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By L. F. Pease, J. H. Brophy

A phase diagram for the Ta-Zr system is presented. The system is of the minimum-melting point type with the 0-zirconium phase decomposing monotectoidally at 785°C and 95.5 at. pct Zr. The minimum solidus temperature is 1875°C and the temperature of the top of the monotectoid loop is 1775°C. Techniques employed included X-ray diffraction and fluorescmce, electron microprobe analyses, diffusion couples, metallography, and melting-point measurements. Errors due to interstitial solutes and in melting observations are particularly common in this system, and their occurrence is discussed. SEVERAL versions of the Ta-Zr phase diagram have been reported in the literature.lm7 Williams et al.' report a diagram of the minimum-melting point type with a monotectoid reaction at 800°C and 12 wt pct Ta. The minimum in the solidus occurs at 1820°C and 25 wt pct Ta, while the top of the monotectoid gap is located at 1780°C and 80 wt pct Ta. The experimental techniques employed were metallography, electrical resistance variation with temperature, dilatometry, X-ray diffraction, and direct observation of melting by the technique of Pirani and ~lterthum.' Experience in the Nb-Zr phase diagram has shown that small changes in the interstitial content can cause large shifts in the positions of the phase boundaries. Small amounts of inter -stitials can cause similar changes in the Ta-Zr system and may be responsible for the wide variations in the phase diagrams previously reported.'-' The authors15 have found that alloys containing 0.75 wt pct 0 and 1.0 wt pct Ni with tantalum contents from 19 to 85 at. pct often contain a lamellar or cellular precipitate after annealing above 1400°C. This precipitate is very similar to that reported by pollack,12 Ralls," and Donlevy17 for the Ni-Zr system. In the present investigation, a wider variety of experimental techniques and improved alloy purity were applied to the resolution of errors in diagrams for this system as they now appear in the literature. New results have been obtained in the areas of alloy homogeneity and purity. Errors in the common techniques of direct melting observation in binary alloys have been demonstrated. In the commercially important high-tantalum region, the more accurate metallographic method of solidus determination has been employed. EXPERIMENTAL PROCEDURE Nominal analyses of the materials employed are given in Table I. The zirconium was low hafnium reactor grade iodide crystal bar, and the tantalum was in the form of high-purity sheet. Powders were impossible to use because of gas content. Alloys were melted on a water-cooled copper hearth, with a thoriated tungsten-tipped nonconsumable electrode in 2/3 atm of Zr "gettered" argon. Alloys were

Jan 1, 1963

By R. W. Stahl

An award is a form of recognition given for superior performance in a special field of endeavor. Each year awards are given by the Joseph A. Holmes Safety Association and the National Safety Council to mineral industries' mines, quarries, and plants that have worked a specific number of man-hours without a lost-time injury. These awards have a dual significance in that they prove that efficiency can be attained without injury to persons. Safety awards do not result from luck or good fortune but do result from sincere desire coupled with sufficient effort and cooperation to achieve a desired goal.

