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By Kenneth B. Higbie

METALLURGICAL ACTIVITY in 1963 was again dominated by the insatiate demands of research and development conducted in conjunction with the nation's defense and aerospace programs. An increasing effort was noticeable throughout the year, however, to apply to the commercial field many of the processes and techniques that have been developed by government-sponsored research. Particularly effective has been the Industrial Applications Program of the National Aeronautic and Space Agency through which many of the technological advancements made during the course of NASA research and development have been published and released to the public. POWDER TECHNOLOGY Powder metallurgy techniques for fabricating metals, not long ago declared outmoded because of improved casting and shaping methods, have since made an astonishing comeback. Traditionally mechanical pressing of powder shapes has been employed when melting and casting was difficult or impossible, when phase relationships needed to be sidestepped, or when machining costs could be avoided. Hence, it has long been used for producing relatively small special shapes of high-melting metals and alloys. Small iron parts produced with a punch and die have been common for many years, but powder metallurgy techniques are now applicable to a wide range of materials and items. Hard-to-handle materials including refractory metals and their alloys are now rolled, forged, or extruded from billets made by sintering isostatically compacted powders. The major element of the powder metallurgy industry still comprises iron shapes, however, and two-thirds of the annual 100,000 tons of powder metallurgy products are made of iron. The largest single user of powder-forming techniques is the automobile industry which currently consumes 14,000 to 16,000 tons of iron powder per year. A typical 1963 model auto contained more than 100 pressed powder parts (e.g., transmission gears, timing gears, sprockets, ball joint suspensions) totaling 5 to 7 pounds per car. Some of these powders are used in self-lubricating parts of porous copper and copper alloys containing as much as 20 volume-percent lubricating oil. The expanded use of powder techniques, coupled with

Jan 1, 1964

Some low grade South Australian iron ores were classified on the basis of their physical characteristics. Ores from Mount Christie and Billeroo are coarse grained mixed ores; Mount Christie ore could be concentrated by gravity or dry magnetic separation at 10 mesh, but Billeroo ore needed to be crushed minus 36 mesh. Ores from Razorback Ridge and Wilgena Hill are fine grained mixed ores; ore from Wilgena Hill could be concentrated by flotation, but poor results were obtained on Razorback Ridge ore. Malcolm Creek ore is non-magnetic and crystalline, and can be concentrated by flotation, but the deposit is small. Ores from Grants Quarries and Peeralilla Hill are nonmagnetic and earthy and could not be satisfactorily concentrated.INTRODUCTIONThe Geological Survey of South Australia has for several years been undertaking a systematic study of the iron ore resources of the State (excluding the Middleback Ranges) in relation to their geology, reserves, and beneficiation. As part of the latter phase of the investigation samples of the ores have been submitted to The Australian Mineral Development Laboratories (AMDL), and it was the study of these samples which provided the material for this paper.The mineragraphic and metallurgical work was undertaken by several officers of AMDL and the results are contained in unpublished reports submitted to the South Australian Department of Mines. Field data published here was obtained from unpublished reports by G. F. Whitten, Senior Geologist, Iron Exploration, of the Geological Survey of South Australia.

Jan 1, 1964

A field method combining solvent extraction and paper partition chromatography permits a simple and rapid semiquantitative estimation of gold in siliceous, argillaceous and sulphide ores. The method will facilitate the eyaluation of prospect samples in which the gold is too fine for separation by panning.Ethyl alcohol-hydrobromic acid mixtures are suitable for chromatographic development of the gold complex, and give clear reproducible definition of the gold zone. Substitution of commercial "methylated spirits" for the ethyl alcohol gives equally good definition, improving the potential of the method for field use.A batch of six samples in the range of 0·5 to 5·0 dwt/ton can be completed in two hours. The range may be extended by simple modification to higher or lower values.INTRODUCTIONIn a chromatographic method described previously (Lever 1958, Nevill and Lever 1959), gold from a standard volume of ore clamped between -plate glass was extracted by aqua regia on to the paper. After cautious drying the chromatogram was developed by an ethyl acetate-nitric acid-water mixture and gold was identified by spraying with stannous chloride solution. Sensitivity of the method in the low range was poor. The brown line obtained in the 1-3 dw/j ton range, caused by movement of gold in the reduced form, was not considered to be a satisfactory confirmation of the presence of gold. It was felt that the method would be improved by using a more elegant extraction and applying developing conditions which would produce a well defined purple line at all gold values. Iron was a limiting factor, and a method of eliminating its interference was needed.The method now developed overcomes these shortcomings, and gives a reliable result with a purple line for assay values of 0·5 dwtjton and over. Gold is dissolved from an...

