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By Eugene S. Meieran

The effects of methods of crystal growing, wafer sawing, polishing, routine handling, diffusion, and epitaxial growth on the defects in GaAs are reviewed and studied using reflection and transmission X-ray topographic techniques. In general, it was found that boat-grown crystals exhibited fewer defects than Czochralski crystals, although all crystals showed large numbers of precipitates visible when examined in the electron microscope. Mechanical surface treatments such as sawing and mechanical polishing introduce damage to a depth of about 5 µ, most of which can be removed by suitable chemical or chem-mechanical polishing. In addition, defects can be introduced through routine handling of wafers, for example with metallic tweezers. These defects can be quite severe, and have been observed 20 µ below the wafer surface. Defects can also be introduced through diffusion and epitaxial growth. These defects, which include precipitates, growth pyramids, stacking faults, dislocations, and so forth, can be detrimental to device fabrication. It is shown that wafers or films which appear defect-free optically can contain defects visible in the X-ray topographs. WHILE the use of GaAs in the semiconductor industry has increased very rapidly in the last few years, due mainly to the recent development of many important GaAs devices,1,2 the major limit to the production of commercial quantities of many GaAs devices remains a severe lack of suitable materials technology. This lack is apparent in two critical areas. First, production quantities of high-quality GaAs crystals, reproducibly doped and precipitate-free, simply are not available commercially, although some reasonable quality material is available on a limited first-come, first-serve basis. Second, in comparison to silicon technology, little is known about the effects of processing variables on the defects either present in as-grown GaAs or introduced through processing and handling of wafers. These areas are now receiving some attention from semiconductor device manufacturers, who are studying defects in GaAs in order to better understand how either to prevent their occurrence or to cope with their existence. Most investigations of the defects in GaAs have been made by optical microscopy3-5 or transmission electron microscopy techniques.'-' Recently, however, the imaging techniques of X-ray topography, electron mi-croprobe analysis, and scanning electron microscopy are being applied to the study of GaAs.9-14 In the case of X-ray topography, a one-to-one image is obtained that must be photographically enlarged. In compensa- tion, the defects within entire wafers may be imaged by simple scanning (Lang technique15) if the wafer is reasonably perfect, or by using the scan oscillation technique developed by Schwuttke16 if the wafer is warped or distorted. The purpose of this paper is to both review and extend the general application of X-ray topographic techniques to GaAs. Emphasis will be placed on the effects of growth and process variables on the quality and perfection of both bulk and epitaxial GaAs. Reference to optical or electron microscopy results will be made when useful. Since the effects on defects of a wide variety of processing variables such as crystal growing, sawing, polishing, diffusion, and epitaxial growth will be somewhat superficially reviewed, a fairly extensive bibliography of the most important recent results in these areas is included. However, for completeness, important defects will be illustrated here, although such defects have been previously shown by others. While this paper is concerned with defects rather than with the physics of X-ray scattering, the mechanisms of contrast formation in the topographs will of necessity be briefly mentioned. EXPERIMENTAL GaAs crystals, both boat-grown18 and Czochralski-grown,'8 containing a variety of dopants of various concentrations, were purchased from outside vendors. Wafers were sliced from the crystals using a Hamco ID saw and were mechanically polished using 1 µ diamond paste. Chem-mechanical polishing was done in bromine-methanol as described by Sullivan and Kolb.18 Chemical polishing was done using a modified sulfuric-peroxide solution, 11 parts H2SO4, 1 part 30 pct H2O2, 1 part DI water.5 Zinc diffusion was carried out in a closed tube, using a 10 pct Zn-In source at 825°C for 1 hr. Oxide masking techniques were used to select the area to be diffused. Epitaxial wafers were either purchased or prepared here. All epitaxial runs prepared here were carried out using a Ga-GaAs-AsC13 source in a closed tube at a substrate temperature of 750°C. Wafers were chem-mechanically polished and gas-etched prior to deposition. The X-ray topographs were taken on a Krystallos Lang camera, operating in the transmission scanning geometry (Lang technique15) or in the reflection scanning geometry (modified Berg-Barrett technique20,21). MoKa, radiation was used for all transmission topographs using a Jarrell-Ash 100-µ spot focus. CuKal radiation was used for all reflection topographs using a General Electric CA-7 1-mm spot focus X- ray tube. Topographs were printed from an intermediate contrast inversion film, so the contrast shown in all figures here is the same as that of the original 50-µ-thick emulsion L4 Iiford nuclear plate used to record the topograph.

Jan 1, 1969

By J. J. Beeson

The second part of the paper includes a detailed account of the processes of secondary-enrichment which have been effective in producing the disseminated ores. While both parts present new features, it is hoped that the discussion on secondary chalcopyrite and bornite may be of interest to those who are engaged in the study of secondary processes in other districts. The excellent work' Economic Geology of the Bingham Mining District, by J. M. Boutwell, was published in 1905. Since that time the extensive development work-surface cuts and underground drifting-of the Utah Copper Co. has made possible the collecting of samples for more detailed microscopic study. The writer has taken advantage of this fact and presents the following work, not as a criticism, but as a' continuation of the work which was begun by Mr. Boutwell. b. Acknowledgments.-The present study was undertaken at the suggestion of Dr. A. F. Rogers; to him, and to Prof. C. F. Tolman and Prof. S. W. Young, the writer wishes to express his thanks for criticism in the preparation of this paper. The writer also expresses his thanks to D. C. Jackling, Vice-President and Managing Director of the Utah Copper Co., for permission to publish this paper, and to William Spencer, D. W. Wadleigh, T. S. Carnahan, J. A. Caulfield, Percy Dayer, and Edward Norsefall, for the courtesies extended to him while a co-worker in the mines.

