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By R. L. Nyirenda

One of the problems with ammoniacal-ammonium carbonate leaching of EAF carbon steelmaking flue dust is that zinc present in spinel phases is not leached. This paper presents results of test work in which prior to leaching, EAF dust was reduced with CO containing gas to decompose the spinels into zinc oxide and iron bearing phases, mainly metallic iron and wustite. From such reduction products, the amount of zinc leached increases but the iron co-leached becomes extensive. The effect of various leaching parameters such as liquor concentration and redox potential on zinc and iron dissolution has been investigated. Supplementary experiments utilizing pure zinc oxide and pure iron phases were also carried out. Results show that the co-dissolution of iron from severely reduced EAF dust cannot be prevented. This is because the wustite phase contains zinc which can only be leached when iron also dissolves. Further, the zinc bearing wustite phase is not totally soluble so that the residue cannot be made zinc free. In the absence of air, dissolution of metallic iron hardly occurred, though in leaching experiments of a long duration its transformation to a spinel structure was observed.

Jan 1, 1992

By Xiaolong Bi, Shaohua Luo, Longjiao Chang, Shiyuan Cao, Jianan Liu

iliary agent was proposed. The mineralogical transformation and silicon extraction kinetics of laterite nickel ore in alkaline hydrothermal treatment were studied. The effects of reaction temperature (175 ~ 250℃), molar ratios of sodium hydroxide to ore (1.05 ~ 1.2:1), and laterite nickel ore particle size (44 ~ 178 μm) on the extraction ratio of silica were investigated by using the shrinking core model. The results show that the extraction ratio of silica increases with the increase of reaction temperature, sodium hydroxide to ore molar ratio, reaction time, and the decrease of raw ore particle size. The kinetic analysis shows that the separation of silica in laterite ore can be described by internal diffusion model. The apparent activation energy (Ea) of the reaction was 8.87 kJ mol− 1, and the kinetic modeling was established.

Dec 2, 2021

By M. M. Fine

This report presents the results of laboratory mineral-dressing investigations by the Bureau of Mines of 14 individual or composite character samples from deposits in the Batesville manganese district. It will be noted that some concentrates have met or approached analytical specifications for metallurgical manganese ore although great variations in both physical and chemical composition from once deposit to another make each a new problem. In most cases it is evident that a substantial loss of manganese has occurred in the various slime and tailing products. An important aspect of this work is the research being conducted on manganese-bearing limestones. Recent reconnaissance indicates that this resource constitutes one of the major domestic reserves of manganese. Laboratory study has shown that ferrograde concentrates can be recovered from samples of manganese-bearing limestones from two properties. Research on samples from other areas is still underway.

Jan 1, 1957

By G. L. Oldright, Virgil Miller

"This paper is the tenth 4 of a series on smelting in the lead blast furnace, and the fifth 5 on modifications brought about by the introduction of richer charges.ACKNOWLEDGMENTSAll of the data on handling rich charges in lead smelting given in this recent set of five articles describing the results of a cooperative study by the United States Bureau of Mines and the University of Utah were obtained through the courtesy and with the cooperation of the staff of the Bunker Hill & Sullivan Mining & Concentrating Co. at Kellogg, Idaho. The authors acknowledge with appreciation the assistance given by Stanly A. Easton, vice.-president and general manager, F. M. Smith, smelter director, and A. F. Beasley, smelter superintendent, whose generosity, sympathy, and assistance made it possible to obtain this information for the mining industry.GENERAL DISCUSSIONWhen the charge has been dropped into the lead blast furnace, it is out of control of the operator to the extent that, whatever the material is, it must practically all be melted and run out of the blast furnace. The necessary uniformity of mixture to produce slags of regular composition and the choice of the slag—forming ingredients and products to be formed can be made only before the charge to dropped.It was found (R.I. 3096) at Kellogg, where the charge is mostly sinter, that the ratio of the slag—forming ingredients taken from each tuyere was nearly constant, in contrast to the irregular composition of slags taken similarly from a furnace whose charge consisted of ingredients differing greatly in chemical and physical nature, including size. If the charge consists almost entirely of sinter, the blast furnace should then operate more uniformly."

