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By V. G. Cawagdan, E. M. Sacris

The performance of the grinding circuit, from the initial stages of operation to the present, is discussed. The mill efficiency as measured by the Bond (Bond and Maxson, 1943) grindability data and the operating work index is presented. The objective was to produce a sand cyclone overflow containing not more than 6% 210 µm (+ 65 mesh). This has never been attained, even at low milling rates. Significant improvements in throughput were achieved by instituting equipment changes and process modifications within the grinding circuit. Grind improvements were achieved with enlargement of cyclone spigots, grinding at reduced densities, and decreasing the opening of the ball mill discharge. Additional grinding capacity was realized by converting the concentrate regrinding mill into a secondary ball mill. The previous 20% 210 µm (+ 65 mesh) grind improved to under 15% 210 µm (+ 65 mesh). The latest approach to solving the coarse grind problem is also discussed.

Jan 1, 1985

By C. L. Siebenthal

C. E. SIEBENTHAL, ? Washington, D. C.-From being one of the most maligned of metals-a veritable bugaboo-cadmium has almost overnight become respectable, though its slender claim to respectability rests almost wholly on the possibility of its substitution for tin. Preliminary to any campaign for such substitution, particularly for enforced substitution, the possible supply of cadmium should he determined as closely as possible; for that reason the statistical inquiry of which this paper embodies the results was undertaken. Production Cadmium is marketed in two forms, as metallic cadmium, in sticks or bars, and as cadmium sulfide, the pigment. The metal has found its greatest field of use in this country as a component of an easily fusible alloy that is used in automatic fire extinguishers. The sulfide is .used to some extent in paints but chiefly to give color and luster to glass and porcelain. The metal was first made in this country by the Grasselli Chemical

Jan 12, 1918

By F. Habashi

Conclusive evidence is given showing that the dissolution of gold in cyanide solution follows mainly the over-all equation A similar equation can also be written for the dissolution of silver. Theoretical derivation of the velocity equation for this reaction has been obtained, which describes quantitatively the experimental facts. The equation is as follows: where [CN-] and [O2] = the concentrations (in moles/ml) of cyanide and dissolved oxygen, respectively. DcN- and Do2 = the diffusion coefficients of cyanide and dissolved oxygen; 1.83 x 10-5 and 2.76 x 10-5 cm2 sec-1, respectively. A = the surface area of the metal in contact with the aqueous phase, in cm S = the thickness of the boundary layer; varies between 2 and 9 x 10-3 cm, depending on the speed and method of agitation. Rate being expressed in g. equiv. sec-1. INTRODUCTION During recent years a number of papers have been published on the kinetics of dissolution of gold and silver in cyanide solution.1,6 The authors agree that the rate of dissolution is diffusion-controlled, but disagree regarding the mechanism of the reaction. Some authors'-3 support the Bodlander equations: The apparently conflicting results, when critically reviewed, are concordant and lead to the conclusion that the proper equation for the dissolution reaction should be only Eq. 1. This conclusion is based on the following facts: 1) For every 2.2 equivalents of metal dissolved one mole O2 was consumed. 2) For every 1 equivalent of metal dissolved, 2 moles of cyanide were consumed.' 3) Hydrogen peroxide is formed during the dissolution of gold or silver, and for every 2.2 equivalents of metal dissolved, one mole H2O2 was produced.1,2 The fact that Kudryk and Kellogg4 did not detect H2O2 during the dissolution of gold should not throw doubt on the many affirmative reports of other investigators. Lund2 has shown that depending on the crystalline nature of the silver surface, (e.g. method of etching the sample) H2O2 may undergo catalytic decomposition heterogeneously according to: Further Kudryk and Kellogg4 carried out their experiments in the presence of 0.5% KC1 to achieve a greater electrolytic conductivity, and Matsudaira7 has shown that H2O2 is catalytically decomposed (homogeneously) in the presence of C1- ion in alkaline solution. 4) Experiments carried out by Boonstra8 and Lund2 showed that the dissolution of gold and silver respectively in KCN + H2O2 in the absence of oxygen was a slow process. Thus the reaction takes place to a minor extent only. Further kinetic studies showed that: 1) The rate of dissolution depends on the surface area of the metal in contact with the liquid phase, thus indicating that the process of dissolution is a heterogeneous process. 2) The rate of dissolution depends on the speed of stirring,5,6 thus indicating that the process is controlled by a physical phenomenon.