Jan 11, 1915

By R. J. Anderson

Roughly, a crack in a casting may be considered, for the moment, to be due to fracture of the alloy resulting from the stress set up by the contraction in volume on passing from the liquid to the solid state. Cracks may be external or surface, internal or deep-seated, or incipient or so-called strain cracks. Draws may appear as depressions, unevenness, and "pinching in" of the surface of a casting. Roughly, draws are due to contraction in volume and are governed largely by the same factors as cracks. A casting may be cracked, however, without being drawn. Shrinkage is a foundry term and refers to the contractio~l in volume of a metal or alloy on passing from the liquid to the solid state. Patternmaker's shrinkage is the total contraction in volume (including liquid, solidification, and solid shrinkage) that occurs when an alloy is poured into a mold. The contraction in volume of aluminum is one of the principal factors affecting the occurrence of cracks, as will be shown later, and the question of shrinkage and its control requires careful study in any treatment of cracking in castings. In the case of sand and die castings, cracks have been attributed to a number of causes, but in the case of most light aluminum alloys, they are due to the large contraction in volume on freezing and the lack of its regulation or control. The most important factors are: (1) Contraction in volume; (2) composition of alloy; (3) quality of melting charge; (4) design of casting; (5) method of molding; (6) hardness of ramming; (7) method of gating; (8) hardness and characteristics of cores; (9) chills; (10) risers; (11) melting temperatures; (12) furnace used for melting; (13) pouring temperatures; (14) inclusions in alloys; (15) hot shortness of alloys; and (16) physical properties of alloys at high temperatures. Of these, the first, second, third, and eleventh to sixteenth involve ascertainable metallurgical facts; the remainder are largely matters of opinion, judgment, and technical knowledge of men experienced in the production of castings.

Jan 1, 1923

By W. D. Robertson, W. L. Phillips Jr.

Stress-strain curves were obtained for single crystals of alpha brass in tension and in direct shear. Specimens were strained various amounts in a given slip direction, unloaded, and immediately strained in a second slip direction 60°, 120°, or 180&apos; from the original slip direction. Crystals strained in tension and direct shear had comparable critical resolved shear stresses and stress-strain curves. The density of slip lines in direct shear and in tension was essentially the same. The stress-strain curves obtained in shear were independent of initial orientation, choice of {111 } slip plane, choice of <110> slip direction, prior annealing temperature, and rate of cooling after annealing. There was no recovery after annealing for 4 hr at room temperature or 200°C; recovery was observed after 4 hr at 400°C. The crystals showed no asterism and mechanical properties were completely recoverable up to 20 pct strain. It was found that there is a barrier to slip in all latent close-packed directions, and that the magnitude of these barriers, evaluated at 3 pct strain, is proportional to prior strain and independent of the choice of latent direction in the {111} plane. The formation of Cottrell-Lomer barriers is discussed as a possible explanation for the hardening of the latent systems. AN idealized concept of plastic deformation indicates that a single crystal should yield at some stress that is dependent on crystal perfection and it should then continue to deform plastically by the process of "easy glide," which is characterized by a linear stress-strain curve and a low coefficient, ds/dE, of work-hardening. Hexagonal metal crystals generally conform to this ideal concept of laminar flow. In face-centered cubic metals the range of easy glide is always restricted in magnitude and it is strongly dependent on orientation, composition, crystal size, shape, surface preparation, and temperature. Since one of the principal differences between the two crystal systems, both of which deform by slip on close-packed planes, is the existence of secondary (latent) slip planes in the face-centered cubic crystals, it has been proposed that the transition from easy glide to turbulent flow, characterized by rapid linear hardening, is due to slip on secondary planes intersecting the primary plane.&apos;-.; However, the characteristic differences between individual face-centered cubic metals remain to be explained; in particular, it is not clear why the range of easy glide should vary so greatly in different metals and alloys similarly oriented for single slip. An investigation and comparison of different metals with respect to latent hardening on the primary slip plane should provide some of the information required to specify the necessary and sufficient conditions governing the transition from easy glide to turbulent flow. But, in order to accomplish this purpose, plastic strain must be produced by simple shear in a chosen plane and in a predetermined direction by some form of directed shear apparatus, the results of which must be correlated with the corresponding tension experiments. Two such experiments have been performed previously with zinc and with aluminum. Edwards, Washburn, and Parker" and Edwards and Washburn7 found that the strain-hardening coefficients in two latent directions in the basal plane of zinc were the same as in the primary direction. However, to initiate and propagate slip in either the [2110] or the [1210] direction, following primary slip in the [1l20] direction, it was necessary to increase the stress above that required to continue slip in the primary direction; when the direction of shear was reversed 180 deg plastic strain began at a much lower stress than that required to initiate slip in the original direction and the stress to propagate slip in the reverse direction was lower than the stress to continue slip in the forward direction, indicating a permanent loss of strain-hardening. Rohm and Kochendorfer observed softening in aluminum for all latent close-packed planes and directions. They also found that the critical resolved shear stress obtained from their direct shear apparatus was 50 pct lower than the value obtained from conventional tension tests, that the stress-strain curve was linear at 50 pct plastic strain, and that slip lines were not visible at strains less than 30 pct. At present it is uncertain whether these diverse results correspond to real differences in work-hardening characteristics of the close-packed planes of aluminum and zinc or to differences in experimental technique. In view of Read&apos;s analysis &apos;" of the stress distribution in the experimental arrangement of Rohm and Kochendorfer, there is some reason to question the significance of the latter results. In order to resolve this problem it is necessary to re-valuate the direct-shear technique and either repeat the previous measurements or investigate a third system. The latter choice seemed most likely to produce significant results with respect to work-hardening, and accordingly, it was decided to examine the hardening characteristics of the latent slip directions in alpha-brass. The choice of alpha-brass was dictated by the fact that easy glide is more extensive in this alloy than in any other face-centered cubic metal or alloy and, presumably, more nearly like the idealized hexagonal system. Experimental Procedure Crystals were made in graphite by the Bridge-man method in the form of cylinders, 11/2 in. diam and 8 to 9 in. long. Material for the crystals was 70/30 brass containing the following impurities:

