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By T. C. Campbell

Copper is extracted from the Chuquicamata oxide ore by a hydro-metallurgical process. The ore is crushed to 3/8-in. sizing, and leached with a sulfuric acid electrolyte. Chlorine is precipitated. and the ferric iron reduced in the enriched electrolyte, after which the copper is recovered by electrolysis with insoluble Chilex and lead-antimony anodes, the spent electrolyte being returned to leaching. Cathodes are melted and refined in market furnaces and cast into commercial wire-bar and cake shapes. Sulfuric acid for the process is supplied by the brochantite in the ore. Water for washing the ore is advanced through the solution system and finally after cutting by electrolysis to from 6 to 16.0 grams per liter is completely stripped by the cuprous chloride method and run to waste. The cuprous chloride so obtained plus that resulting from precipitation of chlorine from strong solution is dissolved in ferrous chloride brine and the copper cemented on scrap iron. The cement so obtained is in part used to reduce ferric iron in electrolyte, and as it is of exceptional purity is also furnace refined and cast into an exceptional quality of fire-refined copper. Fig. 1 is flow sheet of the operation. The reduction plant is composed of seven divisions as follows: (1) crushing, (2) leaching, (3) tailings disposal, (4) dechloridizing, (5) sulfur dioxide treatment, (6) electrolytic tank house, (7) smelting and melting. A brief description of each of these divisions will be given. Crushing Ore that is frequently blocky and up to 5 ft. in section is crushed in four stages to 3/8-in. mesh. The first stage of crushing is called primary and the next three stages are known as secondary crushing. The first stage is accomplished with two 60-in. Superior McCully gyratory breakers by which the ore is broken to 9 in. The second coarse gyratory breakers crush the ore to 3-in. sizing. There are seven No. 10 McCully gyratories in this service, for one of which recently has been substituted a No. 7 cone crusher. The third and fourth stages of crushing are accomplished by fifty 48-in. disk crushers. In the third stage 14 disk crushers break the ore to 1 in., and in the last stage 36 disk crushers turn out the final product of 0.371-in. sizing. Reference to the flow sheets of Figs. 2 and 3

Jan 1, 1934

By E. Orowan

LONG before the role of dislocations in the plastic deformation of crystals was recognized, the stress-strain field around dislocations received considerable attention in the theory of elasticity. It seems that Weingarten1 was the first to consider dislocations as simple and typical sources of internal stress in elastic solids, and Volterra2 and Timpe3 investigated their elastic field. Fig 3-1 shows the two basic types of dislocations considered by Volterra. The first arises by making a straight-edged .plane cut in a solid, displacing the two surfaces of the cut in their own plane relatively to one another by a constant amount in a direction perpendicular to the edge, and welding them together; this is shown in Fig 3-la, where the outer cylindrical surface represents the boundary of the solid, and the thin spiral cylinder around the edge of the cut has been removed in order to avoid infinities of stress and strain. The second type of dislocation is shown in Fig 3-lb; here the surfaces of the cut have been displaced relatively to one another by a constant amount parallel to the edge, and then welded together. After J. M. Burgers,4 these two types are called edge and screw dislocations, respectively. They represent simple limiting cases; in the general case, the surfaces of the cut are displaced by a constant vector that lies in the plane of the surface but has components both parallel and perpendicular to the edge of the cut. This vector is the Burgers or slip vector. The name “dislocation” was given by A. E. H. Love;5 it was bor-

Jan 1, 1954

P. H. ARGALL, Magdalena, N. Mex. (written discussion *).-The Chilean mill has generally been considered a fine-crushing machine and as such has had many advocates; it has also. had quite a number of denouncers; hence, the action of the Portland engineers in using the Chilean mill for the preparatory work usually accomplished in, rolls or rock breakers and adding a ball mill to do the fine grinding is novel, though of doubtful utility in the long run, even though a fair efficiency is obtained for the combination machines, as measured by Chilean mill practice. In order to follow the development of Chilean mill practice on Cripple Creek ores, I might say that two 6-ft., Chilean mills were placed in operation in Stratton's Independence mill in April, 1908, treating ore crushed by rolls to pass Y4 in. screen aperture. Screening was, however, found to be an unnecessary refinement, as was also the use of plows in the mills; both screening and plowing were abandoned before the Portland engineers finished the experiments in stamp milling upon which they were then engaged. Two additional 6-ft. Chilean mills were added in the spring of 1911, three of them giving the required 10,000 tons per month capacity, one being always in reserve. The Portland company began using Chilean mills in June, 1910, at its Victor mill, and the same company purchased the Stratton's Independence mill in June, 1915, and remodeled it; it is now known as the Independence mill. A description of Stratton's Independence milling practice, is given in the November, 191.1, issue of Mining Majazine (London). These Chilean mills were used as fine grinders and that they accomplished their purpose is shown by the screen analyses, in which 62 per cent. of the pulp passed 150-mesh screens. To make coarse crushers of these Chilean mills, the Portland engineers have increased the speed, substituted steel in various parts for cast iron, provided new and enlarged thrust bearings to take care of the centrifugal force incident to higher speed, and have, thereby, greatly increased the cost of the machines. They have also reduced the width of the tires and dies from 8 in., as used in the original mill, to 7 in., a reduction of 12 ½ per cent. in the crushing surfaces, to say nothing of the loss of abrasion or attrition incident to the larger surface. At the same time, they have apparently increased the weight of the rollers by using tires 5 7/8 in. thick as against tires varying between 3 and 4 in. on the original mills, thereby increasing

