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By Akinobu Kasami, Keiji Maeda, Makoto Naito, Masaharu Toyama

Gap electroluminescent diodes have been prepared by the vapor phase diffusion of zinc into n-Gap crystals which were grown from a gallium solution (10 wt pct Gap) doped with tellurium and Ga203. A marked improvement in the efficiency of the red electrolumines -cence has been achieved by heat treatment after diffusion. External quantum efficiencies of diodes annealed under optimum conditions are 0.2 to 0.6 pct at room temperature, or about 200 times higher than the efficiencies of diodes quenched after diffusion. The optimum dopant concentrations in the gallium melt from which the crystals were grown are 3to6 x at. pct Te and 4 to 8 x 10-2 mol pct Ga203. The efficient diodes are characterized by linearly graded junctions with an i-layer 0.1 to 0.2u thick. Annealing increases the emission intensity by a factor of 20 to 50 and decreases the current density to 1/3 to 1/8 that of quenched diodes at a given bias. The decrease in current is attributed to an annihilation of deep recombination centers in the depletion layer. The increase in emission intensity is interpreted in terms of an increase in lifetime of minority carriers and an increase in the relative intensity of red-to-infrared emission. The dependence of these quantities on the tellurium and oxygen doping levels is also discussed. A number of studies have been made of the red light emission from for ward-biased Gap diodes.' At room temperature this emission band is centered at 7OOO? with a spectral width of nearly 1000?. Low-tempera-ture photoluminescence indicates that this emission is due to either the radiative annihilation of an exciton bound to a pair of zinc and oxygen atoms substituting on nearest neighbor lattice sites2,3 or the radiative recombination of an electron bound to this Zn-O pair with a hole bound to an isolated zinc shallow acceptor.3 An emission band is also observed with a spectral peak at 9800?. This infrared emission has been shown to be due to the recombination of an electron trapped at an isolated oxygen deep donor with a hole trapped at an isolated zinc acceptor.4 The red emission from Gap diodes is fairly efficient at room temperature because the nearest neighbor Zn-0 pair forms a deep electron trap at 0.3 to 0.4 ev below the edge of the conduction band.2'4 In diodes grown by liquid epitaxy an external quantum efficiency of 2.1 x 10-2 (photon/electron) has been attained by heat treatment at relatively low temperatures.5 This heat treatment was found to increase the efficiency by a factor of 3 to 6. However, no detailed studies have-been reported on the effects of heat treatment. We can only cite Onton and Lorenz's work6 on the change ; in the relative intensity of red-to-infrared emission. Heat treatment has also been tried on junctions built in during growth, but contrary to expectations the efficiency decreased. In-diffusion is a simple and controllable method of fabricating p-n junctions. For Gap, zinc is generally used to form a p-type layer on n-type crystals. The emission efficiencies of in-diffused diodes are, however, extremely low in comparison with liquid epitaxial diodes.' Although efficiencies as high as 2 x 1O-3 have been reported, values from 10-6 to 10-4 are generally obtained by typical diffusion techniques. Out-diffused diodes are known to be a little more efficient than in-diffused diodes. Nevertheless, the quantum efficiency is at most 7 x 10- 3 and ordinarily of the order of 10-4.8 NO results have been reported on heat treatment of either in-diffused or out-diffused diodes. This paper reports a marked improvement in the efficiency of the red emission observed for in-dif-fused diodes as a result of heat treatment after diffusion. The method described reproducibly yields diodes with external quantum efficiencies of 2 to 6 x 10-3. The observed dependence of efficiency on annealing time and on doping level will be discussed in terms of the lifetime of minority carriers and the formation of Zn-O complex pairs. EXPERIMENTAL A) Diode Fabrication. The n-Gap crystals used in this study were grown from a saturated gallium solution by a slow cooling method.8 The Gap content in the gallium melt was fixed to 10 wt pct corresponding to a growth temperature of about 1100 Tellurium was chosen as the n-type dopant and added to the melt in concentrations ranging from 0.001 to 0.06 at. pct. Oxygen was added in the form of Ga2O3, whose concentration was varied from 0.004 to 0.2 mol pct. The resulting crystals were platelets with well-developed (111) surfaces. Typical electrical properties were Hall mobilities of 130 to 30 sq cm per v-sec and carrier concentrations of 1016 to 10" cm-3 at room temperature. Diodes prepared from crystals with relatively low doping levels, in which u = 130 to 100 sq cm per v-sec and n = 0.6 to 6 x 1017 Cm-3, were examined in detail. The p-n junctions were produced in these n-Gap crystals by the diffusion of zinc from the vapor phase by the following procedure. The platelets were carefully lapped on both sides to a thickness of 150 to 200 u while maintaining the (111) orientation. After being etched in hot aqua regia, the crystals together with the zinc were sealed in an evacuated 12 mm ID quartz ampoule 20 cm long. The crystals and the zinc were then separated from each other at opposite ends

