in factory-scale and developed the sensor system for practical uses [11, 12]. In this report, the structure and system of the hydrogen sensor for molten copper will be introduced first. The reliability of the sensor will then be demonstrated from the results of experiments for sensor probes carried out in TYK's laboratory."

Jan 1, 2000

By Leo Brewer, Kazuyoshi Shimakage, Mamoru Mitomo, Toshiyuki Nishimura, Yoichiro Uemura, Shinji Hirai

"In the synthesis process of ß -La2S3 via the sulfurization of La2O3 powder using CS2 gas, La2O2S was formed. This occurred at an initial stage of the reaction for sulfurization temperatures below 973K, and ß -La2S3 was also formed at a shorter period for higher sulfurization temperatures. It was found that the oxygen content in ß -La2S3 powders decreased gradually with an increase in sulfurization temperature. On the other hand, the carbon content in these powders increased gradually with an increase in the sulfurization temperature. Though it has been reported that ß -La2S3 was transformed to Y -La2S3 at 1723K± 50K, the sintered compact of double-phase Y -La2S3 and ß. -La2S3 was formed at a rather higher temperature of 1973K when the synthetic powder of ß -La2S3 containing a high amount of oxygen was used. However, phase transformation of -La2S3 to Y -La2S3 progressed preferentially with a decrease in the oxygen content of synthetic ß -La2S3 powder. The Seebeck coefficient of the sintered double-phase Y -La2S3 and -La2S3 was higher than that of the single-phase Y -La2S3, reported previously.Introduction La2S3 exists in three polymorphic forms that are similar to a series of Ce2S3, Pr2S3 and Nd2S3: a, ß , and Y'. The a -La2S3, which is stable at low temperature, is irreversibly transformed to ß -La2S3 of various compositions in the solid-solution range between La2S3 and La3S4, at 923 ± 50K. The -La2S3 may also be an oxysulfide of La10S14O2. Moreover, the ß .-La2S3 phase is transformed to Y -La2S3 ,which has a Th3P4 structure, at 1573 ± 100K. The melting point of Y -La2S3 is 2398 ± 30K where this temperature is similar to those of common refractory materials such as silica and alumina. Therefore, it can be predicted that y -La2S3 which has a high melting point and a thermodynamic stability due to the strong affinity of La for S, would have &high refractory character and chemical inertness in many molten metals. The y -La2S3, colored vivid faint yellow is stable up to 623K in air, where oxidation starts. y -La2S3 is frequently used as pigments for plastics and paints3. Furthermore, Y -La2S3 which is a semiconductor, is considered to be useful as a thermoelectric conversion materials, because it has a high Seebeck coefficient."

Jan 1, 2000

By Y. Ide, K. Kishitake

It is expected that an Al-Cr-N composite nitride film may have a higher resistance to oxidation at elevated temperatures than the well-known Ti-Al-N films. The formation conditions of Al-Cr-N films by a de reactive sputtering method and their properties were studied in this study. The films characterized with respect to their high temperature properties such as chemical composition, crystal structure, microhardness, wear and· friction. The crystal structure of the Al-Cr-N films changed from hexagonal phase to cubic phase with an increase in Cr content in the films. The resistivity to thermal oxidation of the Al-Cr-N films is superior to that of usual TI-Al-N films. A half of the friction coefficient in the Al-Cr-N film was obtained comparing with that in the ordinary TI-Al-N film at room temperature and the wear rate of Al-Cr-N film was 2 order smaller than that of TI-Al-N film. The Al-Cr-N films show a small friction coefficient at 500°C and then they are recognized to have good tribological characteristics.

Jan 1, 2000