Jan 1, 1967

By Hans Lundberg, Theodor Zuschlag

Based upon an instrumental improvement, a new development has taken place in the art of electrical prospecting, and some remarkable results have already been obtained with regard to potential exploration. In order to visualize the importance of this development, it is deemed advisable to review briefly the fundamental facts about potential surveys. Potential exploration may be carried out qualitatively or quantitatively. Qualitative investigations are made by determining and plotting on a map points of equal potential, whereby any anomalies are revealed, without, however, much clue to their magnitude. Quantitative investigations determine the variations of potential or potential drop, and thus show not only the location of the anomalies, but also their magnitude. Figs. 1 to 6 illustrate the influence of simple types of ground inhomo-geneities, assuming one effective exciter potential only. Such a condition can be closely realized by connecting an electric current source to two electrodes, one of which is located at a great distance. Assuming uniform ground resistivity, the resultant potential distribution mar be represented by concentric spheres. Any change from the normal condition causes a characteristic distortion of the spheres, which becomes different for different types of resistivity variation. The series of Figs. la to 6a illustrates schematically results of qualitative investigations and series lb to 6b results of quantitative investigations. Figs. 1 and 2 picture the well-known case of local resistivity variations normally encountered in ore prospecting. Figs. 3 and 4 show the reactions caused by more or less vertical resistivity contacts and Figs. 5 and 6 refer to the problem of ground-water and bedrock investigations where the resistivity contact is horizontal or nearly SO. It is evident from Figs. 5a and 6a that qualitative measurements do not permit an identification of such general geological features as widespread horizontal strata, because the resultant contraction or expansion of the equipotential circles at the surface cannot be recognized without quantitative determinations. On the other hand, qualitative measurements are well suited for the exploration of local or lateral resistivity

Jan 1, 1932

By L. J. Cabri

The calculation of metallurgical balances for precious metals is very dependent on a precise mineralogical understanding of the distribution of each element. Determination whether the precious metals occur as dilute solid solutions in major minerals is not always easy because of the relatively high levels of detection (9200-500 ppm) of the precious metals by the most common methods of in-situ analysis (e.g. electron microprobe). Particle Induced X-ray Emission (PIXE) analysis of sulfides from Izok Lake, N.W.T., Canada and from the Hilton mine, Mount Isa, Australia with a proton beam (proton microprobe) confirms solid solution of Ag in chalcopyrite from both deposits. In addition, chalcopyrite and sphalerite from Izok Lake both contain indium.

Jan 1, 1984

By K. Sallmann

Spurred by a variety of factors, coal flotation is making headway among the preparation plants of West Germany. Mr. Sallmann provides a general view of flotation practices being employed in his country, with special emphasis on the many-sided problems that confront German coal preparation engineers.

Jan 9, 1961

By C. W. Jr. Gennet

ANNOUNCEMENT was made in the spring of 1926 that the Boston & Maine R. R. Co. had contracted with the well known German steelmakers, Messrs. Fried Krupp, for the manufacture of 15,000 tons of basic open-hearth steel rails at the Rheinhausen Works, for delivery to Boston, Mass. The manufacture of rails in the United States has for many years been almost a national pride, and as this feeling is chiefly the result of a long-time liberal and consistent patronage of, American rails by American railroads, it is not strange that this somewhat unusual announcement should arouse more than ordinary interest. Since the end of the World War, the importation of foreign rail has been fairly large, principally because the newly created economic conditions have rendered some American competition more difficult, but the tonnage imported, for the most part, has been made up of small orders for miscellaneous use; and the contract referred to constitutes the largest single importation of foreign rail in over ten years. In 1915, the Algoma Steel Co. of Sault Ste. Marie, Canada; supplied the Illinois Central R. R. with 30,000 tons of rails,1 and various other American roads with smaller amounts. In 1902, 1903 and 1904, large tonnages of rail from abroad were purchased, the Louisville & Nashville R. R. alone obtaining 30;000 tons from German mills. It is the object of this paper, to present, in what is believed to be a new and concise form, figures showing the production and consumption of rails in the United States, and to record some of the testing and inspection results of the recent Krupp rails; also, to direct attention to two quite unique departures from American practice that were regular features of the Krupp process and which are worthy, it is thought, of careful study.

