Search Documents

By A. Lawley S. Schuster

The tensile behavior of copper foils prepared from rolled bulk material has been studied over the thickness range 2 to 53 , and for a range of pain sizes. For foils of comparable grain size, having the cube texture and tested along (100), yield strength increases with decreasing foil thickness t below -26p, with a corresponding decrease in ductility. Deformation occurs in the form of localized slip clusters distributed throughout the gage section. To the extent that the tensile strength (10 to 18 kg mm-) is unaffected by foil thickness, and that the foils possess fair ductility, the stress-strain behavior resembles that of bulk material rather than that of whiskers or evaporated films of comparable dimensions. The dependence of yield strength o on foil thickness t below -26p is of the form: oy = oo + kt-1/2. Possible explanations for the stress increase are considered based on 1) the dependence of active dislocation source length on foil dimensions, 2) the locking of surface sources, or the blocking of mobile sources at the surface due to surface film. It is now well-established that filamentary whiskers of many materials show exceptionally high strength compared with bulk crystals.'-11 As the diameter of the whiskers decreases to -1, the observed fracture strength approaches, and in certain cases exceeds, the calculated shear stress for the nucleation of slip in a perfect crystal.' In general, the stress-strain curve is entirely elastic, with strains at fracture approaching 1 pct. Similarly, thin films12-24 of evaporated or electrodeposi-ted material have been shown to possess tensile strengths three to seven times that of bulk material, with total strains at fracture -1 to 2 pct. In the present study, attention has been directed to the room-temperature tensile behavior of thin foils of copper over the thickness range 2 to 53, prepared from rolled bulk material. Yield stress, ultimate tensile strength, elongation to fracture, and work-hardening behavior are measured as a function of grain size and foil thickness. Structurally such foils are superior to either evaporated or electrodeposited films, and in the recrystallized condition exhibit considerable ductility. Apart from preliminary work by Sumino and Yamamoto25 on the work-hardening behavior of rolled and recrystallized copper foils, no systematic tensile studies have been carried out on material of this form. EXPERIMENTAL PROCEDURE Tensile specimens were prepared from 99.995 pct purity rolled copper foils of thickness 2, 6, 12, 26, and 53, obtained from the Hamilton Watch Co., Lancaster, Pa. Irrespective of specimen shape, it is necessary to use tensile foils with edges free from notches or tears. To this end, any form of cutting operation was excluded, and the tensile foils prepared using a photoengraving process, the details of which are described elsewhere.26 Since tensile data are required under conditions of uni-axial stress, the specimen shape is extremely important. Ideally, the foil should be infinitely long, allowing a gradual taper from the grip area to the gage section; however, from a practical standpoint, long foils are easily damaged during testing. A modified tensile specimen was therefore selected having a parallel gage section 1.25 by 0.20 in. with a tapered shoulder section increasing to 0.5 in. at the grips, and an over-all length between grips of 4 in., Fig. 1. In practically all tests, these foils fractured within the parallel gage section. By approximating the foil contour (Fig. 1) to a hyperbola it is possible to analyze the stress distribution in the tensile foil using two-dimensional elasticity

Jan 1, 1964

By S. C. Sun

[There are significant quantities of anthracite silt deposits in Pennsylvania, known as 'liver silts" (l,2). These contain from 20 to 55 per cent of non-combustible materials, the major portion of these impurities being clay slimes. Both the anthracite coal and impurities are mostly of extremely fine particle size. The utilization of these raw silts in power-plants faces such serious problems as, handling difficulties causing plug-up in equipment, disposal of enormous ash-residue, and corrosion. These problems may be solved by upgrading the raw silt with a cleaning process, which will be capable of removing most of the clay slimes and electrolytes.]

Jan 1, 1964

By F. R. Lee

When the Bureau of Mines was established in July 1910, one of the problems immediately attacked by the new organization was the development of standard, for the design and testing of electrical equipment that could be used without fear of initiating fires and explosions in underground coal mines. Research and investigation by Bureau personnel, supplemented by the published results of similar work by European mining authorities, led to the establishment of standards or "schedules." which guide manufacturers ill the design of many types of electrically operated machines and devices used in underground coal Mining. By issuing these standards, Bureau personnel establish the requirements to be met by such equipment before it tan be approved by the Bureau of Mines as permissible for use in gassy coal mines. Every 2 years the Bureau of Mines publishes a list of equipment that leas been accepted as approved or permissible during the preceding 2 calendar years. This is done to inform the mining industry of the availability y of the latest equip¬ment for safe use underground.