Jan 1, 1970

By T. A. Rickard

RICO, in the southwestern corner of Colorado, is one of the productive mining centers of the San Juan region, so-called because its waters drain into the river of that name, which is tributary to the Colorado. The San Juan region includes the counties of Ouray, Hinsdale, San Miguel, Dolores, San Juan and Montezuma. It is traversed by a network of picturesque mountain ranges on whose lofty summits there rests perpetual snow. The region is peculiarly rugged, and, in the early days of its development, tested to the full the hardihood of the adventurers who first explored its can ions 111 search for gold and silver. A prospecting party, guided by Jim Baker, scout and trapper, penetrated in 1861 this part of the territory of Kansas. At that time the country was in the possession of the Ute Indians. In October, 1873, by the Brunot treaty, they ceded to the United States Government the richest mineral-bearing portion of their

Jan 1, 1897

By W. Bradley, R. G. Hall

This paper will attempt to show how a metallurgical problem at one California quicksilver mine was solved, and how the solution was applied successfully at another mine. The pronouns "we" and "our," as used below, refer '0 the Bradley 'lining Co. of San Francisco. The term "concurrent firing" for the purpose of this paper can be defined as feeding and firing a a kiln at the same end—that is, of course, the upper end' This is as opposed to "countercurrent firing," the orthodox method, in which a kiln is fed at the upper and fired at the lower end. The terms "quicksilver" and "mercury" are used interchangeably. Early References The earliest work on nonferrous metallurgy, we believe, was The Pirotechnia of Vannocio Biringuccio,l its first edition having been printed in Italy in 1540. Quoting from its chapter entitled "Concerning Quicksilver and Its Ore": Quicksilver ... is one of the gods and has divine strength in itself, and also, to the annoyance of the alchemists, it is winged. Hence, when it sees that it is in gravest danger, it loosens itself from . . . every bond . . . and fies away into the heavens, escaping from the hands of those who crucify it. Almost laughing, it leaves all its adversaries mocked and scorned, with their phials and filters empty . . . How thorough a job, under certain conditions, it can do of mocking its adversaries and leaving their phials and filters empty, was found out four centuries later at the Sulphur Bank mine, on the east shore of Clear Lake, in Lake county, California, The other mine mentioned in the title is the Reed, in Yolo County, California, 35 miles by road southeast of Sulphur Bank, Reed and Sulphur Bank ranked respectively Nth and seventh in U. S. production in 1943. The earliest direct reference we can find to furnacing troubles at these mines was by Thomas Egleston in 1890.2 Speaking of Sulphur Bank, Egleston says: of there is more sulphur than cinnabar in the ore, which is a detriment to both . . . making the sulphur impure, and rendering the cinnabar difficult to work on account of the soot. In some of the early . . . furnaces the accumulation of soot from the excess of sulphur has been known to penetrate as far as the fan blower at the end of the . . . condensers, and completely prevent its revolution. In order to get rid of the inconvenience of this accumulation . . . , as well as to get a commercial value from the sulphur, it (the sulphur) is now separated by steam and sold. It is claimed that the sulphur alone pays all the expenses of ... the mine. The mine was first worked for sulphur, and the cinnabar it contained was considered to be an inconvenience, and was carefully picked out and thrown away, as its richness and value were not