Jan 1, 1928

By Dennis V. D’Andrea, Larry R. Fletcher, Peter G. Chamberlain

The evaluation of potential in situ copper leaching deposits requires a thorough examination of the geologic, mineralogic, hydrologic and physiological characteristics of the ore body. The decision to develop the deposit is made with these data along with leaching properties, estimated copper recovery, and economic analysis. A test blast followed by pilot leaching can a so be used for further evaluation and to reduce uncertainty regarding the deposit's potential. This report describes a number of ground characterization techniques that can be used to evaluate potential deposits. Field methods include geologic mapping, groundwater hydrology, core drilling, geophysical logs, permeability testing, and in-situ stress measurements while laboratory tests include assaying, mineralogy, leaching, rock physical properties, size analysis, and computer simulation.

Jan 1, 1980

By Ned Kuenhold

AN equipment manufacturer swallows a bitter pill when he sees his machinery improperly in- stalled and not used to the full potential. This frequently happens with vibrating screens. Screens can be classified according to the path of vibration imparted to the screen surface. On this basis there are: 1) vertical circle or modified circle throw, 2) horizontal circle or modified circle throw, 3) vertical linear reciprocation, 4) tilted linear reciprocation, and 5) horizontal linear reciprocation. The most versatile vibration for medium to coarse sizing is generally conceded to be the vertical circle produced by an eccentric or unbalanced shaft, but other types of vibration may be more suitable for certain screening operations, particularly in the finer sizes.

Jan 6, 1957

By E. S. Machlin

RECENTLY, there has been much activity in the field of nucleation of martensitic transformations.'- One of the problems in this field is the calculation of the rate of nucleation (number of plates nucleated per unit untransformed volume per unit time) in terms of observable parameters. Two such observable parameters are the fraction of the length of a straight line which corresponds to the portion of the total length of the line that lies in the martensitic phase and the number of plates intersected by this straight line per unit length of line. Because of the necessity of a valid answer to this problem, the following investigation was undertaken. Although this problem has been treated in the past, a derivation of the relation between the volume and linear fractions of martensite will be described to illustrate the method used in the succeeding analyses. It is assumed that the martensitic plates are in the form of a right circular cylinder having a small height relative to the radius of the base. The volume fraction of martensite is then: fr = lXNl,hjAl [1] where f, is the volume fraction of martensite, and Nij is the number of plates per unit total volume having the area Ai and the height hi. The linear fraction of martensite is obtained as follows. For the plates having the particular area A, and height h,, the fraction sin 0 dB* will have their cylinder axes between the angles 0 and 0 + d0 to the straight line along which the linear fraction of mar-

Jan 1, 1953

By P. E. Doherty, R. S. Davis

Sub boundaries and micropores, as well as certain other imperfections, may be revealed in aluminum by the formation of pits on the surface during cooling from elevated temperatures. The pits are attributed to the condensation of vacancies from supersaturated solution. This "vacancy pit" phenomenon has been used as an etching technique for studying the structure of aluminum specimens grown from the melt. Three fundamental structures were studied: stria-tions, cells, and dendrites. Two types of striations, as well as a crosswise structure are reported. Mic-roporosity is observed to occur in the cell walls on freezing. Subboundaries between primary, secondary, and tertiary branches are observed in dendritic growth. A special case is cited in which cellular growth suppresses the formation of striations. SMALL, well-defined pits have been observed to form on the surfaces of electropolished aluminum specimens during cooling from elevated temperatures.' This phenomenon was attributed to the condensation, from supersaturated solution, of vacancies at particular points on the surface. It was shown that the amount of cooling required for the formation of pits increased exponentially with decreasing holding temperatures in a way that was consistent with the thesis that a critical supersaturation of vacancies was required for the pits to form. Pits do not form in the vicinity of certain imperfections, namely, subgrain or normal graind boundaries, phase boundaries, certain surface irregularities, and pores. The width of the pit-free region increases with decreasing cooling rate. This observation suggests that the imperfections in question are effective sinks for vacancies and that the pit-free region around them is material that is not sufficiently supersaturated with respect to vacancies to nucleate the surface pits during cooling.