Jan 1, 1959

By R. W. Fountain, M. Korchynsky

The precipitation phenomena occurring in cobalt-tantalum alloys have been investigated in the temperature range frm 500" to 1050°C by correlating the results of metallographic, X-ray, micro-and macrohardness, and electrical resistivity studies. The property andmacrohardness,changes were found to depend on 1) general precipitation, and 2) lamellar precipitation. Two new intermetallic phases have been identified: 1) a Co3Ta, a metastable ordered face-centered-cubic compound, and 2) a stable ß Co3Ta phase of hexagonal structure. In addition, the previously reported Co2Ta phase was found to exist in two allotropic modifications: the hexagonal MgZn,-type and the cubic MgCu2-type Laves phases. SINCE a large variety of structures can result as a consequence of the decomposition of a solid solution, predictions on the nature of property changes are difficult, if not impossible, to make. For any rational attempt to correlate properties and structures of a precipitation-hardenable alloy, a detailed understanding of the kinetics of decomposition and morphology of phase separation, as well as knowledge of phase relationships, appears to be prerequisite. Information of this type has been accumulated in the past for many alloy systems, both of theoretical and pastforpractical importance.1,2 Although the presence of intermetallic compounds has been reported in cobalt-base alloys,3 the amount of published information on precipitation-hardenable cobalt-base systems is very limited. A survey of the binary phase diagrams of cobalt indicates that cobalt-tantalum alloys might be of interest as typical of other cobalt-base systems in which Laves phases of the A,B type can be precipitated from solid solution. The present work has been undertaken, therefore, to study the kinetics and morphology of the precipitation reaction in this system and to establish a base for a correlation between the structural aspects and properties in this class of alloys. PREVIOUS WORK The only available phase diagram of the cobalt-tantalum system is based on the work of Koster and Mulfinger. According to these authors, the maximum solubility of tantalum in cobalt is about 13 pct (at 1275°C) and. less than 7 pct at room temperature. Tantalum additions lower the temperature of allotropic transformation of cobalt (about 420°C), and at 7 pct Ta, the high-temperature face-centered-cubic modification (ß cobalt) is retained at room temperature. The precipitating phase was originally designated as Co5Ta2 compound (55.2 pct Ta, about 1550°C melting point), but subsequent investigations by wallbaum5" identified this constituent as the A,B-type Laves phase. Wallbaum&apos;s data indicate that there are two modifications of this intermetallic compound: one richer in cobalt (Co2.2 Tao.8)of the hexagonal MgNi, type; and another of a higher tantalum content (Co2Ta) of the cubic MgCu, type. On the other hand, Elliott7 found that the cobalt-rich alloy (CO2.10,Tao.~l) was predominantly the cubic MgCu, type at 800°C and a mixture of both the MgCu2 and the hexagonal MgZn,-type Laves phases at 1000°C. At 1200°C, Elliott found only the MgZn, type while at 1400°C, he observed only the MgCu2 type. At the stoichiometric composition, Co2Ta, Elliott reported only the cubic MgCu2-type Laves phase in the temperature range of 600oto 1600°C. The precipitation of the cobalt-tantalum intermetallic compound is accompanied by a marked increase in hardness. According to Koster&apos;s4 data, the Brinell hardness of an 8 pct Ta-Co alloy increases from 230 to 340 upon short-time aging at 800°C. EXPERIMENTAL PROCEDURE The binary cobalt-tantalum alloys investigated contained 5, 10, and 15 pct Ta. The range of tantalum additions was thus slightly broader than the reported minimum and maximum solid solubility limits of tantalum in cobalt (7 and 13 pct, respectively)4 The alloys were vacuum-induction melted in a magnesia crucible using cobalt rondelles and technically pure tantalum sheet as raw materials. Deoxidation of the melt was accomplished with carbon, and the chemical analysis of the alloys is given in Table I. The effect of isothermal aging treatments on the progress of precipitation was studied on samples cut from cast ingots. These samples were solution treated for 2 hr at 1250°C and water-quenched. Aging was conducted in the temperature range from 500" to 1050°C for periods between 15 min and 1000 hr and followed by water-quenching. To prevent contamination from the atmosphere, all samples were sealed in evacuated Vycor or quartz tubes for heat-treatments. For solution treatment, argon at 0.2 atmospheric pressure was introduced prior to sealing of the capsule to prevent collapse at high temperature, and titanium sponge was placed at one end of the capsule to act as a getter. MACROHARDNESS The effect of aging on Vickers hardness (Dph) of