Aug 1, 1932

On account of the increased work required from the assay office, owing to the large additions which have been made to the smelting and superphosphate plants during the last few years, it was found necessary to build a more extensive and up-to-date assay office than the one that had been in use since the starting of the works some twenty years back.A site was chosen adjacent to the main office, so as to be free from smoke and dust.. The building is constructed of red brick, the over-all dimensions being 109 ft. x 37 ft. The roof is of fibrous-cement slates, 31 ft. high, with a two-to-one rise, and overlaps the walls to the extent of 4 ft. 6 in. on all sides.Special care was taken to give light to all working benches, fume cupboards, and balance rooms. The main chemical room occupies the entire western end of the building, and the fire room the entire eastem end. Between these two rooms are the superphosphate, refinery, and gold-parting rooms on one side of the central passage, and three balance rooms, general office, and cloak room on the other side. The height of the roof affords ample space above these central rooms for storage purposes, and also maintains a fairly even temperature. The ceiling of the main chemical and fire rooms is carried immediately under the slates, which gives a total height in the centre of about 25 ft.

Jan 1, 1918

By Antoine Allanore, Luis A. Ortiz, Donald R. Sadoway

"The steelmaking industry has drastically reduced its energy consumption in the last fifty years, and today’s technologies are considered to operate at their optimal efficiency with respect to energy needs. To cope with new constraints related to greenhouse gas (GHG) emissions, a change of paradigm is necessary. One of the promising technologies that could be deployed to help reach CO2 mitigation targets relies on the intensive use of electricity: molten oxide electrolysis (MOE). This paper presents the key process parameters that need to be tuned to address the practical needs for both high productivity in a steelmaking reactor and for an energy efficient process. Herein we show that contrary to common perception, the electrolysis process for ironmaking requires less energy than today’s chemical reduction route. Furthermore, we prove that most of the energy that must be provided to operate the electrolytic iron production cell is thermal energy which is readily generated by joule heating during electrolysis due to large currents being passed through the electrolyte. The energy consumption of the electrolysis cell is therefore shown to be highly dependent on the cell configuration and the chemistry of the electrolyte. As a consequence, the CO2-impact of the technology strongly depends on both the power production mode and the technological choices for design of the process, including cell configuration. Surprisingly enough, even when the electricity generation is not carbon-free, MOE still appears to be viable from the perspective of reducing GHG emissions providing sound reactor design considerations are made.IntroductionIn the context of greenhouse gas (GHG) emissions mitigation, the steelmaking industry is considering several techniques that could sustain the efforts and progress achieved by this sector in the last decades [1]. A recent report [2] on potential routes for low-CO2 steelmaking highlighted for all techniques both the strong dependency of CO2 emissions on electric power production mode and the need for a decrease in energy consumption per tonne of steel. Incited to innovate with respect to this last criterion, the steel industry considers electrolysis to be a promising technological solution, and in particular the molten oxide electrolysis (MOE) process. This process conducts electrolysis in a mixture of oxides that dissolve the iron oxide feed, which by the action of electric current is decomposed into liquid iron and oxygen gas. The opportunity for reduction in energy consumption during steelmaking by MOE is commonly attributed to the “direct” pathway from iron oxide to liquid metal offered by the use of a molten oxide melt and operation at a temperature above the melting point of iron, ideally 1600°C, to provide enough superheat for tapping the molten iron product:"