Jan 1, 1962

By Basil B. Zavoico

During 1937 the Russian oil industry made very satisfactory progress in its exploration branch and added considerably to its proven reserves in the older producing districts, while several entirely new potential areas were opened for development by discovery wildcats. The exploitation of known fields, however, suffered greatly from internal political difficulties, referred to as "sabotage," and was also seriously handicapped by the requirements for national defense under the duress of a grave international situation. More particularly, the necessity for preparing for a major war resulted during 1937 in short-rationing of the oil industry in its iron, steel and rubber requirements, affecting quantitatively drill pipe, casing, tubing and the rubber equipment of automobiles, and qualitatively much of the oil-field machinery for which it was either impossible or difficult to obtain iron or steel of required specifications, which necessitated manufacture of heavier and unwieldy equipment and caused directly and indirectly an unavoidable major curtailment of drilling operations below the planned footage. War-preparation measures during 1937 also required accumulation of a large gasoline reserve in the Vladivostok area and inasmuch as shipments from California can be made much more cheaply than from Caucasian refineries, either by tank cars across Siberia or by tankers via Suez Canal and Indian Ocean, some 2,000,000 bbl. of gasoline was imported from the United States in the past year, resulting in a decline of 46.98 per cent in net exports of all petroleum products from Russia below the 1936 net export volume, which is the lowest level since 1925. Production of crude oil during 1937 is estimated at 212,742,000 bbl. as compared with 202,543,700 bbl. produced in 1936, an increase of 5.04 per cent, but 11 per cent below the planned output. There were no major readjustments as to the source of crude-oil production, Baku district still accounting for the largest share; that, is, 77.21 per cent of the total. Exploration operations were outstandingly successful during the past year, major discoveries having been made on the Apsheron Peninsula, in Grozny and Maikop-Kuban districts, in Ural-Permian Basin, in Middle Volga-Samara district and other areas.

Jan 1, 1938

By I. R. Kramer

The stress associated with the high-dislocation layer at the surface of deformed aluminum crystals was measured by progressively polishing the specimen and determining the change in the initial flow stress when the specimen was reloaded. This surface stress increased linearly with strain in the Stage II and Stage III region. The depth to which the high-dislocation layer extends was found to be 0.0025 in. The influence of the surface layer on Stage I is discussed and it is shown that Stage I ends when, on the secondary slip system, the difference between the applied stress and the opposing stress due to the surface layer is equal to the critical resolved shear stress. In previous papers'-3 it was shown that the surface exerts a pronounced effect on the plastic-flow characteristics of metals. For fcc metals it was possible to increase the extent and decrease the slope of Stages I and II and decrease the work-hardening coefficient of Stage II by removing the surface of the specimen continuously during the deformation process.2,3 More recently,L it was shown that the activation energy for plastic deformation and the activated volume were also influenced by the surface. These changes were related to the existence of a high concentration of dislocations in the region near the surface of the deformed specimen and it was concluded' that the effective stress, T, acting on a dislocation was T = Ta-Ti-Ts [1] where 7, is the applied shear stress, Tj is the internal stress, and TS is the stress associated with the surface region containing the high concentration of dislocations. From Eq. [I] it is seen that the effective stress, 7, acting on a dislocation is a function of 7,. Therefore 7, becomes important in any description of the work-hardened state. In this paper the value of 7, as a function of strain and its variation with depth are reported for aluminum single crystals. In particular, it will be shown that the end of Stage I occurs when the net stress, 7, on the secondary slip system is equal to the critical resolved shear stress. To measure Ts, single crystals of aluminum were deformed in tension to various strains, whereupon the load was removed and a known amount of metal was removed by electrolytic polishing. The differ- ence between the final flow stress before the specimen was unloaded and the initial flow stress upon reloading is designated as ?Tp and is the decrease in the stress due to the removal of the surface layer in whole or in part. The value for Tp is taken equal to -Ts. EXPERIMENT PROCEDURE The details of the tensile apparatus, method of electrolytic polishing, and crystal preparation were the same as those used previously,1"3 The single crystals were 1/8 by 1/8 in. in cross section with a 3-in. gage length. The initial purity of the aluminum was 99.997 pet. The specimens were held in vacuo at temperatures 50°C below their melting points for 16 hr and furnace-cooled. Just prior to the application of the tensile stress the specimens were electrolytically polished to remove 0.004 in. from the thickness. This latter operation was conducted after the specimen was placed in the tensile apparatus. The tensile tests were conducted at a strain rate, i, of 10"5 sec-' and a temperature of 3°C. The aluminum crystals used for the determination of 7, are designated A1-3-12 and A1-116. The orientation of the various crystals used throughout the investigation is shown in Fig. 1. The ?Tp values for specimens A1-3-12 as a function of Ax were determined mainly at four strain levels, i.e., ? = 0.0217, 0.0381, 0.0593, and 0.075, where Ax is one half of the total reduction of the thickness after polishing and ? is the re-