Jan 1, 1963

By Walter A. Backofen, Donald H. Avery

Intense primary and cross-slip traces were observed in easy glide on Cu: 6 pct-A1 single crystals deformed in tension. A mechanism of cooperative source operation is developed which recognizes that both the applied stress and that resolved from dislocation arrays contribute to the stress on a source. By considering the stress from arrays, the activation of secondary systems in easy glide and the difference in appearance of slip markings on pure and solid-solution crystals are explained. Furthermore the cross-slip system is predicted to be second favored during easy glide for a large range of orientations. FROM many studies of easy glide in fcc metal crystals, a pattern of observations has developed which still requires full explanation. In pure copper, aluminum, and silver, the easy-glide, slip traces are fine and uniform with steps 50 to 100A on the primary* system.1-4 Yet it has not been at all clear why slip in the pure materials should occur in this way. On the contrary, one might expect, with simple slip and a low hardening rate, that the weakest sources on the primary system would operate extensively to produce strong slip traces. In a brass, however, intense slip steps up to 0.5 are found on both primary and cross-slip system4,6-9 seeger10 has pointed out that in a material of low stacking-fault energy such as a brass, extensive easy-glide cross-slip could not be thermally activated, but rather must originate on the cross-slip plane. In further explanation, the wilsdorfs4 and seeger10 noted that only the cross-slip system would not harden differently than the primary, whatever the latent hardening tendencies of other systems; therefore, in brass, which exhibits high latent hardening, the cross-slip is the only secondary system which could be expected to operate extensively, once it became active. The explanation of how the cross-slip system, on which the applied stress is low, becomes activated has been related, in a nonspecific way, to pileups by Hirsch11 and Honeycombe.l2 In the work to be described, deformation traces on solid-solution Cu: 6 pct A1 single crvstals were studied with conventional light microscopy and a mechanism proposed to explain both the observed activation of secondary systems in easy glide and the difference in appearance of slip markings on pure and solid-solution crystals. EXPERIMENTAL In preparing the Cu-A1 single crystals, rectangular bars approximately 0.4 in. by 0.4 in. by 6 in. were first machined from ingots made by vacuum melting copper of 99.999 pct and aluminum of 99.99 pct purity. They were then packed in powdered graphite and the crystals grown in a modified Bridgman apparatus at a rate of 5 mm per hr under an atmosphere of purified nitrogen. Crystal perfection as indicated by Laue back-reflection spots was good except for the last inch to freeze, which was discarded. Orientations so determined are shown in Fig. 1. Tensile specimens with a reduced gage section were obtained by masking the ends with electrical tape and chemically polishing in a solution of 20 pct HNO3, 24 pct HAc, 52 pct H3PO4, 2 pct Hcl, and 2 pct H20 at room temperature.13 Finally, the specimens were electropolished in a 30 pct ortho-phosphoric acid bath at 12 v. Tensile deformation was performed in an Instron testing machine at a strain rate of approximately 1 pct per min. During easy glide, extensive cross-slip was observed with all crystals, in spite of the low Schmid factor on this system, and in no case was any other secondary trace encountered. A certain sequence of slip-line development was associated with the extension. At yielding, intense primary traces passing completely through the crystal developed at some point on the gage section, generally near the grips; weak cross-slip traces also appeared, extending from the primary traces into the adjacent undeformed crystal, Fig. 2. Further extension led to primary traces adjacent to the first-formed and connecting with those of the cross-

Jan 1, 1963

By Howard M. Stainer

Published X-ray mass absorption coefficients were compiled and tabulated. These coefficients are required for various X-ray analytical techniques. Values obtained from 28 authors are listed for 87 elements with both experimental and calculated points included; the wavelengths range from 4.01 to 68 A. Representative graphs are presented for six elements (lithium, nitrogen, iron, silver, holmium, and uranium. A 37-item supplementary bibliography is also included.

Jan 1, 1963

By James H. Gary

Data regarding the composition and physical properties of Florida land-pebble phosphate-waste slime are presented, and the feasibility of dewatering and beneficiating the slime by several different methods is discussed. Chemical analyses, electron micrographs, and X-ray diffraction data showed that principal constituents of the slime included quartz, attapulgite, and flaorapatite. Viscosity of the slime changed with pH; thixotropic, Newtonian, and rheopectic states were observed as the pH increased. Use of various flocculating agents was not effective in improving thickening properties of the slime. Dewatering tests using pressure filtration showed that temperature influenced the filtration rate more than pressure; the filtration rate at 165° C was tenfold that at room temperature. Selective flotation of the slime, using two different processes, gave promising results. About 25 pct of the phosphate was recovered in a concentrate assaying 31 pct P205, Other tests demonstrated that the slime could be successfully fractionated at 20-microns using a hydrocyclone. In hydrometallurgical tests about 80 pct of the phosphorus and alumina were chemically extracted from the slime using sulfuric acid. Limited bacteriological studies made of the slime showed that several types of microorganisms were present and grew in the material despite the presence of fluorine-bearing minerals.