Jan 1, 1964

By Luke L. Y. Chang, Bert Phillips

ThE tendency toward further oxidation of the intermediate oxides and the high volatilization rates of the higher oxides have prevented direct attainment of equilibrium data for the system tungsten-oxygen. As a result, St. Pierre et al.1 have proposed a phase diagram (to 800°C) based on thermody-namic data to 1200°C for the known tungsten oxides (WO2z, W18O49, W20O58, and WO3) and a report on a tungsten suboxide W3O.2 Recent modification of a technique previously described3 5 now permits adequate preservation of compositions of mixtures of metallic tungsten and metal oxides (e.g., of tungsten, cobalt, calcium, samarium, titanium) in order that condensed phase relations may be established to 1700 This method has been applied to study the high-temperature stability of tungsten oxides. In the method used, the desired compositions were sealed in nonreactive containers such that only a small gas volume remained. Each sample then established its own equilibrium atmosphere at temperature. This method has advantages in the study of systems of the W-0 type where knowledge of the condensed phases is desirable but for which composition and pressure of the gas phase are not readily attainable because of oxide volatility. Mixtures of 99.99 pct tungsten metal powder and purified tungsten anhydride (WO3) or in some cases W18O49* were equilibrated in pellet form in sealed

Jan 1, 1964

By P. Hadzeriga

Ion exchange techniques have been growing fast and spectacularly in all phases of Science for the last two decades, but still its acceptance as a unit operation in Metallurgy is resisted. Mainly this is because ion exchange procedures are thought of as glamorous techniques by which only relatively expensive metals are to be recovered. Perhaps this concept comes from the early and basic marriage of uranium and other high price metals and ion exchange procedures. The general trend is that ion exchange technique requires equipment and materials which are too expensive to economically perform a chemical step whenever "cheap" commodities are produced. However, we are here presenting a means of utilization of waste hydrochloric acid by an ion exchange technique. We have studied this from the engineering and economic standpoint in a number of variations of the main procedure discussed here and we-conclude that under proper economic circumstances, the cost of the ion exchange material as well as the equipment and labor involved in the ion exchange section, is by no means unreasonable.

Jan 1, 1964

By P. L. Russell

The use of nuclear explosives for excavation has been demonstrated to be feasible and practical. Application of nuclear explosives for overburden removal from large ore deposits appears to offer economic advantages over present methods, but under the present pricing schedule, high-yield devices must be used to obtain an economic advantage. The use of nuclear explosives presents problems not inherent in the use of conventional explosives, and thus they can be used only in areas where large explosions and associated phenomena can be tolerated. Stripping of coal with nuclear explosives does not appear practical at this time, but stripping overburden from copper or iron ore deposits may be a potential use. Even here, however, the use of nuclear explosives would require isolation, favorable topography, favorable ground-water conditions, and a low population density. If these basic requirements can be met, the use of nuclear explosives for overburden removal would offer both economic and time advantages. The possibility of using nuclear explosives for peaceful purposes was a subject for speculation as early as 1945. The PLOWSHARE Program was formally established by the AEC in June 1957 for the purpose of developing and demonstrating peaceful applications for nuclear explosives. The technical direction of the program is the responsibility of the Lawrence Radiation Laboratory, Livermore, Calif. Mining and excavation were two fields that received early consideration as areas in which nuclear explosives might be used. Knowledge gained from underground weapons testing increased this possibility, and the development of the thermonuclear device which has a small fission-to-fission ratio, reduced the hazard of radiation, and spurred interest. Nuclear explosives appear to have the greatest potential in the following mining operations: 1.— Surface Mining a) Stripping of waste for open-pit excavation b) Breaking of ore in open-pit mining c) Quarrying d) Blasting for production of aggregate, riprap, etc. 2. — Underground Mining a) Block caving application b) Crushing of ore for in-situ leaching, etc. c) Preparation of underground waste disposal areas Of the potential applications, excavation is perhaps the most obvious and the best understood, and probably the most practical for use in the near future. Large quantities of rock and earth can be moved by proper emplacement of nuclear explosives, but economic and practical relationship must be determined between the known capabilities of nuclear explosives and the required excavating to remove overburden. REMOVING OVERBURDEN IN OPEN-PIT MINING Removing the overburden is one of the largest jobs in open-pit mining. In 1960 open-pit mines produced approximately 130 million tons of coal, 108 million tons of copper ore, and 135 million tons of iron ore. To obtain this much production, an estimated 3-billion tons of overburden were removed from the coal, 216 million tons from the copper ore, and 135 million tons from the iron ore. These figures do not include the initial stripping required before ore production. For example, the ASARCO Mission mine started stripping operations in August 1959 and by mid-November 1961 had removed 46.3 million tons of material including 1.2 million tons of ore.* Initial excavation of this type offers the most favorable conditions for utilizing the earth-moving ability of nuclear explosives. EXPLOSIVE CASTING FOR REMOVING OVERBURDEN The use of explosives to remove overburden is not a new idea. Conventional explosives have been used for this purpose for many years with varying degrees of success. Several small coal strip operators have used this idea to increase production. At these mines about one-third or more of the overburden is thrown by explosives across the pit and onto spoil piles. The additional costs of drilling more blast holes and more explosives are more than compensated for by a reduction in the time required to uncover the coal, and by an increase in coal production.