Jan 1, 2011

By D. W. Lillie

It has been demonstrated that considerable bend ductility exists in bulk specimens of polycrystalline high-purity silicon. The possibility of hot-forming at 1200°C is suggested. EXCELLENT corrosion resistance in many media and low cross section for absorption of thermal neutrons (0.13 barn) would make silicon of interest to nuclear engineers were it not for extreme brittle-ness and the difficulty of fabrication by any reasonable means. The use of silicon for structural purposes also has been considered in view of its light weight and oxidation resistance. Johnson and Han-sen' have investigated the properties of silicon-base alloys and concluded that there was no way of making pure silicon or silicon-rich alloys ductile at room temperature. In view of reports of appreciable ductility in germanium single crystals above 550°C'." and some plastic deformation in single-crystal silicon above 900oC,' the present investigation was undertaken to define more precisely the limits of high-temperature ductility in pure silicon. After this investigation was begun torsion ductility in both germanium and silicon was reported by Greiner." Through the courtesy of F. H. Horn, a small bar of cast extra high-purity silicon was obtained and small bend specimens were made from it by careful machining and grinding. All of the reported tests results were obtained from samples from this bar (bar No. 1) and one other of similar source (bar No. 2). No complete analysis was obtained but, based on analysis of similar semi-conductor grade material, metallic impurities were under 0.01 pct total. Vacuum-fusion analysis for oxygen showed a value of 0.0018 2 0.0003 pct for the first bar tested and metallographic analysis showed no evidence of a second phase. Bend tests were carried out on an Instron tensile machine using a bend fixture with a 1 -in. span loaded at the center. Supporting and loading bars were 0.250 in. round and the load was applied by downward motion of the pulling crosshead of the machine. Specimen thickness and width were approximately 0.10 in. and % in. respectively. Loading rate was controlled by holding crosshead motion constant at 0.02 ipm. In some cases a smaller specimen was used on a 5/8-in. span with a 0.129-in.-diam loading bar. The entire bend fixture was surrounded by a hinged furnace and all heating was done in air atmosphere. Temperature measurement was made with thermocouples fastened directly to the bend fixture within less than 1 in. from the specimen. Autographic stress-strain curves were recorded during each test, and breaking load, total deflection, and plastic strain could be obtained from these curves. Stress was calculated from the beam formula S = 3PL/2bh2, where P is the load in pounds, L the span in inches, b the specimen width in inches, and h the specimen thickness in inches. This formula is strictly correct only in the elastic range but has been used to calculate a nominal stress for convenience in the plastic range. The stress given is the maximum stress in the specimen. Results The results of the complete series of tests are shown in Table I. The first group of tests (specimens Nos. 1-6) showed the beginning of plastic flow at a test temperature of 900°C, so two additional tests (Nos. 8 and 9) were made at 950°C on small-size specimens from bar No. 2. Specimen No. 8 was tested in the as-machined condition, and No. 9 was heat-treated in hydrogen at 1300°C for 2 hr, cooled to 1200°C and held 1 hr, cooled to 1000°C and held 1 hr, cooled to 900°C and held 1 hr, and finally cooled to a low temperature before removal from the hydrogen. It is apparent that the heat-treatment had a significant effect on yield strength and ductility. In addition, the magnitude of the yield point was conslderably reduced in the heat-treated specimen as is shown m Fig. 1 by tracings of the stress-strain curves. After obtaining a furnace capable of reaching higher temperatures specimens Nos. 10 to 13 were tested at 1100 and 1200°C. Strain rate was increased by up to a factor of 10 to see whether the ductility observed was excessively strain sensitive. Specimen NO. 10, strained at 0.02 ipm and 1100oC, was still bending at a deflection of 0.322 in. when the load rate was increased to 0.2 ipm, resulting in immediate