Jan 4, 1920

By R. D. Pehlke, J. V. Gluck

A study was made of the effect of small additions of metallic solutes on the thermodynamic activity of zinc in dilute solution with molten bismuth in the range 450o to 650°C. The experimental measurements were made in a multielectrode galvanic cell using. a fused LiCl-KCl electrolyte. The activity of zinc in binary solution exhibited a strong positive deviation from Raoult's law and obeyed Henry 's law to at least 0.050 mole fraction. The ternary addition of lead, gallium, or indium increased the activity of zinc. Cadmium or tin additions slightly decreased the zinc activity. Copper, mercury, silver, or antimony caused moderate decreases, while gold strongly decreased the zinc activity. The results are expressed in terms of Wagner's interaction parameter ejZn and a second-order cross-interaction parameter. The interactions for copper, gold, silver, and antimony showed a linear dependence with reciprocal absolute temperature, while the other interactions were essentially independent of temperature over the experimental range. Since tin and antimony decreased the zinc activity, the hypothesis of a purely periodic variation with atomic number was rejected. A semiquantitative explanation was possible with a free-electron model when relative electronegativities were used to express changes in the electron/atom ratio caused by the solute addition. Random solution and quasi-chemical models correctly predicted the majority of the interactions for which binary data were available to apply them. A knowledge of the thermodynamic interactions in liquid (and solid) metallic solutions is of considerable theoretical and experimental interest in the formulation of quantitative thermodynamic relations for metallurgical processes. The approaches to defining the interactions may be either phenomenological (i.e., "What mathematical function adequately describes observed behavior and permits extrapolation to new situations?") or theoretical, such as a specific model

Jan 1, 1968

By W. A. Backofen, B. C. Wonsiewicz

The Plasticity transition in magnesium was studied by plane-strain compression of single crystals and polycrystalline material at temperatures from about 20" to 307°C. Reduction of single crystals along the c axis was accommodated by twinning on {1011) and retwinning on (10 12}, followed by basal shear in the doubly twinned volume. Deformation in that mode can result in sufficient independent shears for arbitrary shape change. Fracture in c axis compression, below about 100°C, has been related to excessive shear caused by unloading from the stress for {1011} twinning (-50 ksi at 20°C) to that for slip within the twin (-3 ksi); ductility follows from heating because the stress difference is lowered and the twin volume, in which elastic strain energy is dissipated on unloading, is increased. The stress for (1011) twinning is strongly temperature-dependent but not given by a critical resolved shear stress law. The latter is attributed to the influence of stress concentration from prior intersecting shear on nonbasal planes, the former to the temperature dependence of the preliminary slip. THE basic symmetry of hcp crystals has the effect of limiting the number of independent slip systems and making twinning an important deformation mechanism. The general result in wrought polycrystalline aggregates is a more or less sharply developed texture (or preferred orientation) which underlies a strong anisotropy in mechanical behavior. Knowing how the one influences the other is essential background for the use of such materials. Magnesium was of interest in this work because of the unexplained plasticity transition that it undergoes somewhere in the neighborhood of 200°c.''~ At lower temperatures plastic deformation before fracture in polycrystalline material is limited, while at higher temperatures extensive deformation is possible. The transition temperature commonly determines the lower limit of the range in which magnesium is worked. The limited ductility can be traced to a lack of independent crystallographic shears. A minimum of five are required for arbitrary shape change.' Around room temperature, however, slip on all known systems provides only four.' In each case, the slip direction is in the (0001) basal plane so that slip does not allow strain along the c axis. With increasing temperature, more slip occurs on the ( 1011) pyramidal plane and the ( 1010) prism plane but without change in direction.'?' Thus, that development alone cannot explain the transition temperature.