Jan 1, 1965

By H. E. Stauss, E. I. Salkovitz, F. W. von Batchelder

EXISTING information regarding the structure of a spherulite in nodular cast iron is based on optical studies. According to these data, a nodule consists of an aggregate of graphite crystallites radiating from the center, with the closely packed basal planes at right angles to the radii. The c axes lie along the radii. This view faces some uncertainty in the fact that the c axis does not represent the accepted direction of fastest growth in graphite. To supplement the optical information, X-ray studies have now been made. The principle used was to screen the nodule in greater part from the X-ray beam and expose only a minor cap. As successively larger portions of the nodule were introduced into the X-ray beam, any differences in the X-ray patterns could be observed. Such photographs have been taken with chromium radiation and a Laue camera. The graphite nodule itself, about 0.010 to 0.025 in. in diam, was mounted with vaseline on a micrometer screw for control of the linear motion. The nodule rotated about 45" each time that it was translated linearly. The nodules were obtained from magnesium-treated hypereutectic iron by electrolytic solution of the iron in hydrochloric acid. In Fig. la is shown the pattern of the thinnest cap examined. In Fig. lb is shown the pattern of the same nodule moved 0.003 in. farther into the X-ray beam, and rotated 45" at the same time. Figs, la and lb indicate incomplete circles for graphite (the two outer circles arise from graphite) with the side arcs much weaker than the top and bottom ones. The arcs obtained are themselves not continuous in intensity but vary with maxima of intensity some 15" and 30" apart. The structure of the nodule that would give rise to such a pattern can be explained as follows. Basically the nodule consisted of small crystallites. The discontinuous character of the diffraction rings demonstrates that the nodule was not composed of randomly oriented crystallites. The strong vertical reflections and the weak lateral reflections show that the reflecting planes were roughly normal to the radii. The absence of sharp reflection spots suggests that the nodule did not contain large crystals. The sharpness of the diffraction rings in their radial direction shows that the variations in intensity along the arcs were not the result of line broadening resulting from extremely small crystals. In the diffraction patterns two rings corresponding to graphite were found. The third and inner ring in the figures originated in the vaseline. The graphite rings correspond to the a and ß lines reflected from the basal planes, showing that the radii of the nodules are the [0001] direction normal to the basal planes of graphite. The picture of the structure that is formed is, therefore, one of aggregates of crystallites. Within each aggregate the c axes of the crystallites tend to align themselves in the radial direction of the nodule, although these axes deviate somewhat in direction by a continuous variation of angle. Correspondingly the basal planes of the graphite crystallites are generally normal to the radii. It is a pleasure to acknowledge the assistance of M. C. Bloom and R. P. Dunphy of this laboratory.