Jan 1, 1960

By J. E. Burke, Y. G. Shiau

SEVERAL attempts have been made to account for the fact that grains in a fully recrystallized metal will coarsen on annealing Two fundamentally different hypotheses have been advanced; with several variations of each. One school considers that the cause of grain growth is the surface energy of the grain boundary The theory of Jeffries1 that grain size and grain size contrast control growth is an example The second school considers the primary cause to be a difference in the lattice energy on either side of the grain boundary The more perfect grains are considered to grow at the expense of their less perfect neighbors, with a decrease in free energy, and a consequent increase in the stability of the system. Burgers2 presents the case for the strain or lattice imperfection theory of grain growth quite completely The latter theory is attractive, since there is no doubt that differences in lattice energy or lattice perfection can cause grain boundary migration A recrystallization nucleus grows for this reason as was beautifully demonstrated by van Arkel and Ploos van Amstel3 Although it is generally stated that grain growth does not precede recrystallization, several workers4,5 have shown that small strains may induce a single crystal in an aggregate to grow, or at least may cause some&apos; grain boundary migration The origin and nature of the imperfections that are considered to be responsible for normal grain growth have never been clearly described, but it is generally agreed that they are a consequence of the difficulty of atomic reorientation in the solid state, and that they do not seriously differ from the type of imperfection that-can be introduced by mechanical deformation An object of the present work was to determine whether the introduction of mechanical deformation would cause grain growth in a specimen which would not otherwise show it under the conditions used It was also planned to determine the effect of such deformation the rate of growth in a specimen which would show - growth in the unstrained condition Recently Maddigan and Blank6 have indicated that slightly strained specimens of alpha brass can undergo considerable growth prior to recrystallization if annealed at low temperatures French7 has reported that at deformations less than 17 pct it is very difficult to detect the beginning of recrystallization in the same material. It was therefore planned to broaden this work to include a complete study of the microscopic behavior of alpha brass under conditions of temperature, time, grain size and deformation such that recrystallization would not occur or would occur to only a small extent EXPERIMENTAL PROCEDURE The brass was prepared by melting cathode copper and commercially pure zinc