Jan 1, 1964

By R. W. Stahl

Burning coal-mine refuse banks were surveyed in 15 States. The following characteristics were tabulated for 495 hanks: County; name, population, and distance of nearest town; size and status of bank; status and stage of fire; and topography. Ways of controlling fires were reviewed, the compacting and sealing method proving most satisfactory. Means for preventing refuse-bank fires by proper construction of banks are described.

Jan 1, 1964

From March to May of 1963, the Bureau of Mineral Resources carried out an experimental aeromagnetic survey at Cobar, New South Wales, to field test a proton-precession magnetometer installation in the Cessna aircraft VH-GEO. The Cobar area was chosen as considerable information was already held on the Earth's magnetic field there, which was known to provide a range of anomalous areas that are not excessively disturbed.A procedure for survey flying and methods for processing data were developed during the survey. Contour maps of the aeromagnetic results were produced in the field. The experimental survey was successful in outlining magnetic anomalies in detail.INTRODUCTIONSince 1951 the Bureau of Mineral Resources, Geology and Geophysics (B.M.R.) has carried out an airborne magnetometer exploration programme with DC.3 aircraft carrying fluxgate magnetometer equipment. Recently a proton-precession magnetometer was developed by the Design and Development Group of the B.M.R. for observatory use. One unit modified for airborne use was installed in the Cessna light aircraft, VH-GEO. The Cessna was modified structurally to take the magnetometer, associated bird, and winch gear.The proton-precession magnetometer has many good features.1. It utilises the transistor and associated solid-state devices in its electronics, and hence is light and small.This is the basic feature allowing its installation in a light aircraft. The transistor circuits have a high reliability factor and owing to the card sub-unit...

Jan 1, 1964

Laboratory scale equipment was developed to recover zinc as oxide fume from granulated lead blast furnace slag. The cyclone furnace process is characterised by high treatment rates combined with continuous and independent operation.Results were sufficiently encouraging to warrant pilot plant scale trials being undertaken.INTRODUCTIONSince granulation of lead blast furnace slag started at Port Pirie in 1921 the stockpile of this material has increased to nearly 5 million tons which averages 17·5 per cent zinc by weight. Although a number of processes for recovering the zinc have been examined, economic considerations indicate that a slag fuming process is likely to be most suitable.In the conventional slag fuming process zinc is extracted by injecting pulverized coal and air into a molten slag bath. By maintaining a suitable air to coal ratio the oxidised zinc contained in the slag is reduced to metal. Volatilization of the zinc is followed by reoxidation in the gaseous phase with the addition of further air above the bath. The zinc oxide fume so produced is collected by normal gas cleaning methods.By examination of the thermodynamics of this process Bell, Turner, and Peters (1955) determined the zinc oxide activity of the slag over the duration of the fuming cycle.A combination of high temperature and high carbon monoxide/carbon dioxide ratio was found necessary for rapid zinc elimination.Since melting of the slag is an essential step in the slag fuming process, only two treatment methods appeared possible at Port Pirie until recently...

Jan 1, 1964

By T. Price, H. A. Holl, A. P. Greenough, A

UdIN, Shaler, and ulff' first used wires for the determination of the surface energy of a solid metal. A gage length was marked by tying knots in the wires, which were then suspended in a cylinder of the same metal, heated in an inert atmosphere for the appropriate time, cooled to room temperature, and finally removed from the furnace so that the lengths of the wires could be measured. With iron wires, difficulties associated with deformation during the phase changeszp3 made it necessary to measure the gage lengths at the tem-