Jan 1, 1963

By John C. Machisak

THIS INFORMATION CIRCULAR contains injury and employment data for all stone quarries in the United States for the Calendar year 1960. This publication contains statistical data on injuries and employment pertinent to the stone quarries and related operations, such as the manufacture of cement and lime, rock dressing etc., but excludes statistics for clay and sand and gravel operations. Data for these commodities may be found in other Bureau publications. Reports received from the operators are voluntary responses to the Bureau's request for information; therefore, the figures may not be complete for the industry. However, since these data contribute greatly to the promotion of safety, every effort has been made to make them representative of the industry.

Jan 1, 1963

By Alfred Wild

The Kraftile Co. plant, Fremont, Alameda County, Calif.--the largest producer of glazed, structural wall units west of the Rocky Mountains-- maintains modern processing facilities to evaluate and blend a wide variety of clays from several sources to produce quality products. The report desribes the prospecting, exploration, and test methods used to locate raw material sources and covers processing methods, cost factors, and trends. Also, the geologic and ceramic factors are considered in a general discussion of the economics, potentials, and requirements of clays as raw materials for ceramic tile manufacturing.

Jan 1, 1963

By Paul M. Price

The Mouat mine, Nye, Mont., was reopened in 1953 by the American Chrome Co. under a Defense Minerals Production Administration contract. Operations were terminated in 1961 after completion of the contract. Mining methods employed during this period are described in detail, and cost data are presented by years for 1953 through 1959. Ultramafic rocks of the Stillwater complex in Montana contain the largest domestic resource of chromite, and the Mouat mine has been the largest producer. Mine reserves were estimated in 1960 to be about 4.4 million tons containing 22.5 percent Cr2O3. The chromite deposits occur as a series of overlapping bands or lenses roughly paralleling the steeply dipping layers of the complex. Only two of the chromite layers have proven to be of economic importance. One layer is 2 to 16 feet wide; the other is 3 to 8 feet wide. Shrinkage stoping was generally used throughout the mine, but various methods of ore breaking, stope drawing, chute construction, etc., were tested to improve output and lower costs. Long-hole stoping proved to have limited use. Breasting down benches, developed outward from the center of the stope with air-leg drills, was satisfactory only in wider stopes. At the close of operations, the company had standardized the use of lightweight stopers to advance a flat back by breaking from a centrally located face. Mining costs were reduced 47 percent during 7 years of operation.

Jan 1, 1963

By T G. Callcott

Australian coking coals are either class 434<tlj534<2l, at Port Kembla, or 634<3> at Newcastle. The former yield good blast-furnace cokes; the latter yield poor ones. However, increases in conventional strength indices, by methods applicable with normal coking ovens, seem unlikely to be economically attractive. Characterization of the coals has enabled an "economic" blend to be developed in the Newcastle area, and this has affected mining, preparation and handling operations. Coking studies have led to a specification for the making of strong coke, especially from the high-volatile Newcastle coals. Continuous coking studies, developed from the efforts to make very strong coke, have taken two directions. Firstly, coking thin layers of coal on strands; secondly, coking, in various types of vessels, compacts of coals with or with-out the inclusion of non-coking coals, iron ores or other inert materials. Gas, "sand" and hot metal coking have been tested for use in compact coking. Particular attention has been paid to pellets of coal and ore. The probable industrial problems in adopting any of the ideas are presently being examined.