Jan 1, 1959

By C. W. JEFFERS

During the past few years the use of mechanical equipment for the loading and transportation of coal at the working face has rapidly increased . Many mining officials are of the opinion that mechanical methods have tended to reduce the hazards of mining, and a number of statements have been made to this effect . Little actual data upon which to base conclusions in regard to the relative safety of various methods of mining have been made available . While it may be possible that these systems of mechanical mining are inherently less hazardous , obvious dangers should not be disregarded in the belief that the mere act of installing mechanical loading equipment automatically brings about better accident records . The same rules and regulations , modified to meet the new regime must be applied with the same discipline as heretofore . By diligent study and application there is reason to believe that new methods of concentrated mining can be utilized with at least a possibility of increased accident performance . With the idea of preventing accidents by taking available precautions against their occurrence , attention should be directed to the dangers that exist where room and face conveyors are in operation . Due to the cost pressure prevalent in the mining industry at the present time mechanical means are often used in an attempt to decrease cost of production. The management , after having spent considerable sums of money for new equipment , is expected by stockholders and investors to show results by increasing tonnage and reducing operating costs . Consequently the operating officials apply the same pressure to local mine officials to obtain results . The natural reaction of the superintendent and mine foreman is to secure the maximum production from the new method , and unfortunately safety is frequently , if not generally , sacrificed to this end . In many instances , operators of new types of mechanical loaders are difficult to secure and after being obtained are difficult to hold , especially if the new equipment is more or less in the experimental stage . The tendency is to handle the machine operators with " gloved hands " and to permit many unsafe practices which ordinarily would not be allowed, in order to keep from antagonizing them and losing their services . Although these unsafe practices become habitual and even uneconomical , conditions thus established are difficult , sometimes impossible , to change .

Jul 1, 1930

By Karl J. Benecke

Though the first patent on a bucket wheel excavator (BWE) was granted in 1881 in the US, this technology was developed in Germany to the high standards of today. However, this development was only possible in parallel with development of shiftable belt conveyors and boom stackers. The combination of these three types of equipment in the open pits of the Federal Republic of Germany has made lignite the cheapest energy source for power generation, despite the low heating value of German lignite on the order of 8500 kJ/kg (3600 Btu/lb) only. Comparing the costs for fuels used in power generating on the basis of their heating value, the relation between lignite, high quality black coal, and imported crude oil is on the order of 1 to 1.5 to 2.5, hence highly in favour of lignite. These cost advantages for lignite in Germany are due mainly to the concentration of lignite mining in a few high-output mines. The largest one, Fortuna mine in the Cologne district, produced a total of 45 million tons of lignite in 1976. That equals the annual fuel need of a 5750 MW power plant running 7000 hours per year at full capacity. Altogether 95.2 million bank m3 equal to 200 million tons of overburden had to be removed to accomplish this lignite output. The largest BWE ever built is working in the Fortuna mine [(Fig. 1)]. At a digging height of 51 m above crawler level, the total vertical reach in relation to the face conveyor level is 98 m by means of its conveying bridge and loading unit. The hourly output is 10 400 bank m3. Its weight in operation is 13 000 tons and its wheel diameter 21.6 m, as high as a seven-story building. Major reasons for the development of BWE technology in Germany were: ? Lignite deposits with moderately consolidated, alluvial-type overburden (gravel, sand, loam, marl, clay, etc.) ? Great overall depth of the deposits, ranging far beyond 100 m, requiring a wide opening of the mine, hence not permitting direct overcasting of overburden. ? Multiple-seam deposits of poor-quality coal divided by reject partings, which demand a perfectly selective digging tool for clean separation. In general, these conditions are almost identical to those prevailing in the lignite deposits of Texas and neighbouring states: The type of overburden suitable for BWE digging, the overall deposit depth ranges down to around 100 m, and finally, the multi-seam occurrence with partings between seams, the latter ranging from just 1 m to a few meters in thickness. Technique As the Texas-type lignite deposits come into focus more and more as a possible fuel source in power plants to replace natural gas and crude oil, the following will deal with the BWE technology for mining a typical Texas lignite deposit under the aspect of producing enough fuel for a 500-MW power plant located at the mine mouth.