Jan 1, 1964

By Melvin P. Silverman

The literature on methane-oxidizing bacteria is reviewed in regard to (1) the growth and isolation of cultures by special techniques; (2) the distribution of these organisms in nature and descriptions of individual species; (3) the physiology of methane-oxidizing bacteria as influenced by temperature, light, pH, aerobiosis versus anaerobiosis, and carbon and nitrogen sources; and (4) the biochemistry of methane oxidation revealed by studies with intact cells and subcellular systems. Present practical applications of methane-oxidizing bacteria are limited to prospecting for natural gas and petroleum deposits. Desirable areas for future research are discussed as well as some possible applications such as (1) the removal and/or early detection of methane gas in coal mines by intact cells or enzyme preparations; (2) the generation of electrical energy by microbial fuel cells using methane as fuel; (3) the growth of methane-oxidizing bacteria on methane for their food value; (4) the purification of hydrocarbon gas mixtures using methane-oxidizing or other alkane-oxidizing bacteria; and (5) the synthesis of methane from mixtures of H2 and CO or H2 and CO2 by me thane-forming bacteria.

Jan 1, 1964

By John C. Hartley

Three systems that monitor ventilating fans are described. These electronic monitoring systems automatically perform most of the operations required to conform with the provisions of the Federal Mine Safety Code in the event of fan failure or slowdown.