Jan 1, 1964

By Sumner M. Anderson

THE ENORMOUS contrast between the mineral economy of Cuba in 1963 and in 1958 was the result of the overall Political changed to which the total economy of the country was intimately lined. Creation of the Cuban Mining Institute (Instituto Cubano de la Minería) to direct all mining activities in the country was an early act of the new Government after the revolution on January 1, 1959. During the next 2 years, the Government confiscated foreign holdings,2 including Unite States investments exceeding $1 billion in value. Foreign mining and metallurgical technicians-predominately from Communist areas-were brought in to reorganize the mineral industries. On January 3, 1961, diplomatic relations between Cuba and the United States were severe and then on May 2, Cuba announced its full-fledged membership in the so-called Communist Bloc. Fifty-four international treaties assured Cuba of Communist economic support, technical and financial assistance, machinery, raw materials, and manufactures. The Soviet Union agreed to buy some Cuban mineral products, and Czechoslovakia stated that it would buy all mineral production offered for the next 20 years, but in both cases at prices said to be much lower than the world market. The mineral productivity segment of the mineral economy during and since the period of political metamorphosis, has withstood the political disruption better than has the economy as a whole, but with no direct measure of the magnitude of its cost. The overall economic record is marked with steady deterioration; the annual average per capita income has dropped from $374 in 1957 to $185 in 1963, when Cuba's deficit with the Soviet Union alone reached an admitted $1 billion.

Jan 1, 1964

THE problem of reaction rates in the open-hearth process is essentially that of trying to form a fairly clear picture of the "chemical mechanisms" in the bath. Quantitative data on reaction rates would perhaps not be of much practical importance even if they were available; however, what few approximate data there are can be used in combination with data given in Chapters 16 and 17 to sketch a picture of the "chemical mechanics" of the open-hearth process that is consistent with essentially all the present available evidence. The result may later be found incorrect in many details but even so it will illustrate certain useful methods for obtaining a clearer understanding of the process. Consistent with the treatment in Chapter 15, but in simpler terms, we may say that chemical reactions in general involve the following elements or steps : 1. The reacting molecules are mixed together in space in such fashion as to favor collisions among them. 2. Units of what is usually an intermediate molecular arrangement called an activated complex are formed at a certain rate, depending on temperature and concentrations. 3. .These activated complex units decompose into the reaction products (this step usually assumed to be so rapid as never to limit the over-all process). 4. In any of these steps, heat energy may have to flow into, or away from, the reaction zone to permit the reaction to proceed. 5. The products of reaction will usually have to move out of the way to permit further reaction. The temperature factor enters mainly through step 2, and its effect is very marked. (What is called temperature is really the mean energy content of all the molecules of the substance involved; at any one temperature a certain proportion of the molecules will have much higher energy content than the mean value.) Various reaction rates measured at around room tem-

Jan 1, 1964

By J. L. Ratliff, R. I. Jaffee, H. R. Ogden, D. J. Maykuth

An experimental program was carried out to improve the low-temperature ductjlity of tungsten through the combined use of dispersed oxides for grain-size control and Groups VII and VIII metal additions for matrix softening. Separate binary -alloy studies showed that increasing amounts of finely dispersed thoria or zirconia and critical amounts of rhenium, osmium, and iridium were effective in significantly reducing the ductile-to -brittle bend transition temperature of tungsten as well as in increasing its re crystallization temper - LIKE most of the high-melting point bcc metals, tungsten undergoes a marked transition from ductile to brittle behavior with decreasing temperatures. The material factors which influence the transition temperature include grain size, metal purity, and the presence of dispersed phases. ature and decreasing its recrystallized grain size. The beneficial effects shown by each of these additions on transition temperature and grain size in binary combinations appeared to be additive in tevnary combinations. Thus, combined additions of 2 to 8 vol pct thoria with 5 pct Re, 0.87 pct Os, or 0.30 pct Ir were effective in lowering the transition temperature of tungsten pom 2000 to 75"C, increasing its re crystallization temperature from 1600 to 1800°C, and decreasing its recrystallized gain size from 1175 to 6800 grains per sq mm. The mechanism by which these factors are operable in tungsten is not yet clearly understood. Nevertheless, it has become increasingly apparent that the interrelationship of grain size and matrix composition governs to a large extent the degree of low-temperature ductility which can be achieved. Though it is not possible to accurately assess the relative importance of these variables, the available evidence suggests that, at low temperatures, grain-size effects predominate over purity effects. This was indicated in recent studies by Allen, Maykuth, and Jaffee,' involving single crystals containing 20 to 40 ppm 0 and 1 to 30 ppm C. Thus, while each