Jan 1, 1949

By C. D. Wiseman

THE concept of alloying to increase the strength of metals originated during the bronze age. However, at the present time there is no single theory capable of explaining all of the observed strengthening effects of alloying elements on the mechanical properties. In general, it may be said that solid solutions are stronger than the pure metal and that the strengthening effect increases with increasing alloy content. Various theories for solution hardening have been proposed, the first of which was presented by Rosenhain who suggested that the alloying elements roughened the slip planes, thereby requiring a higher stress to initiate slip. Recent work by French and Hibbard2 confirmed Norbury's3 conclusion that those alloying elements which cause a greater change in lattice parameter have larger effects on hardness. However, a given change in lattice parameter produced by different alloying elements does not cause the same change in hardness. A further refinement was suggested by Dorn, Pietrokowski, and Tietz4 who considered differences in valence between the solute and solvent with the change in lattice parameter to explain the plastic properties of aluminum alloys. Allen, Schofield, and Tate5 further investigated the valency contribution to solution strengthening by testing some copper-base solid-solution alloys having constant electron densities. Tensile tests performed on these alloys gave identical stress-strain curves even though the atomic size effect, which varied by a factor of two, was neglected. The advent of dislocation theory6-8 provided a new and powerful tool capable of explaining many phenomena of plastic deformation and indicated new approaches to solution hardening. The basic con- cept of recent theories is that solution hardening is not due to stresses associated with randomly dispersed solute atoms, but rather to a nonuniform distribution of the solute. This conclusion was reached by consideration of the effective tension present on each dislocation line and the ability of a dislocation to pass an obstacle. cottrell suggested the possibility that the internal stresses due to randomly distributed solute atoms would offer essentially no resistance to the passage of dislocations. He reasoned that an edge dislocation may be considered as a rigid line discontinuity. As the dislocation moved through a crystal, the random stress fields would be equally distributed along its length. Since half of the stress fields would be acting to move the dislocation forward and the other half trying to move it back, the net effect on the dislocation would be zero. Thus the randomly distributed solute atoms would not contribute appreciably to solution strengthening. Mott and Nabarro10 considered the dislocation as a flexible, rather than a rigid, discontinuity. They obtained a simple model for a dislocation moving in a lattice having precipated particles, where the dislocation would actually bend around the obstacle until it would loop back onto itself to rejoin and then continue onward. Their work indicated that the minimum radius of curvature of the dislocation line, under the action of an external stress and in the region of an internal stress, would be such that the dislocation would be unable to pass through a matrix containing small closely spaced precipates by the looping process. The dislocations would tend to remain rather straight, approaching the condition of Cottrell's rigid dislocation. Hence, the strengthening must not be due to random solute atoms; however, it might be due to the concentration of atoms, either as clusters of like atoms or as short-range ordered regions, or to the concentration of solute atoms around dislocations. To date, four mechanisms of solution strength-

Jan 1, 1959

By Roger M. Nendick

The recovery of precious metals from heap leach solutions can be accomplished by two processes: 1. The Carbon Adsorption Process 2. The Merrill-Crowe Zinc Precipitation Process A brief review of the relative process economics is made. Each process presents certain design considerations that must be addressed during the evaluation and engineering design for the project. Discussion is presented on the design criteria for each process.

Jan 1, 1984

By Alden Greninger

THE time-honored description of the growth of metal crystals to form polycrystalline aggregates is one in which two important steps are con-sidered: (1) nucleation, and (2) dendritic growth, each dendrite starting from its individual nucleus and resulting (upon slow cooling, assuming no solid phase changes) in a macrograin. This picture of the process of crystallization is incomplete, and it is with the hope of enlarging upon it that the following summary and correlation of experimental results are given. MOSAIC STRUCTURE For an exact definition of the mosaic structure of metal crystals-if, indeed, one can be found that will hold for all metals-one must await the results of much experimental work in this field. The writer's investiga-tions have been confined almost entirely to copper and a few of its alloys. The following terms are proposed, and will be used in this report: Macromosaic Structure l.-Large-scale mosaic structure; more specif-ically, mosaic structure of a scale large enough to produce splitting of Laue spots on back-reflection Laue X-ray patterns2. The deviation from exact parallelism of neighboring macromosaics varies from a few

Jan 1, 1935

By J. Ruzicka

IN creep testing, material is subjected to a constant load, preferably at a constant temperature, and its rate of deformation is measured. The method of loading can be of various types but in this paper only creep testing under tensile load will be considered. The ordinary tensile test is essentially a comparison test in conditions that frequently bear little or no relation to those under which the test material is to be used in service. The purpose of creep tests is to measure the strength of the test material at slow rates of deformation that more nearly approach the rates realized in service. One purpose of this paper is to illustrate that the creep test, in addi-tion to its value as a service test, is superior to the ordinary tensile test as a sensitive tool for the comparison of certain metals in investigative testing. The other purpose is to describe equipment having distinctive features of design that make it especially suitable for such tests. Representative data obtained with this equipment on a group of rolled zinc-base materials are given. These data are compared with those from practical comparison tests of the creep type on weatherstrip fabri-cated from the same group of materials. The comparison illustrates the value of the fast creep test and of the equipment.