Jan 1, 1947

By Claudio Barsotti, Leonard C. Kitchener

INTRODUCTION The major mining operations of the Ontario Division of Inco Metals Company are located in the Sudbury Basin. Around the rim of this geo- logical formation and within thirty miles of the City of Sudbury are located eleven under- ground mines of the Company, two of which are on standby. In addition, there is one mine in Northwestern Ontario at Shebandowan, 1127 Km (700 miles) northwest of Sudbury. In 1980 ore production totalled 10.6 x 10 mt (11.7 million tons) from underground and open pit operations. Underground mining methods include blasthole, vertical retreat, sublevel caving, cut-and-fill and undercut-and-fill. Inco reduction operations in the Sudbury area include two concentrators, one smelter, one iron ore recovery plant, a copper refinery a nickel refinery and a high purity plate rolling mill. As well, an electrolytic nickel refinery is located on Lake Erie at Port Colborne, near Niagara Falls. In the Sudbury District, Inco employees total 14,278 of whom 6,490 are directly employed in the mining and milling operations. I T H DRILLING Background - The use of long blastholes in underground operations at Inco mines in the Sudbury district started more than 30 years ago at the Levack Mine. At that time, diamond drills were used to mine ore by open stoping and for pillar recovery. By the 1950&apos;s the concept had been extended to all mines. The heavy percussion drill was also developed by this time and led to the acceptance of the 11.43 cm (4% in.) piston diameter drifter for bar and arm and fan drill applications. The use however, of the nominal 5.08 cm (2 in.) diameter blastholes drilled radially from the level or sublevel causes overdrilling at the periphery. As well, the smaller holes are subject to hole deviation, are difficult to drill beyond 38.1 m (125 ft.) and require the need for several drilling horizons or sublevels. The need to improve blasthole stoping techniques and our experience with large diameter blastholes in open pit mining led to the trial of an I T H drill in 1962. The test was unsuccessful however, since button bits were not available at the time and the tungsten carbide cross bit experienced short life, gauge loss, and caused hole deviation and poor penetration rates. The successful application of the raise borer beginning in 1964 and the ability to drill 20.32 cm (8 in.) to 27.94 cm (11 in.) diameter pilot holes led to the development of smaller, more portable, rotary drills for blasthole mining. As a result, a mining method based on the use of 20 cm (7 718 in.) diameter, 60.1 m (200 ft.) long rotary blastholes was developed and tested successfully at our C.C.North Mine. Between 1972, when the method was first tested, and 1973 over 4572 m (15000 ft.) of large holes were drilled with rotary drills in the recovery of 175,960 mt (194000 tons) of primary stoping and pillar remnants. A new mining method was developed that made use of this large hole drilling equipment. Instead of longhole carbide drilling by bar-and-arm or fan drill set-ups at sublevels, the large diameter holes were drilled full stope height from the top sill, which substantially reduced development, drilling time and improved fragmentation. These drills however, were difficult to move and set-up, and had a high maintenance cost and low productivity. The capital outlay and extensive technical development required to improve these drills and reduce the high drilling costs however, was economically unattractive. New development in drills and button bits INTRODUCTION The major mining operations of the Ontario Division of Inco Metals Company are located in the Sudbury Basin. Around the rim of this geo- logical formation and within thirty miles of the City of Sudbury are located eleven under- ground mines of the Company, two of which are on standby. In addition, there is one mine in Northwestern Ontario at Shebandowan, 1127 Km (700 miles) northwest of Sudbury. In 1980 ore production totalled 10.6 x 10 mt (11.7 million tons) from underground and open pit operations. Underground mining methods include blasthole, vertical retreat, sublevel caving, cut-and-fill and undercut-and-fill. Inco reduction operations in the Sudbury area include two concentrators, one smelter, one iron ore recovery plant, a copper refinery a nickel refinery and a high purity plate rolling mill. As well, an electrolytic nickel refinery is located on Lake Erie at Port Colborne, near Niagara Falls. In the Sudbury District, Inco employees total 14,278 of whom 6,490 are directly employed in the mining and milling operations. I T H DRILLING Background - The use of long blastholes in underground operations at Inco mines in the Sudbury district started more than 30 years ago at the Levack Mine. At that time, diamond drills were used to mine ore by open stoping and for pillar recovery. By the 1950&apos;s the concept had been extended to all mines. The heavy percussion drill was also developed by this time and led to the acceptance of the 11.43 cm (4% in.) piston diameter drifter for bar and arm and fan drill applications. The use however, of the nominal 5.08 cm (2 in.) diameter blastholes drilled radially from the level or sublevel causes overdrilling at the periphery. As well, the smaller holes are subject to hole deviation, are difficult to drill beyond 38.1 m (125 ft.) and require the need for several drilling horizons or sublevels. The need to improve blasthole stoping techniques and our experience with large diameter blastholes in open pit mining led to the trial of an I T H drill in 1962. The test was unsuccessful however, since button bits were not available at the time and the tungsten carbide cross bit experienced short life, gauge loss, and caused hole deviation and poor penetration rates. The successful application of the raise borer beginning in 1964 and the ability to drill 20.32 cm (8 in.) to 27.94 cm (11 in.) diameter pilot holes led to the development of smaller, more portable, rotary drills for blasthole mining. As a result, a mining method based on the use of 20 cm (7 718 in.) diameter, 60.1 m (200 ft.) long rotary blastholes was developed and tested successfully at our C.C.North Mine. Between 1972, when the method was first tested, and 1973 over 4572 m (15000 ft.) of large holes were drilled with rotary drills in the recovery of 175,960 mt (194000 tons) of primary stoping and pillar remnants. A new mining method was developed that made use of this large hole drilling equipment. Instead of longhole carbide drilling by bar-and-arm or fan drill set-ups at sublevels, the large diameter holes were drilled full stope height from the top sill, which substantially reduced development, drilling time and improved fragmentation. These drills however, were difficult to move and set-up, and had a high maintenance cost and low productivity. The capital outlay and extensive technical development required to improve these drills and reduce the high drilling costs however, was economically unattractive. New development in drills and button bits

Jan 1, 1981

By T. L. Joseph

THE extent to which hot metal from the blast furnace affects open-hearth practice and the quality of steel produced has been discussed widely. Open-hearth operators have attributed difficulties experienced in making satisfactory steel to characteristics of the pig iron not disclosed by ordinary analysis. The commonest criticism of the iron has been that it is "physically cold" or "dirty." Often when the blast furnaces are working irregularly the quality of the iron is questioned. A cold hearth, slipping and hanging, the use in the past of unsintered flue dust, and the use of ores difficult to smelt have been associated with the production of iron of poor quality. The difficulty of the situation is that we have no proven yardstick for quality aside from ordinary analysis. Uniformity in analysis is recognized as being important, but the difficulty of changing the open-hearth practice when the iron analysis varies widely may not always be fully appreciated. Although the problem of correlating the characteris-tics of steel with those of pig iron is admittedly obscure, the effort of producers of quality steel to investigate all factors that may have a bear-ing on the final product is justified. This report contains data on the oxides in several hundred casts of basic iron produced in a furnace during the course of normal operation on Lake ores. Incidental to the study of the oxides in the iron, it was desir-able to follow closely the temperature of the iron. The effect of tempera-ture of the iron upon the silicon and sulphur present is discussed. A general relation between the basicity of the slag and the sulphur in the metal was developed. The amount and composition of oxides in the hot metal and in the steel bath during various intervals between melt-down and tap are discussed. Heats of rimmed steel, lulled steel, and semikilled steel were investigated. The hot metal on individual heats was either all taken from a mixer or consisted partly of direct metal and partly of