Jan 1, 1964

By L. A. Hanson

Jan 1, 1964

By D. W. Fuerstenau, P. C. Kapur

The kinetics of green pelletization in a laboratory balling drum have been studied, using pulverized limestone as a model system. The growth characteristics of green pellets were found to be extremely sensitive to the moisture content of the material. Empirical kinetic equations, which incorporate a function of specific surface of the pellets as the criterion for growth potential, have been found to describe growth in a nucleation region and in a ball growth region. The rate constants in the kinetic equations are strongly dependent on the moisture content of the material being pelletized. Size distributions of the balls at different stages of pelletiz-ing are also discussed. In many industrial chemical processes, particulate matter can only be utilized if it is in an agglomerated form, such as pellets. Pelletizing is now widely used in iron ore technology1, and it has also been applied to a number of diverse fields such as the production of cement-kiln feed2, fertilizers3, and fluorspar4. Recently, it has been proposed to pelletize dispersion-type ceramic nuclear fuel elements5. In iron ore technology, for example, the production of agglomerates by pelletizing involves two major steps: 1) the preparation of green balls by rolling particles in a suitable balling device and 2) the firing of the green balls to form compact, strong bodies upon sintering. The critical step in a successful iron ore pelletizing operation is generally considered to be the balling operation1. In this paper, which is not concerned with the sintering of green pellets, the words green pelletizing and balling will be used interchangeably. Green pelletizing, or balling, will be defined as the process of forming larger bodies by rolling fine particles on a surface without the application of direct pressure. Two recent literature surveys6" indicate that in spite of the considerable amount of industrial pelletizing, very little is known about the fundamental principles of balling and its kinetics. The first reported research on the kinetics of pelletizing is the work of Newitt and Conway-Jones8. Using silica sands of different sizes in a batch laboratory balling drum, they found that the average green pellet diameter increased linearly with time at constant drum speed, and qualitatively the growth rate increased with moisture content. Generalized conclusions cannot be drawn from their research since the materials which they pelletized were sand and sand-silt mixtures rather than comminuted materials. Moreover, Newitt and Conway-Jones used testing sieves to estimate the size distribution of the green pellets, and this technique limited the range over which they could study the growth kinetics of the pellets. Bhrany and co-workers9 investigated the kinetics of balling iron ore fines on disk pelletizers ranging in diam from 1 to 18 ft. In their investigation, balling was carried out as a continuous operation, and growth kinetics were studied in terms of retention time of the material on the disk. Although the feed material in their study was quite coarse (the maximum size being about 1/2 in.), they also found qualitative relationships between pellet growth and water content, and feed size. In the present investigation, a number of innovations were introduced that refined the experimental measurements and established the reproducibility of balling experimentation. This enabled extension of the range of measurements to include study of agglomerate nucleation phenomena in the fractional mm size. This paper presents a detailed analysis of the nucleation and growth of green pellets in a laboratory balling drum. MATERIALS AND METHOD Pulverized limestone of specific gravity 2.72 was used as a model system in these studies. It has already been established that the balling characteristics of limestone and silica are similar to those of iron ore concentrates 2,8,10, depending on physical, rather than chemical, properties of the particles. The size distribution of the limestone was determined by a wet-dry sieving technique in the sieve range and by a sedimentation balance in the sub-sieve range. Fig. 1 presents the size distribution of the limestone used in this research. This figure shows that the material is finer than 200p (65 mesh) and that 25% of it is finer than 12. The specific surface area of this powder, as measured by BET gas adsorption methods,

Jan 1, 1964

By R. I. Garrod, R. A. Coyle

The shapes and positions of X-ray reflections from specimens of copper, steel, and aluminum alloy haue been examined in the elastic and plastic ranges both while the specimen was under stress and in the unloaded condition. For the aluminum alloy the shape was unaltered by the application of stress either within the elastic limit or in the plastic range provided that no additional plastic strain was induced. In copper the broadening accompanying plastic deformation was very slightly reduced when the specimen was unloaded. A similay but more marked elastic component of broadening was also found for steel, but in this case below the yield stress. Line profiles corrected for instrumental and particle-size broadening indicate very large internal stresses in local regions of the plastically deformed metals. The results are discussed in terms of a recent suggestion that the heterogeneous dislocation distribution between the cells and their boundary walls plays a major role in the peak shifts and broadening of the X-ray reflections. STUDIES of the X-ray line profiles from strained polycrystalline aggregates concentrate usually on one or the other of two main parameters: a) the displacement of the peak of the intensity contour from its position for a strain-free aggregate, or b) the shape of the profile. From peak shifts data can be obtained either on the relation in both the elastic and plastic ranges between applied external stress and average lattice strains in a given (hkl) direction, or, alternatively, on the residual lattice strains which are present after a plastically deformed specimen is unloaded.' On the other hand, the shapes of the broadened profiles from cold-worked metals can be analyzed to separate the broadening produced by small particle size and by heterogeneous lattice strains.' In this paper the terms "size broadening" and "strain broadening'' are used in the general sense adopted by warren.' In the past, apart from two early qualitative observation, it has been customary to examine only the movements of the peaks of the profiles while the specimen is actually under load, since the line broadening induced by plastic strain remains after removal of the external stress. Consideration of the implications of existing data of this type suggests, however, that fruitful additional information on a number of fundamental aspects might be gained by careful examination of whether the X-ray line profile is in fact different in the loaded and unloaded states of the specimen. By taking advantage of the sensitivity and convenience of modern diffractometer techniques it is possible to explore with relative ease the magnitude and importance of any elastic effects which may be superimposed upon the well-known permanent changes in profile. The main aim of the work to be described was thus to investigate this point for typical metals and alloys. For this purpose annealed specimens were extended first elastically and then plastically and the positions and shapes of X-ray reflections were recorded. Initially it was anticipated that prime interest would center on observations within the plastic range; it has been found, however, that small changes in profile sometimes occur both before and after the nominal elastic limit of the material is reached. It is shown that the results obtained have important implications in relation to the structural changes and processes associated with deformation. I) EXPERIMENTAL To enable the diffraction lines to be recorded while the specimen was under uniaxial-tensile stress, a small hydraulic testing machine was designed and constructed for direct attachment to the goniometer of a Philips diffractometer. The specimens, which were machined from 1/2-in.-diam rod and had a central rectangular section 3/8 by 1/16 in. over a gage length of 1 in., were held in the machine by split collets mounted in grooves in the cylindrical ends of each specimen. No special precautions were taken to ensure precise axiality of loading. Constant oil pressure was maintained by a lever and weights system and transmitted to the loading rig by flexible pipe. The actual load on the specimen was measured by a load cell in the machine to an accuracy of * 1 pct. To enable smooth X-ray profiles to be obtained the specimen and machine were oscillated continuously during recording through *7-1/2 deg about the normal half-angle position of the goniometer. The three materials chosen for the investigations were high-purity copper as representative of a ductile fcc metal, a low-carbon steel for a bcc metal, and an aluminum alloy as a material in which the proof stress/ultimate strength ratio is high. Details are as follows. a) Copper. 99.999 pct purity. After machining the specimen surface was polished mechanically and