Jan 1, 1937

By J. Groyecki, M. Markuszewicz, J. Lassota, A. Zawada

The ratio of stable to unstable inclusions was found to ploy an essential role in the process of sccorldar-y recrystatlizalion in Si-Fe. The analysis of the free energy of inclusions in the range of heat-treatment of individual inclusions to be predicted. The effects MnS. ns inslable inclusions. were investigated. TO secure a high induction, the secondary recryslulliztt-lion associated wilh the texture is necessary. To obtain a low core loss an additional refiuing in the solid state is required. It has been found that sulfur can be more easily removed in racunm than in hydrogen and thai this process was hindered by the prescrzce of INCLUSIONS play an essential role in the development of cube-on-edge texture in Si-Fe. Their function consists in restraining the growth of primary grains up to about 900°C and in passing subsequently into solution at higher temperatures. This process is accompanied by the selective growth of secondary grains with (110)[001] orientation. The general effect of inclusions depends on such factors as the type of impurities, their amount. dispersion and stability, the conditions of diffusion in the space of lattice of metal, and the reactions at the metal/gas interface. In recent years, some of these factors were the subject of a special investigation. A positive influence of Mns, siN,' and vN3 has been established. The quantity of impurities4 and their dispersion5 have been found to be of major importance. Attention was called to the vital importance of diffusion and the conditions under which the impurities are removed from metal., It has also been demonstrated that in Fe-Si alloys by the techniques of powder metallurgy a special opportunity exists to obtain the (110)[001] type texture. 6 The aim of this work was to conduct qualitative investigations on the influence of inclusion stability on the development of cube-on-edge texture in a metal containing approximately 3 pct Si. Experiments were carried out on cast alloys and on those manufactured by powder-metallurgy techniques. The results obtained from these experiments were utilized to explain the phenomena involved and to analyze the relationships between stable and unstable inclusions and the magnetic properties of alloys. EXPERIMENTS AND RESULTS The raw materials used in these experiments were the powder of carbonyl iron with the analysis (in pct) 0.044 C, 0.01 Mn, 0.005 Si, 0.009 P, 0.002 S, traces of Cu, 0.06 Ni, 0.0015 Al, 0.03 Cr, 0.02 Mo, 0.01 Ti, 0.002 Co, traces of Pb, and the powder of silicon containing 94.14 Si, 0.003 S, 0.048 C. The powders were ground and mechanically mixed in 100-g batches. and then pressed at 9 tons per sq cm into 74 by 24 by 8 mm blocks. Sintering was carried out at 1100°C for 12 hr in vacuum (2 x lo-' Tr) or in hydrogen. In this instance the material was heated slowly and subjected to prolonged soaking at 350°, 650°, and 750 2C, respectively, to secure reduction of ferro-oxides. This was checked by making measurements of the dew point, which was found to change from -15" to -35°C after reduction. The compacts after sintering were hot-rolled to 2.4 mm, annealed at 800 C, and finally cold-reduced to 0.35 mm with intermediate annealing at 800°C at a gage of about 0.8 mm. Impurities were added in the powdered form and mixed with iron and silicon powders. Sulfur in the elemental state, electrolytic manganese, and pure aluminum oxide were employed. Besides, to obtain a material with low contents of impurities, especially

Jan 1, 1967

By K. C. Strebig, C. W. Schultz, A. A. Selim

The effect of some organic additives in diamond drilling of quartzite was investigated in the laboratory. The drill was designed to measure the rate of penetration, the thrust, and the torque and to record each as a function of the distance drilled. A statistical plan was followed throughout the investigation and an equation representing the bit performance was derived from the mathematical theory of reliability. The drilling torque was found to increase with the use of additives while the sliding coefficient of friction and the wear coefficient decreased. The energy per unit volume consumed was found to increase with the use of additives. A hypothesis explaining the effects achieved with the additives is given. INTRODUCTION For some time researchers have attempted to increase drilling efficiency by adding certain agents to the flushing medium. Much of this interest is the result of the observations of Rehbinder, Shreiner and Zhigach1 They postulated that "...in processes for the mechanical destruction of solids, a region of increased crack formation is created in the deformed layers adjoining that surface of destruction, forming the predestmction zone. The surrounding medium (for example, a liquid) which wets a given solid will penetrate the embryo microcracks of the predestruc-tion zone. Increasing the molecular affinity of this liquid for the surface of the solid considerably facilitates the deformation and destruction by softening the solid in the zone of increased crack formation. In this manner, the hardness or strength of the deformed body is decreased by the influence of the penetration of the liquid into the predestraction zone." This is known as the "Rehbinder effect". Rehbinder's work has prompted many investigators to examine the effect of additives on the mechanical destruction of rocks. Engelmann, Terichow and Selim reported that the maximum penetration of the rock by a diamond point in a solution environment was at the isoelectric point of the solution.* Robinson reported that his results did not appear to support the theory of Rehbinder.3 Joris and .McLaren suggested that additives with surface tension lower than water will be more efficient in cooling the diamonds.4 Their effectiveness in removing the fine cuttings from the face of the bit will also improve the efficiency of the system. They reported an improvement in impregnated bit life and penetration rates with the use of soluble oil additives. In contrast, Long and Agnew, drilling with surface set bits, reported that lubricating agents increase bit temperature and wear.5 A significant change was reported6 in the mechanical properties of rock with polar additives. It was concluded that this change in the mechanical properties of the rock in the presence of the additive is due to the rock hydrophilic properties. Ethylene glycol, glycerine and anionic detergent were selected for this investigation because their surface tension is lower than that of water. The surface tension of these additives for the concentrations studied was 42 to 75 percent of the surface tension of water. A low surface tension additive would wet the surface of the diamonds more easily and hence would be more effective in cooling the diamonds. Another characteristic of these low surface tension additives is their effectiveness in removing the cuttings and preventing the flocculation of the formed particles in the drilling process. This article summarizes the results of an investigation performed at the laboratories of USBM, Twin Cities Mining Research Center. The objective of the investigation was to study the over-all effects of some organic additives on the performance of diamond impregnated bits in atmospheric drilling conditions only and not in downhole pressured conditions.