Jan 1, 1952

By R. B. Woodworth

INTRODUCTION IN the sinking of bore holes, there are but two fundamental operations -drilling and hoisting,-which determine in the main the character of drilling mechanism and structures. There are endless ramifications, however, in the execution of these fundamental operations, according to the purposes for which the bore holes are drilled, their maintenance after completion, the protection and convenience of workmen, etc. The three main lines of use for bore holes are in mineral exploration, the sinking of water and salt wells, and the exploitation of petroleum and natural gas. This paper has to do more especially with the last. Here again there are many divergences. Wells may be drilled by either the percussive, the hydraulic, or the abrasive method. Finally, each of these methods, as applied by drillers of diverse nationalities, has followed somewhat different lines of development. The American system of cable-tool drilling has perhaps had the widest application; the hydraulic rotary is also in extensive use; but the Canadian system, the Galician system, and the Russian free-fall system all have their points of recognized merit and are preferred by operators accustomed to their use. These differences in drilling procedure, which rest ultimately on essential variations in geological conditions, are reflected in the chilling structures as well as in the drilling mechanism. The purpose of the present paper is to record those stages in the development of the application of steel to the construction of drilling mechanism and structures with which the writer has been intimately associated, and to contribute to the history of the art of drilling other data acquired in the course of his personal investigations. It is necessarily limited by reason of space to American practice, with especial reference, therefore, to the cable-tool system and the hydraulic rotary method of drilling wells for oil and gas.

Jan 11, 1915

By Charles Fulton

The study of the condensation of zinc from its vapor was undertaken to shed light on certain problems encountered in large-scale electric zinc-furnace work recently conducted. It is a matter of common knowledge that one of the disadvantages of the arc type, electric zinc furnace, is the production of a large amount of blue powder and proportionately little liquid spelter, for, as stated by Stansfield,1 "A notable defect in the electric smelting of zinc ores is the difficulty experienced in obtaining the distilled zinc in the liquid state; when zinc ores are smelted electrically, very little liquid metal is commonly obtained, nearly all of the zinc being in the state of powder."

Jan 8, 1918

By Walter Kauzman

ALL viscous or plastic flow of incompressible matter is the result of shear strain; the changing shape of any body that is being plastically deformed can be completely described in terms of the shear strain occurring at each point in the body.[t] Furthermore, the relative amounts of shear strain occurring in different parts of a body under stress depend upon the relative rates of shear strain at those different points, so that if the dependence of the shear rate of any material on the temperature, shear stress, previous history, etc., were understood, the principles of plastic deformation would be known, and we could calculate how a body made of a given material, having a given shape, and subject to a specified system of forces, would change its shape with time. It may be said, then, that the problem of plasticity resolves itself into, first, the problem of the rates of pure shear processes, and second, the application of what is known about pure shear to actual cases. It is the purpose of this work to investigate the former problem -i.e., the dependence of shear rates on temperature, stress, etc.-from the standpoint of recent developments in the field of chemical-rate theory and with particular reference to the phenomena occurring in the creep of metals and in the plastic flow of crystalline solids in general. It is left for the mechanical engineer, and perhaps the expert in hydrodynamics, to deal with the problem of applications.1 RESOLUTION OF MACROSCOPIC SHEAR INTO MICROSCOPIC MOVEMENTS; RESEMBLANCE TO CHEMICAL REACTIONS Just as any large body is made up of many small units, or atoms, so macroscopically observable shear is the result of many microscopic unit shear processes; just as the understanding of the behavior of large bodies demands the understanding of the atoms of which it is made, so the understanding of macroscopic shear demands the understanding of these fundamental unit processes. The study of shear from this "atomistic" point of view has made considerable progress. There has been fairly complete understanding of shear processes in gases for a long time, at least for nonturbulent flow, as a chapter on gaseous viscosity in any text on the kinetic theory of gases will prove. In recent years Andrade2 and Eyring3 have presented important theories for the flow of liquids and amorphous solids. Becker,4 Orowan,5 Taylor,6 Burgers,7 and Kanter8 have considered the