Jan 1, 1980

By S. S. Babu, T. Hong, T. DebRoy, S. A. David

"Oxide inclusions form in welds because of deoxidation reactions in the weld pool. These inclusions control the weld microstructure development. Thermodynamic and kinetic calculation of oxidation reaction can describe inclusion characteristics such as number density, size, and composition. Experimental work has shown that fluid-flow velocity gradients in the weld pool can accelerate inclusion growth by collision and coalescence. Moreover, fluid flow in welds can transport inclusions to different temperature regions that may lead to repeated dissolution and growth of inclusions. These phenomena are being studied with the help of computational coupled heat transfer, fluid-flow, thermodynamic, and kinetic models. The results show that the inclusion formation in steel welds can be described as a function of the welding processes, process parameters, and steel composition.IntroductionThe relationship between inclusions and formation of a high-toughness phase, namely acicular ferrite in low-alloy steel welds, is well known (1-4). Past research has focused on maximizing acicular ferrite amount in welds by controlling welding processes, process variables, and welding consumable parameters. Research has shown that there is a complex interaction between inclusion characteristics, prior austenite grain size, and weld metal hardenability. In a low-alloy steel weld, the small addition of titanium lead to a change in the inclusion composition and resulted in a transition in the microstructure from bainitic to acicular ferrite [see Fig. I]. This in turn lead to the best combination of strength and toughness. This paper describes the inclusion formation in low-alloy steel welds."

Jan 1, 1999

By Dong Joon Min, Joo Hyun Park, Mi Sun Choi, Jae Hong Shin

Sublimation of ZrCl4 is important for the production of nuclear grade metallic Zr in Kroll’s process. The sublimation kinetics of ZrCl4 was investigated by TGA under both isothermal and non-isothermal conditions. The sublimation rate of ZrCl4 increased with increasing temperature under isothermal conditions. ZrCl4 sublimation was confirmed to be a zero-order process under isothermal conditions, whereas it was first-order kinetics under non-isothermal conditions. The activation energy of ZrCl4 sublimation under isothermal conditions was 21.7 kJ/mol. The activation energy for non-isothermal sublimation was 101.4 kJ/mol and 108.1 kJ/mol with the Kissinger method and Flynn- Wall-Ozawa method, respectively. These non-isothermal activation energies were very close to the heat of sublimation (103.3 kJ/mol). Sublimation occurs by two elementary steps: surface reaction and desorption. Therefore, the overall activation energy of ZrCl4 sublimation is 104.8(±3.4) kJ/mol. The activation energy of the surface reaction and desorption steps are proposed to be 83.1 kJ/mol and 21.7 kJ/mol, respectively.

Jan 1, 2014

By Floyd G. Anderson

Bureau of Mines studies show than an electronic counter can be used for determining just concentrations from midget impinger samples collected in bituminous coal mines. A sample correlation coefficient of 0.91 for data obtained using the electronic counter and the Bureau of Mines microprojector procedures indicates a significant linear relationship between the methods. The electronic counter provides better counting precision and reduces analytical time.

Jan 1, 1968

By Walter G. Brusey

This paper describes a comprehensive pile test program conducted at John F. Kennedy International Airport (JFKIA) to evaluate pile types and design capacities ranging from 890 to 4450 KN (100 to 500 tons). Driven cased piles and drilled shafts, both standard construction and post-grouted after installation, were tested with platform loads extending to 8900 KN (1,000 tons). Alternate load test procedures were developed, extensive structural integrity testing and dynamic load tests were performed on selected shafts. A brief update is provided covering the application of results of the test program to pile selection for support of major structures incorporated in the on going redevelopment of JFKIA.