Jan 1, 1937

By M. C. Flemings, G. E. Nereo

General expressions are given to describe macro-segregation in castings and ingots which results from mass flow of solute-rich liquid to feed solidification and thermal contractions. Analytical solutions are given for solidification with planar isotherms (unidirectional and bidirectional heat flow). These solutions describe inverse segregation and centerline segregation. Numerical examples are given for A1-4.5 pct Cu alloy. In 1540, Vannoccio Biringuccio published one of the first references to macrosegregation, describing the problem of exudation and inverse segregation in the manufacture of bronze gun barrels.&apos; Since then, a great many studies of macrosegregation have been reported. Recent work of particular engineering interest includes that of Marburg 2 and others:" on centerline segregation and other types of segregation in large steel ingots, and work of Adams,5 Scheil, 6 and Kirkaldy and youdelis7 on inverse segregation in nonferrous ingots. In most studies on this subject, the various types of macrosegregation have been treated as separate phenomena. For example, quite different mechanisms have been proposed for formation of centerline segregation, negative cone of segregation, inverse segregation, banding, and so forth. In this, and in several papers to follow, it is proposed that these as well as other types of macrosegregation result from the same basic mechanism and can be quantitatively described by the same basic equation. It has often been suggested that some types of segregation (such as centerline segregation and banding) occur as a result of buildup of solute at the tips of growing dendrites.2-4 ,8-10 As example, banding can be induced in centrifugal castings by mechanical vibration, and Northcott 10 suggests this might be due to the influence of the vibration on the boundary layer at the dendrite tips of the growing dendrites. However, in view of the extremely small boundary layer known to exist at the tips of the dendrites,11,12 any interpretation of macrosegregation based on this boundary layer is clearly incorrect. Note that experiment has shown that significant buildup of solute does not occur at dendrite tips in ingot solidification, but even if such buildup occurred the thickness of the enriched zone would only be the order of D/U where D is liquid diffusion coefficient and U is dendrite tip velocity. For usual casting or ingot solidification this solute-enriched layer is 10"3 cm, far too small to account, for example, for centerline segregation.11&apos;12 It has also been suggested that convection in the bulk liquid (ahead of the advancing dendrites) might cause segregation by sweeping away the solute-rich boundary layer in front of the dendrites.3 However, since there is no significant boundary layer, this explanation must be incorrect. The convection might directly cause segregation by penetrating between the dendrite arms, and presumably in a rimming steel ingot it is sufficiently vigorous to cause some segregation in this way. Centerline segregation, however, cannot be interpreted as resulting from this convection since a sharply segregated zone is usually found near the centerline, with the bulk of the ingot being nearly of nominal composition. If convection in the bulk liquid were the direct cause, a gradual change in ingot composition over the entire cross section would be expected. It is known that sudden changes in convection of the bulk liquid during solidification can result in banding,14 but it is not clear that the banding results directly from the effect of convection on solute distribution. Changes in convection also affect thermal conditions in the liquid-solid region of a solidifying ingot. It will be seen later in this paper, and in a paper to follow, that macrosegregation is strongly influenced by these thermal changes. Recognizing that in some cases of ingot solidification (as in solidification of rimming steels) convection in the bulk liquid may have a direct effect on solute distribution, we neglect it in this paper and in the several to follow. We then derive general expressions describing macrosegregation which results from the mechanism of interdendritic flow of solute-rich liquid

Jan 1, 1968

By A. B. Kinzel

PRECISE knowledge regarding the effect of heat treatment on the properties of steel has made possible the detailed specifications and instructions covering optimum heat-treating temperatures and practices that are in current use. A distinct contrast is presented by the metal-lurgical treatment of steel adjacent to a fusion weld, as such steel is subjected to each, temperature from room temperature to fusion tempera-ture, and cooled at a rate that is not generally controllable but is pre-determined by the nature of the assembly to be welded, the kind of welding used, and the surrounding conditions. This is true regardless of the type of fusion welding: oxyacetylene, electric arc, thermit or flash resistance. Therefore it seemed desirable to investigate the effect of this metallurgical treatment on the characteristics of carbon steels commonly used for welding, by a detailed study of metal subjected to each temperature range; i.e., each heat-affected zone. Oxyacetylene welding was chosen for the investigation because of the experimental facility of accurately segregating and studying each tem-perature zone. The nature of the zones produced by other types of welding is the same. The difference is primarily a matter of dimensions of each of the temperature zones involved. The advantages and dis-advantages of the extent of the zone are of prime moment, and are dis-cussed after the presentation of the detailed zone study. No mention is made of the fused metal proper, as this has been the subject of much published research and the nature of the solidified metal is fairly well known.

Jan 1, 1935

By J. F. Keefe, C. J. Bier, O&apos

This study was carried out with copper because it represents the simplest form of sintering, in that but one metal is involved and all reactions occur in the solid state. The present work will cover three variables affecting the sintering process; namely, briquetting pressure, sintering temperature and time in hot zone. Although strength and dimensional changes were observed, this is primarily a metal-lographic study of the sintering process in copper. The term "sintering" should be understood to mean the process by which the metal powder particles of the compact become united into one body. Material Used The copper powder used was made from reduced copper oxide, and is typical of a grade used for the mass production of parts formed of metal powders. The screen analysis of the powder was as follows: Per Cent Per Cent BY BY Particle Size "Weight Particle Size "Weight Mesh Microns /80.... 0.00 43/32.... 17.49 80/I00..... 32/20......16.68 100/140.... 0.34 20/10.... 23.14 140/200___ 15.25 10/5..... 4.64 200/230....... 5.00 5/0...... 0.75 230/325.... 16.70 — 325....62. 69 The minus 325-mesh analysis was made by using a Roller Air Analyzer.1,2 The apparent density is here defined as the weight per cubic centimeter of the loose, unpacked powder as measured with the Hall flowmeter. The value for the powder used was 2.57 grams per cubic centimeter.