Jan 1, 1941

By David C. Yang

INTRODUCTION Over the world, and especially in the United States, there is increasing dependence upon progressively lower grade ore deposits. These lower grade ores are frequently difficult or impossible to process due to complex mineral assemblages being very finely disseminated. Thus, many of the conventional mineral concentration methods are not applicable to these ores. For the last few decades, research in the more exotic mineral processing techniques has been conducted, both in universities and in governmental and industrial laboratories. Since its inception, the Institute of Mineral Research of Michigan Technological University (MTU) has devoted much of its attention to the problems of processing refractory, low grade ores. Recently a new flotation system was developed which shows promise of being applicable to a broad range of ore types. This process has been the subject of two allowed patent applications. This paper describes the details of such a flotation system which is potentially useful for treating ultrafine minerals. Some highlights of the testing program on a variety of iron ores and a group of lithium-bearing ores will be presented. EXPERIMENTAL PROCEDURES Both iron and lithium ore flotation treatments followed the same general procedures, with minor differences in pH and in reagent dosages. The method is rather simple, efficient and economical from the standpoint of recovery and the cost of reagents consumed.

Jan 1, 1979

By Forrest V. Williams

The dislocatiorl and stacking-fault structuve of epitaxial GaAs1-,PX lms been examined by chemical etching. The layers were groun in the (100) direction and etch Pils were developed on (111} planes which nad been lapped and polished on the epiLaxia1 layevs. Tile effecL of the jollolcing cariables on the quality of the epilaxial layers has been examined: doping leuel, grouth rate, and composition. High stacking-faullL densilies weve found in the GuAsi_xpx layers. These are not observed in heavily dolled epitaxial layers tzar in layers with low phosphorus compositions. The dislocatiorz density in GuAsi-x px was highest at the sub-stvate- epilaxia1 layer interface. Composilion changes introduced dislocations in the epitaxial layers. ManY semiconductor p-n junction lasers of Group TIT-Group V compounds and their alloys have been reported in the past several years. Laser action at visible wavelengths in GaAsl-x,Px was first reported by Holonyak and Bevacqua. GaAs, a direct transition semiconductor which lases, and Gap, an indirect transition semiconductor which does not lase, form a continuous series of solid solutions.2 Laser junctions can be fabricated in GaAsl-xPx crystals with phosphorus compositions up to about 40 mol pct. In addition to the production of coherent radiation in these crystals, the efficient recombination radiation of p-n junctions in this material has equally important potential in the development of low-power semiconductor lamps. To achieve a high conversion efficiency of electrical to optical energy in p-n junctions in this material, the relation of physical properties of the crystal to luminescence efficiency must be better understood. Although the electrical, optical, and device properties of GaAsl -xPx junction lasers are understandably of considerable interest, the work to date indicates that the more serious problems are the chemical and metallurgical difficulties encountered in the growth of this material.3 In addition to the problems of chemical purity, crystal imperfections, such as dislocations and stacking faults, can be expected to affect both the efficiency of the radiative recombination process and the perfection of the p-n junction.3 The last requirement, i.c., that of the perfection of the p-n junction, is a particularly troublesome one in the fabrication of laser diodes. To obtain good laser diodes, the p-n junction must be flat, which permits the radiation to be reflected from the resonant cavity boundaries. Junction planarity is extremely sensitive to the crystal perfection of the semiconductor material. Also, it is known that at high dislocation densities (-105 per sq cm) it has not been possible to build laser junctions in GaAsl-xPx . Few studies have been reported on the crystal defect structure of GaAsl-,P,. The first serious study seems to be that of Wolfe, Nuese, and Holonyak,3 who examined the dislocation structure of monocrystalline bulk (nonepitaxial) material grown by halogen vapor transport. In this paper are reported some observations on the dislocation and stacking-fault structure of GaAsl_,P, crystals grown by a vapor transport process on substrates of GaAs. EXPERIMENTAL Crystal Growth. The GaAsl-xPx crystals were grown in an open-tube flow system, using two sets of reagents. GaAs, Pr(red), and HC1 were employed in one method. The transport reaction is =950JC GaAs+HC1 = GaCl +1/4As4 +1/2H2 and the deposition reaction is 2GaAs1-xPx +GaCl3 Composition control is obtained by the flow rate of the HC1 and the vapor pressure of the P4, which is maintained in a separately controlled furnace. The second method has been described by Ruehr-wein4 and utilizes gallium, AsH3, PH3, and HC1. The same transport and deposition reactions as above are involved. Composition control is obtained solely by the flow rates of the three gases involved. All of the crystals were grown on chemically polished GaAs substrates oriented on the (100) plane. The thicknesses of the epitaxial layers were typically 100 to 300p. Revealing of Dislocations. Dislocations were re-vealed on both the( 111 ) and { l l l }b faces by chemical etching. The specimen to be examined was mounted at 54.7 deg, lapped on glass with 3-p alumina, polished on cloth with 3-p diamond paste, and, to remove work damage, chemically polished at room temperature for