Jan 1, 1964

THE primary interest in the subject of this chapter lies in the fact that various heats of steel made to the same chemical specification do not always have the same properties. The properties considered here, of course, are those inherent in the ingot immediately after solidification and not qualities imparted by variations in subsequent mechanical or thermal treatment. The expression "made to the same chemical specification" is used because some of the variations in properties are due to variations in chemical analysis within the specified ranges of those elements commonly specified and determined. Other variations in properties are due to variations in those constituents of steel (elements or compounds) that are not ordinarily included among the elements specified, thus not a part of the specified "composition." The term "constitution" is used to include not only the specified composition but also the nature and distribution of every element or compound contained in the steel entering the ingot mold ; also included are items such as aluminum oxides and nitrides, presence of soluble gases, and dispersion of nonmetallic particles. When it is considered that the constitution of steel is determined by the addition or absorption into the bath of all such constituents from whatever source, it follows that constitution is of necessity the final result of steelmaking practice. It is the agency through which steelmaking practice operates to control the properties of the steel. The term steelmaking practice is here used in the broad sense, meaning the control of all the materials entering the steel and of the conditions under which the process is carried out. Steelmaking practice, thus defined, establishes the chemical system within which the reactions between components must proceed in obedience to the laws of chemistry. Thus the chemical constitution of the steel is established and, through constitution, the properties of the metal are established. In the preceding chapters it has been shown how the constitu-

Jan 1, 1964

By S. Leber, R. F. Hehemann

This investigation describes the kinetics of alloying in a (Cb-15 wt pct W. 5 wt pct Mo, 1 wt pct Zr) powder-metallurgy alloy. The degree of homogeneity obtained in hydrostatic ally pressed and vacuum-sintered samples is described by composition distributions resulting from analysis of X-ray dvfraction line profiles. Sintering variables and degvee of powder dispersion were evaluated. The utility of single-value parameters obtained from composition distributions is disaissed. The spatial distribution of composition, as revealed by anodically tinted metallographic sarrzples, was used to provide diffision models based on a concentric-sphere geometry. Diffusion equations developed from these models were found to be in general agreement with experimental results. The powder-metallurgy method for the production of refractory metal alloys has the ability to produce an inherently fine-grained, fabricable structure. The more general use of this method is inhibited, in part, by the presumed difficulty in obtaining homogeneity on a microscale. The degree of homogeneity therefore is an important, but usually neglected, variable in specifying the quality of a powder-metallurgy alloy. Convenient techniques for measuring the degree of homogeneity are now available,' and have been used to develop a model describing the process of alloying in a simple binary mixture.' In this investigation, the process of alloy formation has been studied in a more complex system. PROCEDURE The columbium-based F-48 mixture was prepared from the constituent powders shown in Table I. The particle sizes tabulated were provided by the vendors of the individual powders. Standard laboratory techniques utilizing a jar mill were employed for blending. The blended powders were hydro-pressed into 1-in. diam rods which were then sliced into thin discs for vacuum sintering. All samples were given a preliminary treatment at 1700°C for 2 hr. Varying degrees of homogeneity were obtained using additional treatments at higher temperatures. The degree of homogeneity obtained by a specific sintering treatment was evaluated metallographi-cally using the anodic-tinting technique described by olff,' and quantitatively by the analysis of X-ray diffraction line profiles using the X-ray diffraction technique developed by udman.' The diffraction technique is strictly valid only for binary systems. However, the relatively small difference between the lattice parameters of tungsten and molvbdenum when compared with columbium permitted the treatment of the complex composition of F-48 as a (W, Mo)-Cb pseudobinary. Calculations were weighted in accord with the W-Mo ratio in the F-48 composition. The contribution of the 1 pct Zr was ignored since it could not even be detected in the blended powder. Two factors are required to convert an X-ray line profile into a composition distribution. The variation of these factors with composition is shown in Fig. 1. Curve A was used to convert angular posi-