Jan 1, 1945

By G. Austin Schroter

ALTHOUGH there is now an extensive literature on the bleaching clays, not a great deal of material is to be found concerning the geological fea-tures of these deposits and their bearing on problems of exploration and development. At the same time, chemical and crystallographic research on the clay minerals during the past few years has laid a suitable founda-tion upon which to base conclusions of economic value drawn from field observations. All of the criteria and deductions herein presented are based upon extensive field work by the senior author, both in the United States and Canada, and when subjected to the ultimate tests of development and exploitation they have held up remarkably well, despite the fact that many of these conclusions apparently have not been reviewed in the litera-ture heretofore. The nomenclature of the bleaching clays is rather confusing in the light of present-day commercial standards and has even led to litigation." The old term "fuller&apos;s earth" is largely based upon trade usage and the definition of the term therefore is dependent upon the changing standards of commerce. For statistical purposes the Bureau of Mines81 classes as "fuller&apos;s earth" all natural bleaching or filtering claylike materials that possess high adsorptive capacity without previous chemical treat-ment or activation. Conversely, the so-called activated or acid activated clays are now generally recognized as any clay mineral or mixture of the clay minerals whose adsorptive capacity has been developed to commercial standards by chemical or physical treatment. Therefore, without attempting to propose any additions to the nomen-clature of bleaching clays, this paper will refer to naturally adsorptive clays and activable clays, respectively, for the two types indicated.

Jan 1, 1940

Jan 1, 1924

THOSE MARKED THUS * ARE MEMBERS, MARKED THUS ?ARE ASSOCIATES. THESE SIGNS DOUBLED INDICATE LIFE MEMBERS AND ASSOCIATES RESPECTIVELY. THE FIGURES AT THE END OF THE ADDRESS INDICATE THE YEAR OF ELECTION. HEAVY-FACED TYPE SIGNIFIES HONORARY MEMBERSHIP. *AARONS, J. BOYD, Vivian Gold Mining Co., Ltd., Harris, West. Australia. &apos;05 *ABADIE, EMILE R., Cons. and Min. Engr., 214 Union Savings Bank Bldg., Oakland, Cal. &apos;76 ?ABBÉ, MAX F., Prest., Abbé Engineering Co, 220 Broadway, New York, N.Y. &apos;07 ? ABBÉ, PAULO., Secy.,Abbé Engineering Co., 220 Broadway, New York, N.Y. &apos;07 *ABBOTT, CHARLES W., Min. Engr. Pioche, Nev. ?08 *ABBOTT, CLARENCE Chief EDgr., Iron Mines, Dic Tennessee Caol, Iron & R. R. Co., Bessemer, Ala. &apos;04 *ABBOTT, JAMES W., Min. Engr: Ploche, Lincoln Co., Nev. &apos;94

Jan 1, 1917

By G. Austin Schroter

ALTHOUGH there is now an extensive literature on the bleaching clays, not a great deal of material is to be found concerning the geological fea-tures of these deposits and their bearing on problems of exploration and development. At the same time, chemical and crystallographic research on the clay minerals during the past few years has laid a suitable founda-tion upon which to base conclusions of economic value drawn from field observations. All of the criteria and deductions herein presented are based upon extensive field work by the senior author, both in the United States and Canada, and when subjected to the ultimate tests of development and exploitation they have held up remarkably well, despite the fact that many of these conclusions apparently have not been reviewed in the litera-ture heretofore. The nomenclature of the bleaching clays is rather confusing in the light of present-day commercial standards and has even led to litigation.76 The old term "fuller&apos;s earth" is largely based upon trade usage and the definition of the term therefore is dependent upon the changing standards of commerce. For statistical purposes the Bureau of Mines81 classes as "fuller&apos;s earth" all natural bleaching or filtering claylike materials that possess high adsorptive capacity without previous chemical treat-ment or activation. Conversely, the so-called activated or acid activated clays are now generally recognized as any clay mineral or mixture of the clay minerals whose adsorptive capacity has been developed to commercial standards by chemical or physical treatment. Therefore, without attempting to propose any additions to the nomen-clature of bleaching clays, this paper will refer to naturally adsorptive clays and activable clays, respectively, for the two types indicated.

Jan 1, 1940

By T. A. Rickard

Among the names which won a world-wide fame during the golden age of the early fifties, Bendigo and Ballarat were to Australia, what the Yuba and Grass Valley were to California. The map of Victoria did not for a long time show the name of old Bendigo;* for this first and more distinctive name was replaced with the more English Sandhurst, just as the alluvial diggings gave place to quartz mining. Towards the close of last pear, steps were taken to give back the old name, as associated with the early days of rich alluvium, and more suggestive than the application taken secondhand from an English military academy. History. The first discovery of gold? in this district, was made in the autumn of 1851 ; but there has never been any certainty as to the day or the man. At that time the country around Bendigo Creek was a part of the Ravenswootl sheep-run, and its resemblance to the Forest Creek district (now Castlemaine), induced the first prospecting. It was late in November when the "rush" broke out; the shepherds left their flocks; the sylvan solitudes were disturbed by * The name of Bendigo is said to have been derived from a hut-keeper on the Ravenswood sheep-run, who on account of his fondness for " fisticuffs " was nicknamed Bendigo, after the prize-fighter of that name. It is not aboriginal, as is often supposed, but Spanish ; and equivalent to our Benedict. There must always be some confusion between the two names of Sandhurst and Bendigo; the town, and with it the gold-field, having been three tinies named. Several other old familiar names have been likewise unfortunately replaced by second-hand English ones; so that an old digger talks of Forest Creek when he means the modern Castlemaine, Mt. Ida for Heathcote, Growler&apos;s Creek for Bright, etc. I shall use the names Sandhurst and Bendigo interchangeably. The first discovery of gold in Australia, was made by E. H.Hargraves, February 12, 1851, near Bathurst in New South Wales. In August of the same year the discovery at Buninyong, near Ballarat, inaugurated the first of a series of rushes to the Victoria gold-fields.