Jan 1, 1968

By George B. Clark

THE " Munroe effect" of shaped explosive charges was discovered by Charles E. Munroe more than 50 years ago (in 1888), but it was not until World War II that it was put to any practical use. Both Allied and Axis armies used the principle effectively in bazooka projectiles, artillery projectiles and in fixed shaped charges. The first two were used primarily to combat tanks and other armor and the latter to assault pillboxes and other fixed concrete emplacements. Many engineers and others who saw the military application of the jet effect of shaped charges believed application would be possible in many industrial fields where blasting is used, such as mining and quarrying. Some work has already been done on the problem of making shaped charges applicable to mining operations. Experimentation conducted at the National Tunnel and Mines' was directed primarily along the lines of use of shaped charges for secondary blasting in connection with long-hole stoping methods. Experimentation initiated earlier and conducted by the author2 at the University of Utah on a more scientific basis was directed at revealing the basic principles of the functioning of shaped charges, as well as the feasibility of using them in mining operations after the principles of their operation had been clearly defined. It was found that: (I) a given design of charge required an optimum standoff to make it most effective, either in penetrating solid rock or steel (see Fig 3); (2) for a given design of charge there exists an optimum ratio of charge diameter to charge height above which the increase in effectiveness of the charge decreases rapidly (see Figs 4 and 5); (3) partial confinement has the effect of making charge performance much more consistent; (4) the higher power and higher velocity explosives tested are much more effective than relatively low-strength explosives; and (5) shaped charges may be adaptable to mining operations in secondary breakage and drilling blasting holes. Fig I is a diagrammatic sketch of the action of a shaped charge for two types of cavities, while Fig 2 shows the approximate manner in which the jets are believed to be formed when an explosive wave encounters the cavity, approaching it from the top. The experimentation already completed has laid the foundation for further research in the study of shaped charges. Standoff effects, effect of the strength of explosives and other features have been fairly well established. Such elements in the design of shaped charges as (I) geometry of cavity liners, (2) relative horizontal dimensions of explosive column, (3) effect of

Jan 1, 1947

By Albert J. Phillips

IT is a privilege and a pleasure to deliver this, the Twenty-sixth Annual Institute of Metals Division Lecture. Eleven years ago C. A. Edwards addressed this audience on the subject "Gases in Metals." In spite of this relatively recent presentation, I propose to, present to you some quantitative considerations of industrial significance on the separation of gases from molten metals because recent observations and measurements, presented in the literature, have made it possible to evaluate mathematically the gases or gas-forming elements and to develop an understanding of the mechanism of gas separation that should permit, in many cases, the control of this baffling phenomenon. DEFINITIONS Before becoming involved in the subject it seems desirable, for the sake of clarity, to state certain definitions and axioms: I. We are dealing only with gases that separate from the molten metal either during cooling or in the transition from liquid to solid. Gases injected by the liquid stream and trapped in the solidified metal, or those forced into the solidifying metal from the mold due to either thermal or cher4ical effects are not considered. Neither are we concerned with the separation of gases within the metal after solidification is complete for the data on this subject are at least complete enough to permit the practicing metallurgist to satisfactorily control the phenomenon. 2. Only where there is a decrease in solubility or a change in equilibrium of either a gaseous element or an element that reacts to form a gaseous compound, can there be a separation of a gaseous phase from the liquid or solidifying metal. 3. The amount of gas separating from the liquid during solidification can be computed directly from the amount of the element contained in the liquid when freezing commences less the amount of the element found in the solid either as a separate solid phase or in solid solution. 4. There can be no separation of gas bubbles unless the told pressure of the gases in the liquid meld exceeds atmospheric pressure plus the hydrostatic pressure of ' the liquid metal head. (In addition, pres- sure resulting from surface tension in- creases the total pressure requirement for initial gas separation. Probably the remarkable differences in appearance caused by different gases in the same host metal are influenced greatly by the rate of diffusion of the gas in the liquid metal balancing the decrease in pressure as the gas bubble size increases and the surface tension effect decreases. Thus hydrogen with its high diffusion rate in liquid copper separates in the form of relatively coarse cavities for a given rate of heat extraction.) 5. Gas separation can take place at less than atmospheric pressure in the voids created by the shrinkage from liquid to solid, but since the voids are not caused by the gas the presence of gas in the voids is of importance only where it

Jan 1, 1947

By F. E. Bash

Constantan is an alloy of copper and nickel that is extensively used, under a number of trade names, as a resistance wire with a low temperature coefficient of resistance, and one of the elements of base-metal thermocouples, iron usually being the other thermoelement, although for low-temperature work copper is also used. Before the war, constantan was imported, in common with many other technical necessities. Since it required considerable time to receive the constantan after it was ordered, fairly large stocks were kept on hand; but after the beginning of the war no more was imported and the stocks of foreign material were exhausted about the same time that the steel and munition manufacturers began to need great quantities of it for thermocouples for the heat treatment of steel. To meet this demand, the International Nickel Co. began manufacturing constantan that met all the requirements of the users of resistance wire but did not give the same electromotive force against iron as the German material and consequently could not be used with instruments calibrated for a definite e.m.f.-temperature relation. It so happened that all the constantan made had an e.m.f. lower than that necessary to meet the specifications of the Leeds & Northrup Co. for whom this investigation was carried out. If some had been higher and some lower, good wire could have been obtained by a process of selection, but as it was no wire at all could be procured. To remedy this situation, a thorough investigation was started with the close cooperation of the International Nickel Co. and the Electrical Alloys Co. The specifications to which the constantan had to conform were that it should give an e.m.f. of 47.40 millivolts against pure iron at 1500" F. (816" C.) with the cold-junction temperature at 0" F., or a proportional e.m.f. at temperatures near 1500" F. The method of checking a wire was as follows: It was first welded to a piece of iron wire; Armco iron was found to be satisfactory but iron with greater than 0.1 per cent. carbon would give a lower e.m.f. against the same piece of constantan than pure iron. The couple was then insulated and the fire end was tied to the

