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By R. J. Weege, A. W. Schillinger

Conventional underground mapping methods and diamond drilling are being applied in a study to determine the nature of the copper ore occurrences near the footwall of the Osceola lava flow top, commonly referred to as the Osceola Amygdaloid. The work to date suggests that structures formed by relatively impermeable barriers, created by flowage and injection of still-molten lava from the interior of the flow into the solidified, brecciated crust, acted as the ore receptacles. Ascending hydrothermal fluids traveling near the footwall contact were trapped and confined in these barriers which retarded the direct upward movement of the ore fluids and caused deposition of copper. Oreshoots located near the footwall appear to have been formed spatially independently from the hanging-wall oreshoots by fluids traveling simultaneously, but along different channelways. The barrier concept, as advanced by earlier writers to explain the concentration of the ore-bearing fluids into broad shoots constituting entire ore bodies, is found to be equally as applicable for the localization of smaller oreshoots within the Osceola ore body. Recently, the Calumet Division of Calumet and Hecla, Inc. completed the unwatering of the old mine workings on the Osceola amygdaloid. Two shafts were subsequently reactivated and mining commenced on the Osceola lode after an idle period of over 20 years. Early in 1961, the Calumet and Hecla Geological Dept. was assigned the task of locating additional reserves. Accordingly, an intensive mapping and underground diamond drilling program was initiated. Except for a very few years following the first mining on the amygdaloid, the Osceola lode had never been a high grade producer. It was, therefore, recognized from the onset that a concentrated effort would have to be made by the mining, milling, and geological departments to insure success of the project. Company reports contained many references to ore that had been located near the footwall of the Osceola amygdaloid. Information concerning the grade of this ore was meager, but it was known that at least some was very rich. In contrast to ore that occurred near the hanging-wall, however, the footwall copper did not appear to have a systematic distribution and a large amount of poor rock had to be removed in developing this ore. This, of course, resulted in high development costs and discouraged any extensive mining of footwall ore. The possibility of more continuity than had previously been suspected was recognized by other workers, in particular Dr. T. M. Broderick, formerly Chief Geologist of Calumet and Hecla, who suggested attempts be made on a trial basis to follow the footwall contact with the main development drift. As most mining was done on the Osceola lode before a geological department had been established by the company, and almost all of these openings are now caved, very little information concerning the geology of footwall ore was available. It was, therefore, decided that the first step in the exploration program would be to become familiar with footwall ore occurrences by mapping the geology as the openings were driven. It was possible that a mapping program would reveal the features that controlled the localization of the ore. Furthermore, if it could be shown that footwall ore was more continuous, or if its distribution was more systematic than generally believed, it would be possible to produce a high grade ore that could be blended with the lower grade hanging-wall ore. In connection with the geological program, the Michigan College of Mining and Technology Geophysical Dept. under the direction of Professor Lloyal Bacon, is making a geophysical study of the problems of locating footwall ore by electrical methods. GENERAL GEOLOGY OF MICHIGAN NATIVE COPPER DEPOSITS The native copper deposits of Michigan are located in Keweenaw, Houghton, and Ontonagon Counties. The host rocks are Keweenawan in age and are comprised of interbedded sediments and lava flows which form a belt two to four miles wide and over one hundred miles long. These rocks form part of the south limb

Jan 1, 1962

By B. H. Bergstrom, W. Mitchell, C. L. Sollenberger

D. W. Fuerstenau (Associate Professor of Metallurgy, Dept. of Mineral Technology, University of California, Berkeley, Calif.) and D. A. Sullivan, Jr. (with the University of California) — Messrs. Bergstrom, Sollenberger and Mitchell have shown in two excellent papers that the energy per unit mass required for the breaking of spheres is inversely proportional to the size modulus of the fragments of the broken spheres. They found that the fragments of spheres broken within a steel enclosure were finer than those produced by breaking spheres encased in gelatin. This results from utilization of part of the strain energy at fracture for secondary breakage. For spheres not encased in gelatin, these authors found that after fracture the fragments of the spheres possess kinetic energy amounting to 45% of the strain energy needed for initial fracture. Breakage of a sphere in gelatin results in waste of this kinetic energy, whereas breakage inside the steel container makes use of this kinetic energy for further size