Jan 1, 1964

By Frank L. Wideman

THE TREND towards larger quantities of waste in materials handled at metal and nonmetal mines (excluding fuels) continued. A gain of 10 percent from 1962 in the tonnage of waste removed in mineral operations reflects the kind of technological problems being encountered. Technology has a major role in the mineral industry in the task of supplying raw materials obtained from resources occurring beneath the surface of the earth and used in manufacturing commodities essential to modern living. Changes in technology are often brought about by such factors as variations in economic conditions, differences in physical properties of raw material and changes in mineralogical compositions of ore. Mining is usually begun on the richest and most accessible of known deposits, and when these are exhausted, is continued with leaner ores or with less accessible deposits that are either lying at greater depths or are more remote from markets. The increasing difficulties of extraction and depletion of reserves are offset by improvements in extraction technology, improved transportation, and exploration for new deposits. Although depletion has prevailed at many individual mines and in many districts, technology has been the means of providing for increasing demands of an expanding economy with adequate supplies of minerals despite either the changing character or decreasing grade of certain ores. This has been accomplished by various methods applicable to minerals. Among the implements of technology are utilization of lower grade or more complex refractory ores by mass mining, concentration, processing, recovery of byproducts, and mechanization. Better methods to find concealed deposits or to penetrate to greater depths also have been helpful in maintaining a supply of particular minerals.

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 a 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 Charles Will Wright

The present struggle for economic and industrial supremacy by the Communist world is against the United States, its main target, and the other Free World nations. The basis of industrial power is minerals, so the Communist nations are building up mineral production within their borders, often regardless of costs, and are acquiring quantities of mineral products from Free World countries for future use. They are contracting for additional supplies and advancing funds for the development of these quantities. A number of the less developed mineral producing countries of the Free World are being infiltrated by Communists and Communistic influence. This situation is well known, but as yet little has been done to oppose these activities or to awaken the public to their seriousness. The Communist countries are still far behind the Free World Nations in production of many essential minerals. But, shortages are being made up from Free World nations in exchange for petroleum, manganese ore, chromite and other products. Restrictions on shipments of strategic materials to Communist countries have not been maintained.

Jan 1, 1964

Delhi Australian Petroleum Ltd., acting as operator for the joint interests of Delhi and Santos Ltd., has been engaged in petroleum exploration in the western Great Artesian Basin since 1958.Extensive airborne magnetometer, gravity meter, reflection and refraction seisomograph, and surface geological surveys have been carried out. Results of the surveys have considerably altered the concepts of the geology of the area.Seven exploratory wells have been drilled in the area. Results of the drilling have established the presence in the subsurface of previously unknown Paleozoic sediments which are capable of generating hydrocarbons.Production of oil or gas has not been achieved, but each phase of the exploration programme has resulted in progressively establishing the basic conditions necessary for the discovery of commercially profitable accumulations.INTRODUCTIONDelhi Australian Petroleum Ltd. commenced operations in Australia in 1958. They have subsequently been engaged in systematic exploration for oil and gas, acting as operator for their partner, Santos Limited. The methods and techniques employed are those used throughout the petroleum industry. The results of the exploration programme contribute to a better understanding of the basic geology, and concomitantly a firmer analysis of the petroleum producing potential, of the western Great Artesian Basin.Each phase has progressively enhanced the gross geological interpretation of the area with regard to favourable conditions for the generation and accumulation of hydrocarbons, but the stage has not been reached where productive potential is definitely established.Exploration status in 1958Basin configurationIn 1958 knowledge of the pre-Jurassic stratigraphy of the geographically defined western Great Artesian Basin...