Jan 1, 1921

By Edwin B. Wilson, Joseph W. Leonard, Richard W. Borio

preparation of specification coals for the utility industry is approached from the standpoint of a cooperative effort with the power company to assure that the shipped product will be a noncorrosive coal. Selective mining, coal preparation, the use of additives, and coal blending are mine-site techniques proposed as means for upgrading corrosion-retarding constituents of utility coals (CaO and MgO) while, at the same time, reducing the concentration of those constituents of coal (Na20 and K,O) which cause corrosion. Data obtained from large-scale boiler testing in combination with bench-scale physical and chemical tests are used as a basis for the formulation of mine-site procedures to improve coal combustion utilization. Electric power generation remains the greatest market for coal in the United States. A major reason for this strong market has been the ability of the coal industry to supply a superior product for combustion while maintaining competitive prices. Now that the coal industry is engaged in intensive competition with nuclear power for future energy demand, it becomes ever more imperative that superior coal products are produced. One important problem when burning some coals is a liquid phase corrosive attack on boiler tube metal in the superheater and reheater areas of the furnace where steam temperatures may exceed 1050°F. In addition to causing power outages and high maintenance costs, corrosion is a continuing barrier to the future development of more efficient steam cycles which permit lower generation costs when using coal. Research methods of the past which have been directed at finding solutions which could be applied at the power plant site have been only partially successful and are generally costly. This paper contains a suggested --method of corrosion control through investigation of the problem at the source of the trouble—the coal supplier facility. It is proposed that mine-site pre-ventative procedures be considered as an effective means of cooperative corrosion control between the power company and the coal supplier. Economic justification must be applied to the individual situation. This paper is based on recent work by Combustion Engineering, Inc. and the Coal Research Bureau of West Virginia University under a contract from the Department of the Interior Office of Coal Research.',' Results which are of importance to this discussion may be summarized as follows: 1) The alkali minerals of coal (Na2O and K2O), as measured by an acid leaching process, can be related to corrosion rate in utility boilers. As these constituents increase in a coal product, its corrosiveness can be expected to worsen. 2) The alkaline-earth minerals contained in coal, reported as total CaO and MgO reduce corrosiveness 2s their concentration increases. 3) Naturally occuring, alkaline-earth-bearing materials, such as limestone and dolomite, may be added to a coal to reduce its corrosiveness. 4) Coals with very low iron contents tend to be less corrosive. These results provide the groundwork for examination of the system of operations which occur at the supplier facility from the seam face where mining is begun to the point of loading for shipment. The Mining System Fig. 1 is a cross section of one of the typical coal seams (designated coal A) that was boiler tested during this research program. This seam is overlain by material which consists primarily of a gray-black shale. In the lower third of this seam, there exists a thin rock parting of less than 4 in. in thickness which is consistent throughout the seam. The floor material is fireclay. In order to examine mineral distribution throughout this particular seam, the Coal Research Bureau collected a

Jan 1, 1971

By Henry Rawdon

THE METHOD of demonstrating the structure existing in a metal or alloy at high temperatures, by etching a polished sample after it has been heated to the desired temperature, is quite familiar to metallographists. The usual procedure1,2 is to heat the specimen, previously polished for microscopic examination, to the desired temperature, in a neutral atmosphere (hydrogen or nitrogen), then admit the etching gas. (chlorine, hydrochloric acid or similar gas) for. a few seconds, and finally, after flushing out the etching gas with the neutral one, cool the specimen in the neutral atmosphere. The pattern produced by etching at a definite temperature is usually taken as a record of the microstructure prevailing at that temperature. It has frequently been pointed out that changes in composition of the surface metal occur during the preliminary heating in the neutral atmosphere, so that the appearance produced' by the etching at high temperature may not exactly represent the condition of the interior of the specimen. To overcome this uncertainty, the heating has sometimes been done in vacuo,3 the etching gas being ad-mitted when the desired temperature was reached, then pumped out and the specimen cooled in vacuo.