Jan 1, 2000

By Chulgi Suk, Hoon Park, Hyonsoo Kim, Hakman Kim, Sangho Cho

Dust emission from blast demolition and other construction activities can be a nuisance; it is widely recognized that fine particles less than 10 µm in equivalent diameter (called PM10) may cause health problems. Mist spray systems, such as rain guns, sprinklers, water/surfactant sprays (or foams) etc., are some of the most effective dust suppression methods. A large amount of research has showed that when water droplets are produced in an equal amount to that of dust particles, the airborne dust is suppressed by the agglomeration of dust and mist particles. A method for generating micro-sized mist from water, achieved by the detonation of explosives in the water tube, was suggested and is called the ‘detonationdriven water bag burst system’. There are many experimentally observed limitations of the explosioninduced water break-up process. The water bag explosion tests were simulated using the AUTODYN software, in order to investigate the aerosolization mechanisms of the detonation-driven water and water break-up process into micron-sized droplets. As a result of the numerical analyses, the diffusion direction of water when detonating in the central interior part of water tube was radioactive and significantly stronger than when detonating in the bottom exterior part; this is due to the compressive flow of the volume change inside of the water tube, which resulted from the blasting wave inside of the tube, as well as the reflected pressure on the ground. Blast tests of full-scaled reinforced concrete columns were conducted to verify the effectiveness of the suggested detonation-driven water bag burst system. The water breakdown and dispersion that occurred while blasting the reinforced concrete columns were observed using a high-speed camera, and dust generation was monitored using four density detectors. The suggested detonation-driven water bag burst system showed that the average dust density decreased by up to 7 mg/m3.

Jan 1, 2016

By Frank E. Cash

Published or available data on safety in quarries are few except those pertaining to blasting issued by manufacturers of explosives. During the past 25 years the quarrying industry (including various types of quarries producing many different materials) has had a markedly improved accident experience. The downward trend has not been phenomenal or has it been uniform from year to year, owing to occasional major disasters; but from the information at hand it appears that improvement during the 25-year period has been definite.

Jan 1, 1941

By W. L. Fink, H. C. Stumpf, L. A. Willey

VERY few studies of the aluminum-sodium system have been reported. Heycock and Neville1 were unable to detect any solubility of sodium in liquid aluminum. Mathewson2 prepared an equilibrium diagram consisting of two horizontal lines at the melting points of the two metals. He was unable to detect solubility at either end of the system. Scheuer3 first developed a method for the chemical determination of sodium in aluminum and then studied the solubility of sodium in liquid aluminum. His method involved heating aluminum with excess sodium under hydrogen until the two liquids were at equilibrium, chilling the melt, and analyzing the aluminum-rich layer. He reported the solubility to be 0.l0 pct sodium at 700°C, 0.115 pct at 750°C, and 0.128 pct at 800°C. This paper on the aluminum-sodium system is the twenty-first in a series from the Aluminum Research Laboratories describing equilibrium relations in aluminum alloy systems. MATERIALS The alloys for this investigation were prepared from electrolytically refined aluminum (99.99 pct) and sodium of reagent quality conforming to specifications of the American Chemical Society.4 Chemical analysis of the aluminum showed the following impurities: 0.002 pct Si, 0.002 pct Fe, 0.002 pct Cu, <0.001 pct Mn, 0.002 pct Mg and 0.001 pct Na. The sodium content of all alloys was determined by either chemical or spectrographic standard procedures5 No. IIA and No. SII respectively. DETERMINATION OF LIQUIDUS The boundary of the miscibility gap was determined by a modification of the method of Scheuer3 and of that used by Henry and Cordiano.6 As finally developed the method was as follows: A fused alumina crucible 25 mm id with 75 mm depth and 1.5 mm wall thickness was placed on the bottom of a container made from a 4-in. length of 1 ½ -in. iron pipe and pipe caps. The space around the sides of the crucible was filled with 40 mesh crystalline alundum. A charge of 60 g of aluminum and 10 to 15 g of sodium was placed in the crucible, the sodium first being trimmed and rinsed with iso-pentane to remove kerosene. The container was tightly capped, filled with argon (99.6 pct pure), and heated to the desired temperature (between 670 and 800°C). A positive pressure of argon (about 8 mm of mercury) was maintained through a small pipe to the upper cap. After soaking for from 2 to 5 hr, the container was quenched by directing a stream of water onto the base, so that solidification of the aluminum-rich layer was rapid and essentially unidirectional. Analyses were made on drillings taken from the bottom of the ingots after machining off the surface layers. Pre-