Jan 1, 1963

By M. G. Nicholas

The influence of deformation, relative movement and surface cleanliness on the strength of room -temperature "interparticle" bonds between copper surfaces has been studied. No bonding resulted when clean surfaces were merely pressed together, even under pressures of 50,000 psi. Bonding resulted, however, when clean surfaces were simultaneously pressed and moved relative to each other, some bonding occurring no matter how small the pressure or relative movement. Exposure of the clean surfaces to various chemicals inhibited bonding, none at all being produced by small relative movements. The size of the movements which first produce bonding between exposed surfaces depends on the nature of the chemical, being less than 0.002 in. for cleansing reagents and greater than 0.004 in. for lubricants, water and hydrogen sulfide. It is concluded from the experimental data that the prime requirement for bonding is the dispersal of surface films such as oxides and adsorbed contaminants. THE formation of interparticle bonds during the room-temperature compaction of powder metallurgy components greatly increases the ease of handling in subsequent production operations prior to sintering. The strength of unsintered compacts follows the same general trends as their density and hardness, but quantitative data are extremely Scarce. Quantitative correlation of the data on the overall strength of a compact with that of the individual interparticle bonds is virtually impossible due to the extremely complex geometry of powder compacts. Qualitatively, however, the strengths of unsintered compacts can be correlated with variations in parameters known to influence the extent of cold bonding, and hence interparticle bonding, such as surface cleanliness, relative movement, and deformation of the mating surfaces. Kuzmic and seelig4 found that contamination of powder particle surfaces with lubricants reduced the strength of unsintered iron and copper compacts. Interparticle shear has been shown to promote bonding by Train and Hersey7 while Gregory has shown that die rotation is beneficial. Eilender and schwalbe6 concluded that most bonding occurred during the early stages of pressing iron powder compacts when interparticle shear is one of the principal processes occurring. mile there can be little doubt that these and other factors, such as particle size and shape, affect the extent of interparticle bonding produced by compaction, evaluation of the influence of individual factors is not easy. Particle deformation and relative movement, for example, occur simultaneously during compaction, making any precise measurement of their relative influences difficult. Because of these and other difficulties encountered in studying interparticle bonding in actual powder compacts, the approach adopted in this study was to

Jan 1, 1963

By Lindsay D. Norman

Four chloride and seven fixed-nitrogen processes for recovering manganese from domestic resources are described. The chloride processes are divided into two classes (leaching and chloridization) depending upon the major operation responsible for converting the manganese minerals to the chloride from which manganese oxide products are obtained. The fixed nitrogen processes, all of which yield high-grade manganese oxide products, are essentially either leaching or roasting processes. The 11 processes include HC1 leach, HC1 chloridization, HC1 chloride volatilization, CaC12 chloride volatilization, NO2 leach, HNO3-NO2 leach, NH3-CO2-H2O system leach, (NH4)2SO4 leach, (NH4)2SO4 roast, and ammonium salt roast.

Jan 1, 1963

By Michael Sokaski

A dense-medium cyclone pilot plant was built to clean 112-inch to 0 size coal. This pilot plant does not require the removal of the extremely fine material (usually minus 1/2-mm) from the feed, which is necessary in conventional dense-medium cyclone plants. The essential difference between conventional cyclone plants and the pilot plant is in the medium-recovery system. The latter uses a combination of sieve bend screens, classifying cones, and magnetic separators for medium recovery. Eight tests were run in the pilot plant at a feed rate of 5 tons per hour with four different raw coals and one crushed jig middling product. Sharp separations were obtained as indicated by an average error area of 27 and probable error of 0.047 for the 112-inch to 200-mesh size range. Magnetite loss averaged about 2.5 pounds per ton of feed. The influence of several factors on cleaning performance of the cyclone was investigated. The diameters of both the overflow and underflow orifices were found to be important for optimum cleaning performance, but these diameters could vary over a wide range without serious effect; however, if this range was exceeded, cleaning performance deteriorated. Better cleaning performance was obtained when the cyclone inlet pressure was increased from 9 psig to 13 psig. The size of the magnetite particles in the medium was found to have a substantial effect, and the best cleaning results were obtained with grade B magnetite. Demagnetizing the magnetite in an effort to decrease the effective particle size did not improve cyclone performance.

Jan 1, 1963

By Warren C. Gerler

An overland belt conveyor system is installed for only one reason to save money. It must pay its way on a ton-mile basis over a stated period of time, and do so in competition with other forms of transportation. Such a system with its economies has recently been installed at Simco-Peabody&apos;s mine near Coshocton, Ohio by Link-Belt Company. Three miles in length, this system carries coal from open pit and underground mining facilities to the Conesville Power Plant of Columbus & Southern Ohio Electric Company. The coal was formerly trucked from the mine direct to the power plant; but over the years the mining operations have moved progressively farther and farther from the plant, making the over-the-road hauling distance correspondingly greater. Simco-Peabody has mining operations over a considerable area just east of the Conesville Station. The majority of the coal is recovered by conventional strip mining. Some underground mining` is performed by the high wall method.