Jan 1, 1964

By A. W. Fletcher

A nickel-copper sulphide concentrate was treated in a pilot plant at Warren Spring Laboratory during 1961, by a hydrometallurgical roast-leach- solvent extraction process devised to cleanly separate the metal values, and produce acid sulphate liquors containing the metals. It is shown that 86 percent of the nickel and 95 percent of the copper could be leached from the calcine, after a sulphatizing roast on finely ground flotation concentrate. Iron was removed from the leach liquor by limestone neutralization with a small loss of values. Copper and nickel were separated by solvent extraction with naphthenic acid in kerosene after partial neutralization of the iron-free liquors with ammonium hydroxide. Hydrogen sulphide and chlorine were used to remove zinc (and residual copper) and cobalt impurities respectively. The recovery of pure copper and pure nickel, by electrowinning, from the acidic solvent extract strip liquors finally produced, appears technically feasible.

Jan 1, 1964

By Sumner M. Anderson

ATHOUGH scattered signs of increased activity in the mining industry accompanied an incipient improvement in the overall economic situation during the latter months of 1963, production levels for the year as a whole responded to the general 1962-63 business recession with a 4.2 percent decline. The petroleum industry, active since 1907, did not become a dynamic force in the economy until exploration and drilling contracts were concluded with private companies in 1958 and 1959; on November 15, 1963, having virtually achieved self-sufficiency in petroleum in the preceding year, those contracts were unilaterally annulled. In the field of metallics, the only approach to internal sufficiency-aside from the iron and steel industry that has depended heavily on the importing of basic raw materials-has been in mining, smelting, and refining lead and zinc although iron ore, silver, beryllium, tantalite, and tungsten have been mine production items of economic significance. Reserves of lead, zinc, silver, bismuth, vanadium, and low-grade and metallurgically difficult iron ore-as well as those of beryllium, tantalite, and tungsten which are produced primarily for export-appear to be fairly abundant. The exploration of deposits of copper, cobalt, tin, lithium, gold, manganese and uranium has been undertaken on a relatively small scale, and little precise information is available on the extent of reserves. Argentina is dependent on foreign sources for part of its required iron and steel and, except for lead and zinc, most of its nonferrous metals. Nonmetallies and solid fuels present an exceptionally varied array of production items among which cement had the second largest 1963 output in South America. Borates, bentonite, common clay, diatomite, fluorite, granite, lime, limestone, obsidian, onyx, rhodochrosite, salt, and spodumene ordinarily are produced for export either exclusively or in excess of domestic consumption requirements. Barite, cement, chalk, gypsum, marble, and mica are both exported and imported. Argentina depends entirely or partly on imports for coal and coke, certain special types of clay, mineral abrasives, graphite, magnesite, mineral fertilizers, sulfur, talc, and minerals for construction, the last group being chiefly attributable to convenience of river transport from Uruguay.