Jan 1, 1970

By F. H. Buttner, E. R. Funk, H. Udin

A. P. Greenough (University College, swansea, Great Britain)—I have recently made some experiments on the deformation of silver wire at high temperature in an atmosphere of oxygen-free nitrogen. The observa-tions which 1 made confirm the main conclusion of this paper, that the most satisfactory mechanism so far suggested to explain the deformation which takes place

Jan 1, 1953

By Zay Jeffries

This paper will include a brief discussion of Prof. Howe's paper on The Supposed Reversal of Inheritance of Ferrite Grain Size from that of Austenite.l The general subject of grain refining in steel and iron will also be treated. The conclusions reached are stated in the following hypotheses which are discussed more in detail below. 1. The ferrite grain size in pure iron, the ferrite and pearlite grain size in hypoeutectoid steel, the pearlite grain size in eutectoid steel and the cementite and pearlite grain size of hypereutectoid steel are not inherited from the grain size of the mother austenite. 2. The only structural feature that is generally inherited from the austenite of hypo- and hypereutectoid steels on cooling through their transformation ranges is the position of the excess ferrite or cementite at the austenite grain boundaries, sometimes causing complete and sometimes incomplete networks which outline the old austenite grain boundaries. Rapid cooling through the transformation range will cause the non-inheritance of this structural (network) feature. 3. The austenite grain boundaries themselves are nearly always effaced in all steels and also in pure iron during the At transformations. 4. The grain-size refining of steel and iron is brought about by the combined effect of non-inheritance of the transformation products on either heating or cooling, i.e., the austenite transformation products do cst inherit their grain size from the austenite on cooling through the transformation range nor does austenite inherit its grain size from the products which form austenite on heating. 5. In general, in both iron and carbon steel the larger the austenite grain size, the larger will be the grain size of the transformation products on cooling. This, of course, assumes all other conditions constant except the austenite grain size. An exception is found to this general rule in very pure iron such as electrolytic iron. In this instance small austenite grains may form very large ferrite grains on cooling through Arg.

Jan 1, 1918

By Albert Wiggin

THE copper-bearing sulphide ores from the mines in Butte, Mont., which are for the most part concentrated at the Boston & Montana duction Works in Great Falls and at the Washoe Reduction Works in Anaconda, contain the following minerals of economic value: Chalcocite, Cu2S; enargite, Cu3AsS4; cupriferous pyrite; bornite, Cu3FeS3; covellite, CUS; tetrahedrite, 4 CuS2Sb2S3; and tennantite, Cu8AsS7;. All of the ores carry a high percentage of pyrite. Many of the above sulphides are argentiferous and also carry from 10 to 20 cts. per ton in gold. The gangue is quartz and highly altered granite, with sphalerite and galena and more rarely barite and hubnerite as accessory minerals. An average chemical analysis of the second-class ore concentrated at Great Falls and Anaconda would be as follows: Copper 3.2 to 3.4 per cent. Silver 2. 3 to 3.0 oz. per ton. Gold 0.0-1 to 0.15 oz. per ton. Si02.. 55 to 60 per cent. FeO 12 to 15 per cent.. Sulphur 12 to 1.5 per cent. Al2O3, S to 10 per cent. CaO 0.5 to 0.8 percent. As203, 0.5 to 0.6 percent. Lead 0.2 to 0.3 percent. Before describing the Great Falls flow sleet as installed, at Anaconda, a brief history of the Great Falls concentrator will be given, including a description of the various concentrating machines and systems which have been tested in the search for a flow sheet which would give a higher recovery of copper.