Jan 1, 1963

By Peter Moon

THE mineral industry of Canada relies heavily upon the talent of its technical men. It is vital to the well-being of the industry that its supply of young, trained men be adequate. At the present time, the industry is acquiring only 200 new graduates a year. The shrinking supply is far below present and future requirements. Other industries and research organizations are competing for engineers and scientists. Dr. J. B. Mawdsley (1), Past-President of the Canadian Institute of Mining and Metallurgy, has recently outlined a program designed to attack the problem. Dr. J&apos;. C. Sproule (2), another former President of the Institute, has stated that: "The need for selection of trainee material is commonly recognized, but little is done about it." The following paper contains a short discussion of occupational interests, and outlines research, using psychological knowledge and measuring techniques, aimed at the identification of desirable recruits for the mineral industry.

Jan 1, 1963

By Forrest T. Moyer

To keep the mineral and allied industries informed of trends in the causes of accidents and to point out the need for corrective measures, the Bureau of Mines collects, analyzes, and publishes, periodically health and safety statistics. This report includes data for 1961 on injury experience, with related employment statistics, at coal mines in the United Status. These data are presented in tabular form under the following headings; General Injury Experience Tables 1 to 6: Current data on number of injuries, degree of injury, frequency and severity rates, average severity, and related employment and production data by work location.

Jan 1, 1963

By F. D. Everett

This report, based on information made available by four uranium-producing companies, describes the geology, exploration, open-pit development and mining, and shaft sinking in the Gas Hills uranium district of Wyoming. Open-pit stripping features motor-scrapers push-loaded by crawler or rubber-tired tractors. The ground generally can be ripped, and little blasting is necessary. Detailed data are given on grouting for ground stabilization in sinking a small-diameter shaft in the relatively unconsolidated sandstone and siltstone, Cost and performance data are presented as made available by the companies.

Jan 1, 1963

By Scott W. Hazen

This Bureau of Mines report presents the results of a study and statistical analysis of part of the initial exploration churn-drill sampling and some of the subsequent underground diamond-drill-core sampling in the North are body at the San Manuel copper mine, Arizona. These data were derived from regular exploration and mine sampling, not from special samples obtained solely for statistical analysis. The study was conducted as part of the Bureau&apos;s continuing program on sampling-methods research. The major objective of the study was to investigate the feasibility of using the techniques of statistical analysis in evaluating sample and assay data and computing grade and tonnage of Ore from porphyry-type copper deposits. It was recognized that using existing data acquired over a period of several years by different methods would introduce problems and limitations for precise comparisons. However, it was expected that the study would provide some general conclusions and certainly a number of preliminary conclusions on the nature of the mineral characteristics and their effect on sampling procedures, the requirements for sampling deposits of this type, and the comparative results of churn-and diamond-drill sampling in the same area of the deposit. All of this information would be essential for future sampling-methods research for computing grade and tonnage of ore.

Jan 1, 1963

By W. R. Hardwick

This Information Circular describes copper mining and concentrating methods, practices, and costs at the Silver Bell Unit of American Smelting and Refining Co., Pima County, Ariz. It is one of a series being prepared by the Bureau of Mines on mining methods, practices, and costs in various mining districts of the United States. The Silver Bell mining district, one of the older districts in Arizona, is in the western part of the Silver Bell Mountains in Pima County, about 40 miles west of Tucson and about 20 miles southwest of Red Rock, a station on the main line railroad of the Southern Pacific Co. The Oxide and the El Tiro open-pit mines of the American Smelting and Refining Co. are in the district (fig. 1. The principal ore deposits are in T. 12S., R.8E., Gila and Salt River base line, at an altitude of about 3,000 feet. The present town of Silver Bell, established in 1952, is reached by a paved highway, the Avra Valley road, that turns west from Highway 84 at Plata siding near Rillito and extends westward 25 miles to the townsite (fig. 2). The present town is about 5 miles southeast of the old town of Silver Bell that flourished from 1900 to 1930.