Jan 1, 1948

By H. Sevim

Three transportation and handling alternatives for delivering dry coal combustion residues from power plants to underground coal mines were evaluated technically and economically. The objective was to transport, handle, and inject the residues into the old workings of the mine at a minimum cost. This objective was accomplished in two steps: I) Simulation models were developed and utilized in identifying technically feasible designs in each alternative, 2) Technically feasible designs were economically evaluated to obtain the cost-per-ton of material transported. The designs that provided the minimum cost-per-ton were declared optimal An analysis was conducted for varying distances and tonnages to reveal favorable operating ranges of each alternative.

Jan 1, 1996

By Edward L. Burwell

The Bureau of Mines investigated the use of dilute polymer in brine solutions to increase the efficiency of air in gas flooding model oil reservoirs. Slugs (0.23 pore volume) of 500 ppm polyacrylamide were injected into a model, consisting of a high- and a low-permeability core, that had been previously gas flooded to residual oil. Gas flooding was then resumed. Of the total gas volume injected, the percentage entering the high-permeability zone was greatly reduced after polymer injection but remained unchanged when slugs of water without polymer were used.

Jan 1, 1970

By T. H. Ramsey, Richard Shield

A process has been developed for fabricating thin-film resistors that are compatible with integrated circuits. Films are produced by evaporation of single refractory metals using an electron beam heating source. Resistor paths are then made using standard photoresist etching techniques. A low-temperature coefficient of resistance is obtained by control of nucleation during deposition of the film. One application of the process has been the development of a discrete resistor used for current setting in linear integrated circuits. Multiple thin-film resistors were formed on oxidized silicon substrates using molybdenum metal as a source. An evaporated protective layer of SiO2 over the resistor prevents resistance changes which might occur during subsequent high-temperature processing. Properties of a typical resistor are as follows: R = 15.7 ohm per sq, tolerance surface dimensions = 0.028 by 0.028 in., stable after 4000 hr at 0. 75 w without heat sink. THIN-FILM resistors have been investigated for many years with a large selection of usable resistors resulting from a wide variety of materials. Many of the processes necessitate a high degree of complexity but in nearly all cases the conclusions have been that the materials used in each case were acceptable provided the deposition process was reproducible and could be controlled sufficiently to give the required tolerances. It is our opinion that simplicity is still the key to thin-film resistor fabrication. In this regard, the single metal is obviously the simplest process to control, provided all the necessary properties can be obtained. The idea is not original in this laboratory by any means. Others have taken this approach.&apos; It has been demonstrated that a fairly wide range of resistivities can be obtained by careful control of deposition parameters for any given metal, and by selection of several single metals a very broad range of stable resistors can be obtained. The transition from one metal to the next is made when a film becomes too thin for adequate process control or long-term stability. A great deal of emphasis is once again being placed on the thin-film resistor. Although they have been thoroughly studied in the past, new applications have been found that require the properties obtainable only from thin-film resistors. Integrated circuits, in general, are advancing toward higher speeds and radiation environments which require replacement of the present diffused resistors. Linear circuits in particular are requiring high-power, high-precision resistors for the more advanced applications. The particular requirements of some linear circuits are such that a discrete resistor is required. The resistor described in this paper was developed as a 15.7-ohm precision discrete resistor for use in a current regulating circuit requiring a +2 pct end of life overall tolerance, a dissipation of 750 mw, and the ability to operate over a fairly broad temperature range (i.e., a low temperature coefficient of resistance, TCR). State-of-the-art integrated circuit and silicon processing technology lends itself well to the fabrication of thin-film resistors. Not only is the resistor thin film well-suited to integration on individual circuits, but the oxidized silicon surface provides one of