Jan 8, 1913

By Robert C. Freas, William H. Lane, David J. Krohn

Maysville, Kentucky, is the location of Dravo Lime company's new 9 070 mt(10,000 tons) per day limestone mine and 2 727 mt (3000 tons) per day calcination plant. This complex has been designed as a unit, and capitalizes on recent technological advances. Geologically the Dravo facility is.located on the eastern flank of the Cincinnati Arch, with the high calcium limestone being found at a depth of approximately 274 m (900 ft). A systems approach has been employed in designing and equipping the mine. This allows for maximum production while maintaining flexibility and versatility. All hydraulic drilling, large LHD equipment, and an extendable mine conveyor system are utilized in a five-part mining cycle. A modular concept modifies the room and pillar system to optimize ventilation. The limestone is calcined in three 5.18 x 61.87 m (17 x 203 ft) KVS rotary kilns with a design capacity of 909 mt (1000 tons) per day of lime per kiln. The kilns are coal fired and equipped with preheaters. Lime storage is provided by three 57 m (186 ft) high concrete silos with a combined capacity of 40 909 mt.

Jan 1, 1976

By J. M. Woodall

GuAs crystals which have been grown in quartz boats by the horizontal Bridgman method in the pvesence of Ga20 vapov have beetz found to have carrier and donor distributions which do not correspound to those expected from simple dopant seg-vegation during directional freezing; Instead, the carrier distribution is determined by the heat-trentnzent history of the crystal, while the donor distribution, zohiclz is principally due to silicon, is fixed by the pozuth rate, the geo)tlet.ry of the crystal growth vessel, and tlze initial Ga20 pressure. WHEN semiconducting materials are made into doped crystals by the normal freezing method,&apos; they usually exhibit doping variations along the growth axis. If a) there is no dopant diffusion in the solid, b) the dopant is distributed uniformly in the melt, and c) the distribution coefficient, k, does not vary with composition, then the doping variation along the growth axis is represented by the equation: where C is the doping level in the solid at a point where a fraction g of the original liquid has frozen, and Co is the mean concentration. When the dopant is either a singly ionized shallow donor or shallow acceptor, C also represents the carrier concentration. Even though this equation accurately describes the dcping profiles of a large number of normal freeze systems, there are several special systems for which Eq. [I] does not apply. One such system is the horizontal Bridgman method for preparing oxygen-grown GaAs crystals using quartz vessels. Several workers2"* have shown that GaAs crystals grown by the horizontal Bridglnan method using quartz vessels are generally contaminated with silicon in concentrations in excess of 5 < 10lG atoms per cu cm. This contamination is ascribed to a reaction: occurring at the walls of the crystal-growth vessel which liberates silicon into the melt and Ga2O vapor. It has been shown4 that this reaction, and, hence, the silicon contamination, can be suppressed by the addition of oxygen to the crystal-growth apparatus. It is the purpose of this paper to describe a special apparatus capable of yielding single crystals of GaAs grown in the presence of oxygen and to describe both the kinetics of silicon suppression in this system and the relationship between the carrier concentration profile and the silicon concentration profile. EXPERIMENTAL-CRYSTAL GROWTH A schematic diagram of the apparatus used in the oxygen addition experiments is shown in Fig. 1. The most important features of this apparatus are: a) the use of a sand blasted quartz boat, h) a quartz rod of length 1, with a hole of cross section A, that is placed near the boat to limit the free space volume V, over the melt during the growth, and c) the temperature gradient at and near the solid-liquid interface. Sand blasting the boat is necessary to prevent wetting of the melt. The quartz rod retards the diffusion of the GazO vapor away from the melt to the colder portions of the ampoule. A crystal is prepared by first loading a 5.5-in. boat, which has been cleaned in aqua regia, with 40 g of 99.9999 pct Ga along with 1 to 8 mg of Ga203 powder. GazO3 is a convenient source of oxygen since it reacts with gallium at the melt temperature to form Ga20 vapor, the species which apparently controls the suppression of silicon contamination. The loaded boat, the quartz rod, and the 99.9999 pct As are placed in the ampoule as shown in Fig. 1. Generally, GaAs seeds were not used since most of the unseeded growths resulted in monocrys-tals. The ampoule is evacuated to 10-5 Torr and sealed off. The GaAs melt is synthesized by placing the ampoule into a two-zone horizontal Bridgman furnace. The two zones are separated by several sandwiched layers of -in. Fibre-Fax board drilled with holes slightly larger than the OD of the ampoule. This causes a very large temperature gradient between the two zones, which is necessary for single-crystal growth. The two-zone furnace is mounted on a stand fitted with a roller bearing which allows uniform motion of the furnace in a horizontal direction. A uniform velocity of the stand is achieved by the use of a windlass device which winds up a wire attached to the stand. Movement of the solid-liquid interface is accomplished by fixing the position of the ampoule and moving the stand. Growth rates investigated in this experiment were between 0.4 and 1.2 in. per hr. The composition of the melt is fixed by maintaining an arsenic reservoir at 618°C. The stand is moved away