Jan 1, 1963

By T. J. Koppenaal

The surface slip line structure has been investigated by optical microscopy during the easy glide deformation of Cu-A1 single crystals as a function of composition, testing temperature and prior thermal treatment. The slip line structure in alloys of 2.5 or less at. pct Al is similar to pure copper, while alloys of 5 or more at. pct Al show slip tracings typical of a brass. Cross slip is observed in the "a-brass type" crystals and the amount of this type of slip increases rapidly with aluminum content. The cross slip tendency in 14 at. pct Al crystals is signicantly higher when tested at 150°C as compared to 4.2" and 77°K. In addition, cross slip is more pronounced in this alloy in the furnace cooled condition than when quenched from 450°C. The cross slip behavior is analyzed in terms of existing models for this type of deformation. In two previous investigations, reports of yield points1 and solid solution strengthening2 in Cu-A1 single crystals have been given. This paper enlarges upon the brief description of the slip line structure discussed in these reports. Since the easy glide slip line pattern of copper changes markedly with the addition of -30 pct Zn (-brass),3 a study of slip lines as a function of solute additions in Cu solid solutions should help to explain some of these differences. In addition to composition variables, slip lines have also been studied as a function of testing temperature and prior thermal treatment. PROCEDURE The slip line observations were made on single crystals of 0.5 to 14 at. pct Al using a light microscope. Details concerning the preparation and basic testing procedure are given elsewhere.&apos; Prior to testing, each crystal was homogenized at 900°C for 24 hrs, furnace cooled, and electrolytically polished in a 60 pct phosphoric acid solution. The strain rate was-5 X 10 sec-I in each case. Unless otherwise stated, all observations reported upon here were made during the early stages of easy glide. RESULTS AND DISCUSSION The maximum magnification generally used was 1000X, and slip lines could be resolved down to about 105 cm (1000A). This resolution is appreciably less than obtainable with electron microscopy replica techniques where the replication can resolve slip lines down to about 40 A. Thus, while many qualitative features could be studied, the type of quantitative data obtainable with an electron microscopy replica study could not be made. Crystals containing 0.5 and 2.5 at. pct Al deform much like pure copper exhibiting a high density of fine slip lines that cover the entire gage length of the specimens. Fig. 1 shows the surface slip line pattern in a 2.5 at. pct A1 extended 0.01 shear strain at room temperature. Crystals having 5 to 14 at. pct A1 showed appreciably coarser slip lines that were generally concentrated at one end of the gage length. During easy glide these coarse slip lines propagate along the gage length in a manner similar to that observed in a-brass single crystals by Piercy, Cahn, and cottrel14 and refered to by them as a Lüders band propagation. Fig. 2 shows a typical area of these coarse slips in a 14 at. pct A1 crystal after a room temperature shear strain of 0.01. Two slip systems were apparently active. Using a method described by Cullity, the angles, between the specimen axis and the normals of the primary and secondary slip planes were determined to be 50 and 84 deg, respectively. &apos;From the Laue photograph, was 52, 81, 66, and 30 deg for the primary, cross, conjugate, and fourth slip planes, respectively. The secondary active plane in Fig. 2 is thus established as the cross slip plane, and the operative slip system is evidently the cross slip system, e.g., slip

Jan 1, 1963

By L. K. Weaver

The Bureau of Mines has started an engineering study of oil recovery by miscible-phase displacement. As a preliminary part of the investigation a literature and patent study was made to prevent duplication of work already done, to become acquainted with those actively engaged in research of this type, and to learn where the recovery method has been attempted. This bibliography gives results of this study. The bibliography includes 254 references to U.S. and foreign patents and published literature relating to miscible-phase displacement processes of oil recovery. It is divided into the following sections: (1) U.S. patents, (2) foreign patents, (3) literature references, (4) author index, and (5) publication and source reference. The patents and literature references are listed alphabetically by author by intervals of years. References to February 1963 are included.

Jan 1, 1963