Jan 2, 1920

By S. W. Miller

Most of the steel welding done at the present time is in material containing not over 0.3 per cent. carbon, and the tests here described were in similar material. These tests are not as yet completed but it is hoped that more results and more reasons for the conclusions may be presented at the meeting in February. From the time the author found the peculiar structure in electric welds referred to in a previous paper,' that is, needles or plates in the grains and similar material, in larger spots, at the grain boundaries, he has felt that these plates which may be iron nitride and probably contain some carbon, were at least partly responsible for the brittleness of electric welds. He has found but few traces of similar lines in oxyacetylene welds until the last 2 mo., he has since found large numbers under certain conditions. In the top of these welds, they are quite numerous. In the body of heavy oxyacetylene welds, they appear at times, but not nearly to the extent that they do in electric welds; the author has never seen them in the body of welds in material less than % in. (19 mm.) thick. They are shown in Fig. 82. The reason they were not noticed before is undoubtedly due to the fact that in making tests of welded pieces the weld was always ground off level with the plate, and as this structure only appears in the top 1/16 in (1-5 mm.) of the weld, they were removed by the grinding or machining; also, welds 3/4 in. thick had not been examined. It did not appear, in making bending tests, that this structure had much influence on the strength of oxyacetylene welds; while electric welds are noticeably brittle. Further, oxyacetylene welds made with certain special materials were exceedingly brittle even after the tops of the welds were removed; this was true in cases where there was no sign of the plates whatever and where the welds were remarkably free from oxide and the other usual defects. It appeared, therefore, that this brittleness did not depend on any variable that had been noticed so far, and it was decided to find where the rupture occurred in various kinds of welds made

Jan 1, 1920

By E. M. Wise

IN a previous communications the improvement in strength, harden-ability and color, occasioned by replacing gold in a typical gold-silver-copper alloy by various amounts of platinum, or palladium, was discussed. In the present paper the results of further studies upon the constitution and the nature of the hardening transformation in these alloys are pre-sented. This research may be summarized as follows: 1. The liquidus and solidus have been determined for the alloys of the palladium and platinum series. Cooling curves were utilized for deter-mining the liquidus of the palladium alloys but this method proved unsuitable for the platinum alloys so that a, novel quenching method was utilized for the latter. Both the liquidus and solidus of the palladium alloys increase steadily with the palladium content. The liquidus of the platinum alloys increases rapidly with the platinum content, while the solidus temperature increases with the platinum content up to about 14 atomic per cent platinum, but suffers no further increase with additional increments of platinum up to 20 atomic per cent at least, owing to a peritectic reaction. 2. Palladium, and even more effectively platinum, reduces the rate of grain growth. Owing to this fact and to the increase in the solidus temperature, "overheating" does little or no damage to alloys containing reasonable quantities of these elements. This is confirmed both by tensile tests and metallographic examination. 3. The excess phase present in one of the high-platinum-content alloys has been isolated and chemically analyzed and was found to consist almost wholly of platinum, gold, and copper, evidently derived from the compound AuCu, by the partial replacement of gold by platinum.

Jan 1, 1933

By Robert H. Richards

Jan 1, 1897

By H. Shafick Hanna, Carl Rampacek

Wastes generated by the mining, mineral processing and metallurgical industries now total about 1.8 billion tons annually. The wastes include gases, dusts, solutions and a variety of massive solid mineral materials such as tailings and slags all of which now must be disposed of with a minimum of environmental degradation and at an acceptable cost. Some of the metal and mineralconstituents have potential economic value and their recovery can augment our primary mineral and metal resource supply base. The resource potential of wastes generated by the iron and steel, aluminum, clay, phosphate, copper, coal mining and processing, nonmetallic, and selected secondary metals industries is identified. Information on current efforts being made to recover these resources and the technology now employed or under consideration are presented.

Jan 1, 1980

ALABAMA Auburn.-Brown, R. L. Battelle.-Green, G. G. Bessemer.-Abbott, C. E. Dobbs, G. G. Ferguson, V. Birmingham.-Aldrich, T. H. Aldrich, T. H., Jr. Allen, A. W. Bonnyman, J. Bowron, J. Crawford, G. G. Crockard, F. H. Ellis, E. E. Fairbairn, C. T. Gambrill, G. T., Jr. Geismer, H. S. Hiller, E. McCormack, G. B. Maben, J. C.