Jan 1, 1968

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

Several attempts have been made to account for the fact that grains in a fully recrystallized metal will coarsen on annealmg. 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 Jeffriesl 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 Amstel.³ 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 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 on 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 pet 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 condition~ 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, 1949

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 annealmg. 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 Jeffriesl 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 Amstel.³ 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 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 on 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 pet 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 condition~ 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, 1949

By W. H. Bassett, J. C. Bradley

Beads of metal frequently appear at the ends of cast-copper wire bars and on the sides of wedge cakes near the top. These are richer in cuprous-oxide than the rest of the casting. A micrographical study of these exudations has been made. 11 is suggested that the materical is forced through the surface while the copper is solidifying. If not eliminated in process of manufacture, it shows on the finished polished sheet copper in patches differing in color from the main body of the shad. Figures 1 to 4 show the copper exudations, at different magnifications, as they appear on the ends of cast wire bars, and on the sides, usually near the top, of wedge cakes. Sometimes the exudations are in fine "drops;" at other times, large masses of the material are found. Microscopic examination of the copper exudation indicates that it is high in oxide and of eutectic proportions. Because of the difficulty of securing a suitable sample, the protuberances have not been analyzed chemically; but the spectroscope shows no indication that there are any more metallic impurities present than in the balance of the copper. The lowest copper plus silver content of the coppers studied for this paper was 99.914 per cent.; the highest, 99.966 per cent.; so the oxygen content of the whole casting would be well under 0.07 per cent. Structure of Protuberances The segregation of oxide between grains in the interior of the cast bar, not far from the "set," is shown in Figs. 5 and 6. In general, the amount of cuprous oxide begins to increase at a point about 0.01 in. below the normal surface of the casting, i. e., the base of the drop; but it does not attain maximum concentration in the main body of the metal. Vertical sections, Figs. 7 to 12, show that there is a definite line of large cuprous-oxide globules at the base of the drops. Horizontal sections at this place show that these large globules lie in a thin billowy