Jan 1, 1964

By John C. Draper

Little precise information is available on the effect of mining on the surface topography. It is often assumed that after mining the surface will simply sink. This is not an infallible conclusion as is well illustrated in two of the three examples herein. This paper describes the results of an attempt to precisely measure the surface movement in the area around coal pillars left in place for three oil wells in a completely mined and caved area at the Harwick Mine of the Duquesne Light Company. The dates when the various measurements were made are shown on the data sheets and indicate the rate of surface movement. These oil wells are identified as wells Nos. 2, 3, and 6. This mine property is located on the north side of the Allegheny River at Cheswick, Pennsylvania, and extends in a northerly and westerly direction about five miles. The three well pillars are situated on the westerly side of the Bessemer and Lake Erie Railroad some 2,000 feet from Rural Ridge, Pennsylvania (Fig, 1).

Jan 1, 1964

By R. M. Hudson

The removal of nitrogen from a nitrogenized low-carbon sheet steel that contained 0.011 wt pct N was determined during heat treatment in Hz-N, mixtures. TIze process followed a first-order rate law; that is, plots of the logarithm of nitrogen content in steel were linear with the time of treatment at a given temperature. The rate of removal increased with an increase in temperature from 900" to 1300°F. By 1400°F the rate in dry hydrogen had decreased to a value intermediate between the rates at 1200" and at 1300°F; in wet (2.47 vol pct water vapor) hydrogen the rate at 1400°F was less than the rate at 1300°F and nearly the same as the rate at 1200OF. The rate at a given temperature increased as the 3/2 power of hydrogen concentration in the atmosphere. While wet atmosplzeres were generally more effective than the corresponding dry atmosplzeres, the effect of water vapor was much less pronounced than the influence of hydrogen content. NITROGEN is the principal agent in the strain aging of ferrite, the effect of carbon being secondary.' To eliminate the return of the yield point after straining and aging, it is claimed2 that the amount of nitrogen in solution in steel must be reduced to 0.0002 wt pct. Strong nitride-forming elements (titanium, vanadium, zirconium, and aluminum) can act to eliminate strain aging by combining with nitrogen. It is extremely difficult to decrease the nitrogen content in commercial steels to the low level required by conventional coil annealing because of the poor contact between the strip surface and the reactive atmosphere. However, a variety of gas-metal reactions can be effected by use of the open-coil annealing method,3 in which the metal surface is fully exposed to the atmosphere. With this possibility in mind, the Applied Research Laboratory has studied the influence of time, temperature, and atmosphere composition on the removal of nitrogen from low-carbon sheet steel. MATERIALS AND EXPERIMENTAL WORK Samples from a commercial nitrogenized low-carbon steel (0.010 in. thick) in the cold-reduced condition were used. The chemical composition of this steel is given in Table I. The gas mixtures used are listed in Table 11. The moisture content in the "wet" annealing atmospheres was controlled at a +70°F dew point (2.47 vol pct water vapor) by passing the gas mixture through a glass tube packed with a solid mixture of 10 pct anhydrous oxalic acid and 90 pct oxalic acid dihydrate held at 127°F; this technique has been described previously.4 For "dry" atmospheres, the gas mixtures were passed through a cold trap immersed in liquid nitrogen. A hinged-top Hevi-Duty electric furnace was used with a Vycor-glass furnace tube. When the furnace was at the desired temperature, the gas mixture was passed through the furnace at a flow rate between 1.1 and 1.2 cfh; coupons (size 3 by 3/4 in.) of the steel were pulled into the center of the Vycor-glass

Jan 1, 1964

By Kenneth H. Johnston

This report describes an in situ combustion project and three waterflood projects in Allen, Anderson, and Wilson Counties, Kansas, that will be visited during the 1964 annual tour of the Kansas-Oklahoma Waterflood Association. Among the unique features of the projects are the movement of heavy crude oil through the reservoir and into the wellbore with energy furnished by burning s portion of the crude oil therein. Another feature is the simultaneous injection of C02 and water, through separate tubing into input wells during early development, to increase injectivity at moderate pressures, Discussion of individual projects includes information on their early history, source and treatment of injection fluids, oil production-decline curves, and the results of water injection on oil production.