Jan 1, 1917

By I. J. Hegyi, J. J. Tietjen, H. Nelson, J. I. Pankove

The fabrication of p-n junctions in GaAsl-,P, alloys by a vapor-phase gowth technique has for the first tirne resulted in room-temperature injection lasers capable of operating over a broad range of wavelengths extending into the visible region of the spectrum. The shortest wavelength achieved to date is 6750A at room tetnperature. In addition, at 78°K the threshold current density values for these lasers are generally the lo~vest reported, and the emitted radiation extends to the lozc,est wavelength ever attained (6350A). With lasers fabricated from material containing 14 pct Gap, quanticm efficiencies of 26 pct and peak power outputs of 25 zu were obtained at room temperature. ALTHOUGH room-temperature operation of GaAs injection lasers has been well-documented,&apos;-5 the operation of GaAsl-,P, (x > 0) laser diodes has been restricted to relatively low temperatures.8-&apos;0 This has been previously attributed5, 7, 10-12 partially to the difficulty of preparing single-crystalline GaAsl-& alloys having a high degree of chemical homogeneity and purity. Also, with these materials it has been difficult to prepare high-quality, abrupt p-12 junctions by diffusion techniques; and, in turn, this has made it difficult to obtain optimum electrical properties for room-temperature operationL3 in the resulting laser diodes. As a result, GaAsl-,P, laser diodes have not been efficient enough to permit operation at room temperature. For example, using diffused structures, only a few diodes were obtained which could be operated even close to room temperature (255K)." Recently, a vapor-phase growth method of preparing epitaxial deposits of GaAsl - .P, alloys has been described,14 and the high-purity and homogeneity of these materials has been previously demonstrated. Of special significance, with this technique, n- or p -type doping can be initiated or discontinued at any time and at almost any rate during the crystal growth so that the donor and the acceptor concentrations can be easily controlled to obtain desired impurity profiles. This permits high-quality, abrupt p-TZ junctions to be vapor-phase grown entirely during the crystal growth process, so that diffusion or other p-n junction fabrication processes are unnecessary. After growth, the device does not have to be heated to elevated temperatures, which avoids the possible unwanted introduction and motion of both impurities and lattice defects. Using the vapor-phase growth method cited above, over 300 room-temperature injection lasers have been prepared from GaAsl-,P, alloys having compositions in the range of 0 5 x 5 0.41. These lasers have emitted cohe~ent radiation in the spectral range of 8350 to 6350A at 78°K or from 9000 to 6750A at room temperature. The threshold current densities of the best lasers are independent of the alloy composition over the range 0 < x < 0.2 and compare favorably with values for good GaAs lasers.&apos; MATERIAL PREPARATION Multilayer, epitaxial deposits of GaAsl-,P, alloys are prepared by a vapor-growth technique described elsewhere.14 With this technique, the individual layers which comprise the multilayer structure are prepared sequentially in the deposition apparatus without interrupting the crystal growth. The epitaxial layers are deposited on GaAs substrate surfaces oriented normal to the ( 100) direction. The substrate wafers employed in this study were usually doped with tellurium to an electron concentration of approximately 2 x 10" per cu cm. To avoid strains, the first 10 to 15 p of the deposited material is uniformly graded from pure GaAs to the specific GaAsl- ,P, alloy composition of interest. The GaAsl - ,P, alloy growth is then continued to form a layer of constant composition having a thickness in the range of 25 to 75 p. Both the graded region and the layer of constant composition are doped with selenium to an electron concentration of about 2 x 10" per cu cm. The p region of the diode is then incorporated in the crystal by abruptly changing the dopant concentrations in the vapor phase to facilitate doping with zinc. This layer has a hole concentration of approximately 3 X 1019 per cu cm and typically is 50 p thick. DEVICE FABRICATION In general, the GaAs substrate and the region of graded composition are removed. Ohmic contacts are made to the n-type side by tin evaporation and to the p-type side by an electrodeless nickel deposition. This is followed by an electrodeless deposition of gold on both sides. The crystal wafer is then cleaved along (110) planes and sawed into rectangular parallelepipeds. Typical dimensions are 100 by 300 for the junction area and 100 µ for the diode height. The diodes are either soldered to a copper stud or pressure-mounted in a copper clip. RESULTS AND DISCUSSION Approximately 400 laser diodes having compositions in the range of 0.41 have been prepared by the method described above. Each laser was routinely tested at liquid-nitrogen temperature. The lasers were operated with l-psec current pulses at a repetition rate of 60 pulses per sec. The parameters of greatest practical interest are the photon energy or wavelength of the laser output and the threshold current density. Fig. 1 shows the variation of photon energy with alloy composition at 78°K. The composition was determined from the lattice constant of the material obtained by X-ray back-reflection measurements. Although there