Jan 1, 1926

By Erwin L. Zodrow

A geological model of the modes of formation of magnetite and its distribution in the Smallwood iron-ore mine, Labrador, Newfoundland, is given, based on observation and geological mapping. This is called the conceptual model. If mathematical expressions plus probabilistic uncertainty are used to represent the conceptual model, then this is termed a mathematical model. The purpose of this paper is to test if there exists a correspondence between the conceptual model and two related mathematical models (called factor analysis). Details of the statistical technique are given. The results of factor analyses in relation to the magnetite formations in the Smallwood mine are discussed. Several practical mine applications are presented. The difficulty of maintaining quality control over ore mined from any deposit naturally depends on geological conditions; these are usually imperfectly known to concerned mining geologists. One geological condition that would greatly facilitate ore predictions is if a relationship between the observed ore particle distribution* and its mode of origin could be demonstrated. Such a casual interrelationship is normally sought through the application of well-defined geochemical principles of primary mineralization in given geological environments. However, the application of conventional tools of geological research, including geochemistry, to areas that have undergone repeated periods of geological deformation and metamorphism subsequent to primary mineralization becomes rather difficult. More important, the interpretation of such research results are nearly impossible on an objective basis. Mineral assemblages may have been reworked and changed due to tectonic influences to the extent that the present-day observable mineralogy and ore-particle distribution can effectively obscure the mode of origin of the ore. Quantitative measurements, based on petrological investigation of mineral assemblages, reflect the sum-total of all geological influences. Which of several influences had the most effect on existing ore particle distribution is difficult to assess, for these influences can neither be measured directly nor quantified by petro-logical logical or geochemical means. The present study is concerned with the magnetite distribution and its modes of origin within the Small- wood mine,&apos; located in the southern extension of the Labrador geosyncline; see Fig. 1. This geosyncline is thought to have undergone at least two periods of geo-tonic tectonic deformation, separated in time, since the fer-rugenous rugenous sediments were deposited." Detailed geological observations and mappings (1 in. to 40 ft) have highlighted subtle, distinctive features of the magnetite distribution in the Smallwood mine: (1) The magnetite is generally concentrated in bands or layers within this ore body; these bands alternate with specularite-rich bands and quartz bands. The banded or layered nature is common in Precambrian iron-ore deposits, and this has been interpreted as a result of changes in depositional environments. (2) The grain size of the magnetite varies; near the contacts between the iron and quartz-carbonate formations, the magnetite occurs as well-crystallized octa-hedra. In areas of intense folding, magnetite is extremely fine grained and concentrated in bands and occurs in association with earthy manganese minerals. (3) Magnetite tends to be more highly concentrated near the geological contacts of the iron and quartz-carbonate formation in the northeast part of this mine, Figs. 2, 3, and 4. (4) Magnetite is also fine grained and tends to higher concentration near and parallel to fold axes; however, in this case, the ore is much softer than given in item 2. (5) Magnetite mineralization decreases along strike and away from the areas of intense folding, i.e., towards the approximate center of the mine, Fig. 3. How can these variations of magnetite be explained on a geological basis? We can postulate a conceptual model that the distribution of magnetite appears to be related to three basic geological influences: (1) geo-tectonics, i.e., concentrations of magnetite near geological contacts of the iron and quartz-carbonate formations, the fine-grained nature of magnetite and its higher concentrations near fold axes, and decrease of magnetite towards the approximate center of the mine; (2) secondary alterations, i.e., variation of grain size of magnetite near the iron and quartz-carbonate contacts, and in areas of intense folding where magnetite occurs together with earthy manganese minerals: (3) original

Jan 1, 1971

By H. Y. Bassett

THIS paper attempts to show the various major operations used in nonferrous tube mills and does not necessarily represent the current practices at the two plants of the Wolverine Tube Div., of Calumet and Hecla Consolidated Copper Co. Inc. The operations now utilized in the production of tubing are quite varied and show the continual interest and advance metallurgically and mechanically to produce the best quality at the lowest cost. Naturally, any advance or lowering of cost is dependent on large production runs, which mean longer machine running time with maximum worker productivity. Standardization of tube sizes and elimination of unnecessary alloys are therefore very necessary, otherwise the development of costly new production machines would be of little benefit to the consumer as a whole. It should be noted that in such a short presentation it is impossible to describe in any detail the major operations. The short descriptions, it is hoped, will enable all who are interested to obtain a general idea of present, day practices in the copper tube producing field. Fig. I is a flowchart or sequence of operations showing the steps usually employed in tube production. RAW MATERIALS Quality starts with the raw material, and it is absolutely necessary that raw material be controlled and held to rigid specifications. Little need be said, however, regarding the raw materials for the casting of bars or billets, as the material always is purchased and checked against the various governing A.S.T.M. specifications. CASTING Casting, as is indicated in Fig. I, is quite varied and for convenience can be classified into two groups: The casting of solid billets, and the casting of hollow tubes, each of which is the base for subsequent operations. In the melting of the raw materials various types of furnaces are used, and the selection of any one is dependent on many factors outside the scope of this paper. However, as of general interest, a short description will be made of each. Induction Furnace (Low Frequency) This is popular in the melting of copper-base alloys, Fig. 2. In the induction furnace the principle of an inefficient transformer is used for the production of the necessary melting heat. The primary coil is.arranged around a transformer core made of high permeability silicon steel sheet. The secondary circuit is through a melting channel around the primary coil and opens into a hearth which contains the main charge. The heat is generated only in the melting channel, but because of the stirring action there is a constant flow of metal around the channel, which when mixing with the charge causes very rapid melting. The volatilization losses are very low as the furnace atmosphere above the charge is heated only by the heat from the melting metal. The stirring action, however, makes the use of any slag cover difficult. Such furnaces- must be started with molten

Jan 1, 1951

At its meeting on February 21, 1933, the Board of Directors passed the follow¬ing resolution defining and expressing the policy of the Institute with respect to official participation or action m controversial matters WHEREAS, the Board of Directors at its last meeting passed the following resolution "The Board of Directors, having been appealed to by several Local Sections for advice concerning the attitude and policy of the Institute relating to the endorsement of candi

Jan 1, 1952