Jan 1, 1964

By Hsun Hu

The microstructural changes during rolling and at various stages of recrystallization in (111)[112] oriented single crystals of Si-Fe have been studied by transmission electron microscopy. At very low deformation, the dislocation structure consists of jogged dislocation lines, edge dislocation dipoles, and numerous dislocation loops, which may be interpreted by the jog-formation mechanism in moving screw dislocations. Up to 70 pct rolling reduction, no sharply defined cells are formed. Subgrain forma- tion takes place somewhat earlier in the annealing process than in a similarly processed (110)[001] crystal. This may be partly responsible for the reported difference in the rate of recrystallization between (111)[112] and (110)[001] crystals. Evidence indicates that the formation of recrystallization nuclei occurs largely by the coalescence of sub -grains. This is consistent with previous observations on other Si-Fe crystals. AVAILABLE data in the literature indicate that the main features of rolling and annealing textures in (111)[112] and (110)[001] crystals are essentially similar. A (111)[112] or (111)[112] crystal can be rolled 70 pct without changing its initial orienta-

Jan 1, 1964

By Hammett PHJ

Oil Exploration Companies are primarily interested in how much oil or gas is present in the rocks in an area in which an exploratory well is drilled. The solution of this problem requires a combined effort on the part of the petroleum geologists, drilling engineers, logging and drilling contractors. To help in'explaining how the drilling and evaluation is earried out the paper has been divided into two sertions, one titled Drilling which is presented by Mr. P.H.J.-Hammett and the seeond titled Evaluation which is presented by Mr. R.M.L. Elliott. A typical Perth Basin Well has been chosen as art example for this presentation. In Figure 1A is shown the type of sandstone and shale sequence encountered in this area.

Jan 1, 1964

By Jack A. Kanz, Samuel R. Shortes, E. C. Wurst

Zinc diffusion into GaAs from the vapor phase through reactively sputtered SiO, films Izas been inrestigated for various zinc pressures at 1000"C. Diffusions were carried out in evacuated quartz ampules with elemental zinc and with various Zn-Ga alloys. Sputtered films have proved effective in lowering surface concentrations and preventing surface deterioration during diffusion. Approxin.ate complenzentary error-function impurity distributions were found when surface concentrations were reduced to approximately 3 -—4 x 10" atoms cm'3 or less with dilute zinc sources or by diffusion through SiO, films. Zinc difhsions in GaAs tlzrough SiO, films produced more planar diffusion fronts than were observed with uncoated zuafers under identical conditions. A) Surface Deterioration During Diffusion. Device technolorn-- in compound semiconductors has been hampered by several difficult problems not normally encountered with silicon and germanium. 111-V and 11-VI compound semiconductors generally have volatile constituents at temperatures used for diffusion. To achieve specific junction depths in reasonable lengths of time, or to obtain particular impurity distributions and doping levels, it is often necessary to use temperatures which cause surface deterioration and erosion of the wafer. The resultant surfaces are generally unsuitable for devices. The type and extent of surface damage depends to varying degrees on the particular environment of diffusion and on the particular impurity in question. The most common type of deterioration results from simple dissociation of the gallium and the arsenic during diffusin.' The deterioration process is significantly enhanced by thermal gradients in the diffusion zone, usually resulting in vapor transport and condensation at the cooler portion of the system. The resulting damage sometimes appears as a general haziness over the surface or an array of pyramidal etch pits characteristic of the particular orientation. Occasionally, erosion of the surface occurs uniformly over the wafer so that surface loss is not readily apparent. Workers in GaAs usually resort to the sealed-ampule type of diffusion system3"5 rather than the more conventional open system used for silicon and germanium. Another type of deterioration results from direct interaction of the impurity with the surface. The form of deterioration may vary from surface alloying, as in the case of zinc, to direct chemical attack and vapor transport of the reaction products, as in the case of sulfur. Surface alloying with zinc occurs at higher temperatures and source vapor pressures.4 The process is largely controlled by the amount of free gallium on the surface of the wafer in equilibrium with the arsenic lost to the system. The group-VI elements, sulfur, selenium, and tellurium, are commonly used donor impurities for gallium arsenide. These elements are characterized by high vapor pressures and high chemical