Jan 1, 1962

By W. C. Winegard, E. L. Holmes

The effects of the solute elements lead and bismuth on grain growth in zone -refined tin have been investigated. At low temperatures, viz. below 160°C. or at high concentrations, viz. greater than 0.03 at. pct, the temperature dependence of grain growth was found to be constant. A correlation was found to exist between the rates of grain growth in the presence of solute impurities and the factor [C Ir - 1]2 , where C is the solute concentration, r is the radius of solvent atom, and r' is radius of solute atom. It is shown that the Liicke and Detert theory does not give a satisfactory explanation of the results obtained. INVESTIGATIONS of grain growth in zone-refined lead and tin and some effects of solute elements on grain growth in these metals have been reported by Bolling and winegardly2 and Holmes and winegard? The present investigation is an extension of the previous work, and was undertaken to provide additional results which might make it possible to discover the mechanism whereby the rate of grain growth is affected by the presence of foreign solute atoms. The experimental procedure was exactly the same as that described previously.3'4 Figs. 1 and 2 show the results obtained with lead and bismuth additions over the same temperature range, viz. 167" to 220°C, as that used for the investigation of grain growth in zone-refined tin.3 Fig. 3 shows the results obtained for zone-refined tin and for this tin with lead solute additions over an extended temperature range. DISCUSSION OF RESULTS As mentioned previously,3 the character of grain growth in the particular zone-refined tin used in these experiments appears to change as the temperature of annealing falls below about 160°C. The grain growth became somewhat irregular and was characterized by a jaggedness of many of the grain boundaries. The reason for this change is not known, but may be due either to residual impurity effects or possibly an oxide precipitation. It was obvious that normal grain growth only occurred in the zone-refined tin through the high-temperature range 167" to 220°C, and so the effects of solute atoms on grai11 growth over the two temperature ranges will be discussed separately. a) Effect of Impurity on Grain Growth in the Temperature :Range Above 167°C. It is apparent from Figs. 1 and 2 that, for low concentrations of solute, the rates of grain growth tend towards a common value as the melting temperature of tin is approached. As the concentration of lead is increased, the rate of grain growth close to the melting temperature is also reduced, and at high concentrations the temperature dependence of the rate of grain growth appears approximately constant. It should be noteil that the effect of bismuth is greater than that of the same concentration of lead, but both these solutes have a smaller effect on the rate of grain growth than silver, as seen from an earlier investigation of Holmes and Winegard. It should

Jan 1, 1962

By Ralf M. Kleine

THE property of Consolidated 1 Discovery Yellowknife Mines Limited, (Figure I) is situated in the Northwest Territories, approximately 50 air miles north of the town of Yellowknife. The mine is reached by a shaft which extends from surface to a depth of 4,000 feet, with working levels established at 1 50-foot intervals. Stopping operations are carried on throughout a vertical range of 2,000 feet, with both shrinkage and cut and fill methods being used, depending on the ground conditions. Production started in 1950 and milling is done in a 1 65-ton per day cyanide plant. During ten months of the year, the property is serviced entirely by air, utilizing charter aircraft from Yellowknife. A 4,000-foot runway near the mine was constructed from mill tailings. This strip is adequate to receive Bristol freighter planes carrying heavy loads. Other servicing is done by Otter aircraft, equipped with skis or wheels for winter and with pontoons for summer operations.

Jan 1, 1962

By C. E. Lundin, D. T. Klodt

The binary alloy systems, Y-Ti, Y-Zr, and Y-Hf, have been investigated throughout their entire composition regions. There is no compound formation in any of the systems, and each system is characterized by a single eutectic reaction. The eutectic compositions and temperatures are as follows: A eutectoid reaction pct Y and 870°C occurs in the Y-Ti system, whereas a peritectoid reaction,: pct Y and 880°C occurs in the Y-Zr system. Peri-tectic-type reactions at temperatures above the eutectic levels are postulated for the yttrium and hafnium transfovmations. The development of the technology of yttrium has been given considerable attention during the past few years, and studies of binary phase equilibria have, of course, taken a prominent position in this development. In many respects yttrium, in the third group of metals of the periodic table, is similar to the adjacent group of metals, titanium, zirconium, and hafnium, and the knowledge of the phase relationships of yttrium with these metals is basic to their technology. MATERIALS AND EXPERIMENTAL PROCEDURES Materials. The metals for this investigation were supplied by the General Electric Co., Aircraft Nuclear Propulsion Department. The yttrium was in the form of an arc-melted ingot, and the other metals were in the form of high-purity, iodide-Process crystal bar. Table I lists the purities of these materials. Alloy Preparation. Melting was done by conventional techniques in a nonconsumable electrode arc furnace in an atmosphere of purified argon. Melting conditions for each binary system were the same. Each alloy button was inverted and remelted several times to assure homogeneity. Accurate weights of the charges and resultant alloy buttons were obtained to indicate deviations from intended compositions. No chemical analyses were obtained since melting weight losses were consistently in the range of 0.1 to 0.2 pct of the total weight. 10- or 20-g buttons for each 5.0 wt pct composition increment were melted to survey the three individual alloy systems. Additional alloys differing in composition by 1.0 or 0.1 wt pct increments were also melted to study selected regions of the systems. Metallograpllic Techniques. Standard metallo-graphic techniques were followed for mounting and rough grinding. Preliminary polishing was accomplished using 6-u diamond paste as an abrasive on a Metcloth Lap. Final polishing was done on a Microcloth-covered wheel using 1-u diamond abrasive paste. Purified kerosene was used as a lubricant for both polishing stages. • sothermal- Annealing. Alloys were sectioned for as-cast structlure examinations and then homogenized in preparation for isothermal-annealing treatments. Homo{:enization was accomplished by cold pressing the alloy buttons followed by 72-hr anneals at 1100c. The alloys were encapsulated in Vycor or quartz for the homogenization treatments or for isothermal anneals. Resistance-wound or resistance-element tube furnaces were used for the annealing treatments. The homogenized alloy buttons were cold rolled until cracking occurred or until a -in. specimen thickness was obtained. Small -in. square) specimens for the isothermal anneals were then sawed from the alloys. Each specimen was wrapped in tantalum foil before being sealed in the capsule. Temperatures during the anneals were controlled The time at temperature necessary to equilibrate the structures during the anneals was determined for each alloy system by holding triplicate specimens of alloys at a constant temperature for three different periotls. The specimens were quenched and examined microscopically to determine the number and amounts of phases present in the micro-structure as a function of time. Melting Studies. Eutectic temperatures of the three alloy systems were established from the results of incipient-melting studies conducted on as-cast alloys. Specimens to be melted were suspended on a tungsten wire inside a graphite cylinder placed in a glass vacuum chamber. An optical pyrometer was used to follow the temperature of the specimen as it was inductively heated in a high vacuum. The temperatures were corrected for emissivity losses by standardizing the pyrometer with known-melting-point metals. Accuracy of the temperature measurements is estimated to be + 10°C. The melting point of the yttrium was determined to be 1550°C by this technique. The invariant-temperature levels were also checked by an anneal-quench technique. This technique consists of annealing a series of