Jan 1, 1968

By S. R. Goodman, Hsun Hu

The formation of secondary - recrystallization tex-tlires in cube-textured 18-8 stain less steel (Type 304) Ilas been studied at three temperatures. Prolonged annealing at 100°&apos;C protluces a PredoninanGly (520) [OOZJ-type texture, which is related to the cube te.ture of the primary lnatrix by a rotation of approxivzately 22 deg around the [001] axis in the rolling direction. Annealing at 1200 or 1300°C facers the formation of the (123)[272/-type texture, which is related to the matrix texture by a [111] rotation of app.voxiniately 40 deg. These observations suggest that in the secondary recrystallization of cube-texlut-ed stainless steel an apparent actilation energy for growth is higher for grains related to the tncrtuix Og [111] rotations thun those reloted by [100] rotations. THE formation of secondary-recrystallization textures in cube-textured primary matrices of fcc metals has been studied widely by various investigators. For Fe-40 pct Ni alloys, Pawlek&apos; and wassermann2 reported that the orientations of secondary grains were related to the cube texture by rotations of 30 and 38 deg around [001] in the rolling direction. However, Rathenau and custers3 found that, while in one Fe-48 pct Ni alloy, most of the secondary grains were oriented with respect to the cube-textured matrix by rotations around [001] of 26.5 deg, in another alloy of a different origin, the orientations of secondary grains were related to the cube texture by rotations of approximately 35 deg around a [lll] axis. Similar orientation relationships were also observed between the secondary grains and the cube-textured primary matrices of copper.4"a No attempt was made to differentiate these two types of orientation relationships; reorientation by either a [111] or a [100] rotation was considered to be equally favored. The present investigation consisted of a study of the secondary recrystallization textures in cube-textured stainless steel. It was noted that the secondary grains formed in stainless steel were considerably smaller than those of Fe-Ni alloys or copper. This offered the advantage that the secondary recrystallization texture could be determined by the texture-goniometer technique, and a more detailed study of the textural development during the course of secondary recrystallization could be made. The effect of annealing temperature on the formation of secondary-recrystallization textures was also investigated. MATERLAL AND METHOD It was shown earlier"-" that a strong cube texture can be obtained in 18-8 stainless steels by rolling at 800°C to produce the copper-type deformation texture, followed by annealing at 800" to 1000°C for recrystallization. To improve the cube texture for the present study, a commercial-grade 18-8 stainless steel (Type 304) was rolled at 800°C first to 5 mm (0.2 in.) thick plates. Three of these plates were then stacked and welded together along the edges into a sandwich assembly. After annealing at 900°C for 20 min: the assembly was finally rolled at 800&apos;C to 90 pct reduction in thickness with reheats and end-for-end reversals after each pass. Only the central strip, which was reduced from 5.0 to 0.50 mm (0.7 in. to 0.020 in.) thick, was used. The chemical composition of the steel in weight percent was as follows: C, 0.06; Mn, 0.38: Cr, 18.71; Ni, 9.56: P, 0.011; S, 0.009; and Si, 0.39. The purpose of rolling the strip in a sandwich assembly was to prevent direct contact between the central strip and the rolls. It was observed earlier" that, when the strip was rolled at 800°C without being enclosed in a sandwich assembly, the cube texture obtained by subsequent annealing at 900" or 1000° C for recrystallization was largely confined to the central section of the strip, while most of the recrystallized grains formed in the surface section of the strip were not cube-textured. This was obviously due to the fact that the actual temperature at the strip surface during rolling, as a result of direct contact between the strip and the cold and massive rolls, was considerably lower than 800°C. By using a sandwich assembly for hot rolling, the cube texture obtained upon subsequent annealing for recrystallization was found to extend through the entire thickness of the strip. After rolling, the central strip was taken from the sandwich assembly. and cut into specimens. Prior to annealing. the specimens were etched to 0.25 mm (0.010 in.) thick. A tube furnace provided with a purified, dry argon atmosphere was used for annealing. Textures were determined by the reflection technique. using a Siemens automatic texture-goniometer and ZrOz-filtered MoKa radiation. With a time constant of 4 sec. the preferred orientation of the secondary grains could be measured satisfactorily by the integrated intensities. Both (111) and (200) reflections were measured, and corresponding pole figures were constructed according to the techniques described previously.10 The agreement between results deduced from these two reflections was excellent. RESULTS AND DISCUSSION Secondary-Recrystallization Texture due to Prolonged Annealing at 1000°C. Fig. 1 shows the primary-recrystallization texture of a specimen annealed at 1000°C for 30 min. A substantial improvement in both sharpness and intensity of the cube texture, owing to the present processing method, can be noted readily by comparing Fig. 1 with similar pole figures shown earlier in Refs. 9 and 11. Secondary recrystallization