Jan 1, 1964

By Y. Nakada, U. F. Kocks, B. Chalrners

THE orientation dependence of work hardening has previously been studied over the entire range, i.e., including special orientations of high symmetry, in aluminum1-3 and silver.* The differences between various orientations are substantial, and the trend is the same in all fcc crystals. However, there are quantitative differences in behavior between aluminum and silver at room temperature, particularly in the (100) orientation. While many experiments on gold have been reported,5'9 none included the special orientations. We therefore undertook tension tests on gold crystals of the axial orientations (100),(110), (Ill), (211), and, as a representative of single slip, one whose Schmid factor was 0.5 (hereafter referred to as m = 0.5). Single crystals of dimensions 1/4 by .1/4 by 6 in. were grown from the melt1' at a rate of 4 in. per hr, using gold of 99.99 pct purity obtained from Handy and Harman. A growth rate of 1/8 in. per hr, or a purity of 99.999 pct,ll produced no difference in results. The crystals were annealed at 1000°C in air for 24 hr and furnace-cooled down to room temperature, after which they were electro-polished in a solution of potassium cyanide (40 g), potassium ferrocyanide (10 g), soda (20 g), and enough distilled water to make 1 liter of solution, at a current density of 0.02 amp per sq mm. After 2 or 3 hr, a very smooth surface was obtained by this method. Nine m = 0.5, two (loo), one (110), three (Ill), and one (211; crystals were tested at room temperature in a floor-model Instron machine at a tensile strain rate of 0.5 pct per min. The accuracy of the stress measurement was k10 g per sq mm up to 500 g per sq mm, k2 pct for higher stresses. The strain measurement was accurate to t2 pct. The scatter of stress at a given strain among the crystals of the same orientation was small, *5 pct being the largest. The representative stress-strain curves for various orientations are shown in Fig. 1. Table I summarizes the work-hardening parameters as used by seeger.12 Results of other investigators are also included in this table for comparison. There are no previous data for the corner orientations. Values for m = 0.5 crystals agree fairly well with those of Berner. Tm is defined as the stress at which the stress-strain curve begins to deviate from linearity of Stage 11. However, in practice this is a very difficult value to estimate because each investigator has a different idea of linearity. Therefore, the comparison with the values of other investigators may not be valid. In the present experiment, (100) crystals had the highest 111, followed by (111) crystals. The work-hardening rate in Stage I1 was highest for the (111) crystal followed by the (100) crystals. Our value for 0x1 of m = 0.5 orientation agrees very well with those of other investigators. 1) Single-Slip orientation (m = 0.5). These crystals were oriented so that the primary-slip vector was contained in one side face. The dimension perpendicular to this side should then not change if single slip indeed takes place. Within the accuracy of measurement, this dimension did not change during the deformation. Since the accuracy is k0.2 pct, the amount of secondary slip is less than 0.7 pct of the slip on the primary-slip system at 30 pct tensile strain. This is in conformity with the results obtained by Kocks" for aluminum crystals. The tensile axis moved toward (211) during the deformation. Slip bands, Fig. 2(a), were very fine and closely spaced. Some deformation bands were observed. There were no clear-cut cross-slip traces such as the ones observed on aluminum m = 0.5 crystals. 2) (111) Crystals. The orientation of the tensile axis was stable during the deformation. From this observation, one can deduce that at least three slip systems must have operated, and probably all six because the remaining three all have cross-slip relation to one of the first three.' It was very difficult to observe the slip markings. Consequently, we could not confirm by this method that six systems were operative during the deformation. At high strains (above 50 pct shear strain), this orientation had the highest stress-strain curve. At 80

Jan 1, 1964