Jan 1, 1969

By S. M. Purdy

Under certain conditions of hot rolling and air cooling from the hot-rolling temperature, bars of a high carbon (0.40 pct C) chrome-nickel austen-itic alloy were found to show magnetism even though no ferrite or martensite could be detected by microscopic or X-yay methods. The appearance of magnetism in such alloys may come from chromium impoverishment of the austenite grains near the precipitated carbide particles. SPORADICALLY, hot-rolled bars of Silchrome 10, an exhaust valve steel, have been found to be magnetic. Because of the analysis of the alloy—0.40 pct C, 18 pct Cr, 8 pct Ni, 3 pct Si —magnetism is unexpected. Preliminary investigation showed neither martensite nor ferrite to be present; only austenite and Cr23C6. Since a literature search was fruitless, a brief study was made of the appearance of magnetism in this alloy. The only basic difference between the two heats is the nitrogen content. Permeability was measured using a Severn magnetic gauge. This instrument consists of a magnet mounted on a counterbalanced arm. A set of calibrated plugs is placed in contact with one pole of the magnet. The specimen is placed close to the other pole of the magnet. If the specimen pulls the magnet away from the plug, it has a permeability greater than that marked on the plug. This technique is swift and reproducible. Previous experience has shown that the permeabilities obtained corresponded to those obtained on a permeater with a field strength of 100 oe. Specimens from both heats were annealed at temperatures between 1700 and 2300°F. One set of specimens was water cooled and another furnace cooled. All the water-quenched specimens were non-magnetic; the furnace cooled ones were magnetic as shown in Table I with no difference being observed between the two heats. Microstructural examination of the specimens showed the expected increase in carbon solubility with increasing temperature. Carbide solution was complete at 2200°F. The specimens heated to 1900°F or below showed some carbide precipitation from the hot-rolled structure. A furnace cooled specimen from a given temperature showed less carbide out of solution than the water-quenched specimen from the next temperature below; e.g., the specimen furnace cooled from 2100°F showed less carbide out of solution than the water-quenched specimen from 2000" F. These studies indicated that the appearance of magnetism was not related to the quantity of carbon in or out of solution and it was related to precipitation at temperatures below 1700" F. A set of samples annealed and water-quenched from 2100° F was aged for 4 hr at temperatures between 1000" and 1600°F; all were non-magnetic. A second set of samples, similarly annealed, was aged 1 to 24 hr at 1200°F with the results shown in Table II. None of the latter set of specimens showed magnetism until they had been aged about 8 hr. Magnetism was quite strong after aging 24 hr. X-ray diffraction studies on several of the magnetic specimens showed that the austenite had a lattice parameter of 3.58A and that the carbide was Cr23C6. Several of these samples were electrolytically digested in 10 pct HCl in ethanol, with a current density of 0.1 amp per sq cm. None of the particles in the residue were magnetic. Accidentally, one cell was run at 1 amp per sq cm; e.g., magnetic particles were found in this residue. After careful separation, the magnetic particles were mounted on a quartz fiber and their diffraction pattern determined using a 5.73-in. Debye-Sherrer camera with CrK radiation. These particles showed a fcc structure with a lattice parameter of 3.57A. Prolonged exposure, up to 16 hr, produced no other lines on the film. The following facts seemed to be established at this time: 1) Austenite was the magnetic phase. 2) Neither ferrite nor martensite could be detected. 3) Magnetization could be produced by aging at 1200°F. One explanation of these data is that the carbide precipitation impoverishes the region immediately around the carbide particle of carbon and chromium and increases the proportion of nickel. All of these serve to increase the Curie temperature of the region around the carbide particle. If the composition change is enough, the Curie temperature will rise above room temperature. If the volume of the affected region is great enough, the magnetism will become detectable. At low aging temperatures, composition changes are great enough but the overall volume of impoverishment is quite small

Jan 1, 1962