Jan 1, 1967

By George R. Ensminger, E. Heaton Hemingway

During the past year, the Watertown Arsenal has been interested in the occluded gas and oxide content of certain ordnance steels in order to determine, if possible, whether some of the peculiar failures in their physical properties might not be traced to these causes. For the purpose of best accomplishing a study of this nature, it was decided to heat the various samples of steel in a vacuum for definite periods of time at high temperatures and carefully examine the quantity and composition of the gases evolved. By the use of a fused quartz tube fitted with a water-cooled, ground-glass stopper, it was possible to maintain a vacuum at a temperature of 1000" C. for 10 hr. without perceptible leakage being evidenced as measured by a McLeod gage. The silica tube was connected with an evacuating system so constructed that the volatilized gases could be removed from time to time and a low vacuum of 0.0002 to 0.0010 mm. of mercury continuously maintained. At no time during the period of heating or in the removal of the gases did the evacuated system come in contact with rubber stoppers or any rubber connections, making contamination from such a source, impossible. In other words, the only volatile products that could be: obtained must necessarily have come from the steel itself or from the glass and fused quartz system or from the mercury used as a sealing agent. In the carlier experiments, the steel treated was in the form of turnings, but this practice was discarded because the weight&apos;s of the turnings before and after being heated were widely inconsistent,, even when taken from the same piece of steel. This discrepancy developed largely through variation in the amount of metal volatilized with the gases; this metal could always be seen in the form of a ring where it condensed in the cooler portion of the tube in either the amorphous or crystalline condition. Because of the frequency in occurrence and the variation in the manner of deposition, this material was roughly analyzed and found to consist for the most part of iron. At the same time two samples of steel that had been

Jan 1, 1922

By E. Heaton Hemingway, George R. Ensminger

During the past year, the Watertown Arsenal has been interested in the occluded gas and oxide content of certain ordnance steels in order to determine, if possible, whether some of the peculiar failures in their physical properties might not be traced to these causes. For the purpose of best accomplishing a study of this nature, it was decided to heat the various samples of steel in a vacuum for definite periods of time at high temperatures and carefully examine the quantity and composition of the gases evolved. By the use of a fused quartz tube fitted with a water-cooled, ground-glass stopper, it was possible to maintain a vacuum at a temperature of 1000" C. for 10 hr. without perceptible leakage being evidenced as measured by a McLeod gage. The silica tube was connected with an evacuating system so constructed that the volatilized gases could be removed from time to time and a low vacuum of 0.0002 to 0.0010 mm. of mercury continuously maintained. At no time during the period of heating or in the removal of the gases did the evacuated system come in contact with rubber stoppers or any rubber connections, making contamination from such a source, impossible. In other words, the only volatile products that could be: obtained must necessarily have come from the steel itself or from the glass and fused quartz system or from the mercury used as a sealing agent. In the carlier experiments, the steel treated was in the form of turnings, but this practice was discarded because the weight&apos;s of the turnings before and after being heated were widely inconsistent,, even when taken from the same piece of steel. This discrepancy developed largely through variation in the amount of metal volatilized with the gases; this metal could always be seen in the form of a ring where it condensed in the cooler portion of the tube in either the amorphous or crystalline condition. Because of the frequency in occurrence and the variation in the manner of deposition, this material was roughly analyzed and found to consist for the most part of iron. At the same time two samples of steel that had been

Jan 1, 1922

By H. W. Maynor, C. J. McHargue

DURING the course of an investigation of materials suitable for use as thermocouples at elevated temperatures by one of the authors, several nlolybdenum-rhenium alloys were prepared. Micrographs of an annealed alloy containing 25 pct Re (intended concentration; analysis not obtained) showed a number of twins, Fig. 1, suggesting a face-centered cubic structure. This note reports the structure and recrystallized wire texture of an alloy containing 25 wt pct Re. Alloys were prepared from 99.9 pct Mo (Fansteel Metallurgical Corp.) and rhenium obtained from the University of Tennessee (purity unreported). Powders were combined and briquetted at 56,000 psi and sintering was carried out at 2400°C for 5 hr in vacuum. Ingots so prepared were swaged at 982.2" to 1037.8oC into wires 0.036 in. diameter, a reduction in diameter of 85.6 pct. These wires were vacuum-annealed 1 hr at 2000°C. A North American Philips 114.59 mm powder camera and nickel-filtered copper radiation were used for structure determination. For the texture determination a Laue-type camera was used with zirconium-filtered molybdenum radiation and, because of the high background, aluminum foil was mounted next to the film. Exposures were taken with the wire perpendicular to the X-ray beam and tilted by 10". It was found that the X-ray pattern could be indexed on the basis of a face-centered cubic structure. Because of difficulties associated with obtaining a good X-ray pattern for this material, accurate parameter determinations were not made. An indicated parameter value of 3.70A was obtained. The X-ray data are given in Table I. The annealed wire texture was observed to be a sharp [111] texture. The spread about this fiber axis was k8" at the surface of the 0.036 in. wire. The annealed wire textures of aluminum have been reported as retention of the [Ill] deformation texture for anneals below 500°C and a new [1121 texture for anneals above 600°C.1 In copper wires, with a [Ill] plus [loo] deformation texture, results indicate a retention of this texture for annealing at lower temperatures and new components or the disappearance of components for annealing at higher temperatures.&apos; The presence of the strong [I111 texture in the molybdenum-rhenium alloy after a 2000 °C anneal suggests that the deformation texture was the same. Acknowledgment The wires used in this study were prepared and heat-treated at the Institute for Atomic Research, and Ames Laboratory, Iowa State College, and the authors wish to express their thanks to the Institute for allowing the use of the material and permission to publish the results.

Jan 1, 1954