Jan 1, 1968

By C. G. Dunn, P. K. Koh

THE primary recrystallization texture in cold-rolled silicon iron, which is the matrix texture for developing the Goss texture or the cube-on-edge texture by secondary recrystallization at temperatures near 900°C,1-5,21 has not been adequately described. Thus from the present available information, it is not possible to explain satisfactorily both the grain-growth selectivity of the matrix and the often observed magnetic torque curve, which itself provides some information on the texture. Also lacking is information on the special annealing texture that develops in this material when the annealing temperature is 1200°C or higher and the rate of rise to temperature is extremely rapid. From the work of May and Turnbull5 and from unpublished work, it was known that isothermal annealing near 1200°C tends to reduce the extent of secondary recrystallization and that a much weaker cube-on-edge texture results if appreciable normal grain growth replaces secondary recrystallization. Koh and Dunn6,7 have obtained additional information on complex primary recrystallization textures from further studies made after normal grain growth. In these instances the initial textures were retained during normal grain growth. A similar result reasonably could be expected in the present study except for the presence of a grain growth ihibitor1-5,8,9.21 and its tendency to allow only a few grains to grow. However, any information on the orientations of grains in the special annealing texture, even if far from representative of the initial matrix texture, would provide useful information on the nature of the matrix texture. In the present texture study the method of Newkirk and Bruce,10 which is based on the methods of Geisler" and Schwartz, 12 is used to obtain a complete (110) pole figure of the primary recrystallization texture. The high-temperature annealing texture is determined simply from the orientations of a large number of selected grains. The kinetic nature of the process that produces the annealing texture is treated elsewhere13 and it is shown that a form of secondary recrystallization with a very high rate of nucleation occurs during rapid annealing at high temperatures. EXPERIMENTAL PROCEDURE Commercial 0.014-in. cold-rolled silicon iron strip (3.16 wt pct Si), prepared by two stages of cold rolling with an intermediate short anneal, was given a decarburizing 3-min anneal at 800°C. Me-tallographic studies indicated complete recrystallization. Short-time anneals at 900° C and at higher temperatures proved that secondary recrystallization had not begun at 800°C, in fact, the short additional anneals were still in the induction period of secondary recrystallization. A rapid rise to an annealing temperature of 1260°C (2300°F) was obtained in a BaC12and NaCl fused salt bath. The structures that resulted from anneals in the range 12- to 1000-sec duration were relatively finegrained, even though the growth was a form of exaggerated grain growth13 or secondary recrystallization with a high nucleation frequency.= Many of the grains were large enough for an X-ray study using a 5-mil X-ray beam. A transmission Laue Camera and an optical-mechanical stage for moving the grains into the X-ray beam were used. A total of 325 grains were X-rayed in this manner and the grain orientations determined. Complete (110) pole figures were obtained for the primary recrystallization texture using CoKa radiation at 30 kv in the back-reflection range, such as (220) for (110) poles, as described recently by Newkirk and Bruce.10 The low voltage serves to reduce the spurious white radiation to a minimum. A filter of 0.001-inch iron foil was located in front of the detector slit for transmission and in front of the beam slit for back reflection. A new and improved specimen holder extended the useful tilting angle range for transmission to 70 deg instead of 60 deg as previously reported.' A torque magnetometer was used to obtain the magnetic torque curves for a number of l-in. diam disk specimens. RESULTS The (110) pole figure of the material after recrystallization at 800°C is shown in Fig. 1. The positions of the pole concentrations are found to be

Jan 1, 1961