Jan 1, 1964

By D. F. Kaufman, E. D. Levine, L. R. Aronin

The deformation of' impure beryllium crystals by basal glide at room temperature invariably tevminates by basal cleavage after a few percent strain. It is generally accepted that .fracture of this type is caused by the splitting of low) -angle boundaries, or bend planes, by obstacles that restrict the motion of the bed planes in the deforming crystal. The details of such a process have been developed by Stroh, who showed that the high tensile stress norrnal to the basal plane in the region where the bend plane is split results in the propagation of a basal cleavage crack, provided there is no available dejorvrlatzon mode having a shear component normal to the basal plane It has been postulated that puvification of beryllium might lead to increased basal ductility by the vemoval of barviers to bend plane motion and possibly by the activation of nonbasal defor~rlation systems. Large increases in the amount of basal glide that can he sustained prior to fracture have been observed in crystals purified by zone refining. In each case, eventudal fracture was by sharp basal cleavage, suggesting that the split bend plane model still applies to tile fracture of beryllium of rensonably high purity. In the present work, calculations are made to show to what extent basal duetilits can be increased by purification while the split bend plane .fracture process remains applicable. Experimentally observed ductilities are generally somewhat lower than those predicted by calculation because of premature failure due to defects introd~cced during specimen preparation and testing. SEVERAL investigators1-4 have studied the deformation characteristics of beryllium single crystals of commercial purity, and have related the strong anisotropy of plastic deformation in single crystals to the problem of brittleness in polycrystalline beryllium. For most orientations, the principal deformation mode is basal slip, which, at temperatures between 300" and 900°K, begins at a critical resolved shear stress of approximately 1500 g per sq mm and terminates after 3 to 6 pet glide strain by cleavage on the basal plane in the neighborhood of (1120) bend planes that are formed during the deformation. This type of fracture, which is also observed in zinc at low temperatures, has been interpreted by stroh5 to be caused by the splitting of bend planes by obstacles to their motion. In the Stroh model, a (11.20) dislocation wall, or bend plane, moving along the slip direction under the action of the applied stress, encounters obstacles which cause part of the bend plane to be held up, the other part continuing to move. Stress concentrations are built up in the region where the bend plane is split, with a high tensile component normal to the basal plane, resulting in a microcrack at the end of the split wall. Because no deformation mode having a shear component at an angle to the basal plane is available to relieve the stress at the crack tip, the crack can propagate under a sufficiently high applied stress. The Stroh criterion for crack propagation is given by

Jan 1, 1964

By R. W. Stahl

Burning coal-mine refuse banks were surveyed in 15 States. The following characteristics were tabulated for 495 hanks: County; name, population, and distance of nearest town; size and status of bank; status and stage of fire; and topography. Ways of controlling fires were reviewed, the compacting and sealing method proving most satisfactory. Means for preventing refuse-bank fires by proper construction of banks are described.

Jan 1, 1964

Unrelieved residual strains can influence the states of stress in rock masses. If cheap, stable structures are to be constructed in Tock in which large pressures are exterted by unrelieved residual strains, the pressures must be either utilized or neutralized. A photoelastic technique has been used to show that the release of residual strains in rocks is influenced by the mechanical properties of anisotropic rock fabrics. The relationships between directions of residual strain release and the attitudes of minor geological structures have been determined. For engineering design purposes it is possible to estimate the principal stress directions in rock containing unrelieved residual strains if the attitudes of such minor geological structures as foliation planes, lineations, and joints are known.INTRODUCTIONQuarry workers have long been aware that near-surface rocks may be highly stressed. In many cases the stresses are too large to be the result of gravitational loads. Dale (1923, pp. 34-35) gives many instances of deformation produced by the violent release of residual strains in quarry rocks. Coates (1963) has described powerful rock bursts and cases of rock deformation underground implying the existence of much larger stresses than are likely to result from present-day gravitational loads. The only explanation is that pressures of up to several thousands of pounds per square inch may be caused by unrelieved residual strains in rock.Instruments have been developed for measuring states of stress in rock masses. Most stress determinations in rock have been made on the assumption that rock behaves as a simple elastic material. It is now known that rock is a...

Jan 1, 1964

By Erle C. Donaldson

A study of subsurface waste disposal in the United States shows that in eight States a wide variety of industrial wastes are being injected into formations ranging in age from Precambrian to Recent. More than 30 wells ranging in depth from 300 to 12,000 feet are used for waste disposal into subsurface formations which include unconsolidated sand, sandstone, vugular limestone, and fractured gneiss.

Jan 1, 1964