Jan 1, 1892

By C. W. Volek, G. Mandl

Steam-injection tests in the field have shoum that heat transport into the oil/water region, ahead of the steam zone, may have a significant effect on the production process. Earlier theoretical work on reservoir heating by hot-fluid injection can be used to describe the growth of the steam zone, but only if heat transport from steam zone into oil/water region is neglected. It therefore became necessary to re-examine and extend the earlier theory. It was found that this theory ceases to be consistent with the physical model of the process at a certain critical time, tc, which depends on reservoir thickness, temperature, and quality of the steam. The critical time marks an important change in the heat flow across the condensation frovt: the heat flow, which is purely conductive during 0 < t < tc&apos; becomes predominantly convective at t = tc. Accordingly, at t = tc, the equation which governs expansion of the steam zone changes. On the basis of the new equation, an approximate description for the steam-zone growth during t > tc is developed by making use of upper and lower bounds for the exact solution of the problem. The boundary conditions for heat and mass flow inside the oil/water region are established, and a simple method of detennining the saturation at the downstream side of the condensation front is presented. Experimental results show that the theory gives an accurate description of steam-zone expansion before the critical time. At times near critical time, and also after critical time, experimental data show theoretical steam-zone volumes to be high. Even so, the accuracy of the calculated steam-zone volumes is sufficient for practical purposes. THEORY OF STEAM-ZONE GROWTH INTRODUCTION The engineering evaluation of steam-drive processes is based mainly on a mathematical description of reservoir heating by hot fluid injection presented several years ago by Marx and Langenheim.l This theory can be used to determine the growth of the steam zone,2 provided the flow of heat from the steam zone into the liquid zone ahead of the condensation front (Fig. 1) is neglected. Since we must expect, however, that heat transport into and inside the liquid region (the region between condensation front and production wells) will affect both the water/oil flow and the growth of the steam zone, it is necessary to re-examine and to generalize the Marx and Langenheim theory as applied to steam drive, which will hereafter be termed the "old" theory. Observations made in several field tests emphasize the need to study the heat flow across the condensation front (CF). On several occasions it was discovered that heat was transported in the liquid zone far ahead of the advancing CF, resulting in an early breakthrough of warm water. This seems to occur most often when high injection pressures are applied, when "wet" kONINKLIJKE/SHELL EXPLORATIE EN PRODUKTIE LABORATORIUM RIJSWIJK, THE NETHERLANDS SHELL DEVELOPMENT CO. HOUSTON, TEX.

Jan 1, 1970

Jan 1, 1924

By Frederick Laist

ABOUT six years ago the Anaconda Copper Mining Co. decided to investigate the possibility of extracting zinc from the ores of certain mines in the Butte district. These ores are of a complex character and contain so much iron and lead that the concentrate contains only 33 to 35 per cent. zinc. Investigations showed that while a high-grade concentrate could not be obtained by ordinary methods, such as tabling and magnetic treatment, a fair grade could be made by the Horwood process. In this method, the concentrate resulting from the flotation of all of the sulfides is given a light roast and this calcine is subjected to flotation in the presence of a large amount of sulfuric acid; the resulting concentrate contains most of the zinc and a residue contains most of the iron. The fact that the lead, copper, and silver are divided approximately equally between the zinc concentrate and the iron residue and the large consumption of acid, which ranged from 50 to 100 lb. (22 to 45 kg.) per ton of concentrates, were serious objections to this plan. The zinc recovery, moreover, was low, as a considerable percentage invariably accompanied the iron. While a profit might be made on the ores by the use of this process, it was thought that other and more promising methods might be devised. After carefully studying the field and doing some laboratory work on various processes that had been suggested, it was decided that the electrolysis of sulfate solutions was the most promising. We soon found, as have other investigators, that the only way to obtain a good zinc deposit is to have the electrolyte free from all metals more electro-negative than zinc, such as copper, cadmium, lead, arsenic, antimony, etc. Arsenic and antimony are particularly injurious, causing very poor current efficiency and small yield per horsepower when present in amounts so small as almost to defy detection-1 mg. or less per liter.

Jan 10, 1920

By Frank Riddle

PRODUCTS made from the ores of the sillimanite group, and synthetic substitutes for them, have unique properties, and service tests prove that they are playing, and will continue to play, a major part in improvements in metallurgical processes. Also, they are examples of how comparatively useless, rare, or "museum" minerals have been made available in commercial quantities. Until research developed uses for them, the minerals had been observed only in small, scattered masses, or crystals. Improvements in ceramic processes and compositions have come about very gradually. In the last 10 or 15 years, several outstanding developments have been made. Of greatest interest to the mining and metallurgical engineers are those affecting the composition, necessitating the mining of new minerals, and improvements in ceramic products used in metallurgical processes.

Jan 1, 1932