Jan 1, 1962

By Alla D. Mah

The heat of formation of scandium sesquioxide (Sc203) has not been measured previously, and existing values for gallium sesquioxide (Ga203) are subject to large uncertainties. As a consequence, thermodynamic calculations involving these oxides hare lacked scientific exactness. This paper reports newly determined values of the heats of formation of gallium and scandium sesquioxides at 298.15° K., by combustion calorimetry. The corresponding free energies of formation are derived from heat and entropy data.

Jan 1, 1962

By R. M. Caves

High-purity dense tungsten coating is obtained by means of a modified de Boer-van Arkel iodide process using tungsten bromides. The all-glass reaction system is pumped, baked, and sealed (pinched-off) at about 10-7 mm Hg pressure. The bromides then formed in situ are decomposed, depositing tungsten on heated tungsten surfaces. Heating of the specimen is done inductively in a novel arrangement that avoids electrodes of glass-to-metal seals. The tungsten, deposited at specimen temperatures from 2000° to 2800°F and bulb (halide) temperatures of 225" to 725°F, was adherent and uniform, and ranged in thickness to 1/8-in. REFRACTORY metals are of interest at NASA for use in hypersonic aircraft, in rocket engines, and in other thrust devices where very high temperatures are encountered. Tungsten, with a melting point about 6100° F, is potentially very useful for some of these applications. Considerable research on tungsten and its alloys is currently being conducted at the NASA Lewis Research Center. In this tungsten research program, there is need for a method of depositing high-purity, nonporous tungsten coatirlgs. Metallurgical bonding of the coating both to itself and to the substrate is required. In addition, it is necessary to be able to deposit thin, uniform coatings on substrates of a variety of shapes and sizes for laboratory test purposes. A survey of the methods previously used for depositing tungsten coatings indicated that none would likely meet these requirements for high purity, good uniformity, and high density except thermal decomposition of the halides. The method for coating that was selected for investigation was the thermal decomposition of tungsten bromide. This is a variation of the van Arkel and de Boer iodide process established years ago and recently reviewed.1,2 This process is applicable to the transition metals in general. More recently, the application and techniques were extended with chlorine3 and fluorine,4 and included the coating of tungsten. This is believed to be the first report on the use of the bromide for tungsten coating. Bromine was chosen over the other halogens because it promised a lower temperature for tungsten

Jan 1, 1962

By N. S. Kenny, A. A. Burr

THE purpose of this note is to present evidence that vacancies, which have been produced by quenching from a high temperature, alter the rate of strain-hardening of an hep single crystal. The majority of investigations of the effects of quenched-in vacancies on the yield stress of metals have been made using fee samples in the form of thin wires. However, there is an inherent disadvantage in using such wires to study the effects of vacancies on the rate of strain-hardening of metals because fee wires begin stage II slip either immediately upon yielding or very shortly thereafter. When stage II slip occurs, very rapid strain hardening also occurs, masking the effects of vacancies on the rate of hardening. In this investigation single crystals of magnesium hep were studied since magnesium has only one slip plane at low temperatures and has, therefore, an extensive easy glide region. In addition, the effect of both static and dynamic recovery on the rate of hardening were eliminated by testing in liquid nitrogen. Both forms of recovery occur in hep metals by dislocation climb, which is a diffusion controlled mechanism and is negligible at liquid nitrogen temperatures. Finally, the dependence of the strain-hardening rate on the crystal orientation was eliminated by using the equations of Schmid and Boas.' Variations in the strain-hardening rate could, therefore, be attributed to the presence of vacancies. Single crystals in the form of rods approximately 5 mm in diam and 6 cm long were grown by a modified Bridgman technique from commercial high-purity magnesium (99.97 pet) supplied by the Dow Chemical

Jan 1, 1962

By T. D. Tiemann

The caustic extraction of silica from Wisconsin and Minnesota taconite was investigated by bomb digestion over the temperature range from 312 to 40S°F at caustic concentrations from 25 to 500 gpl. Residual concentrates containing as much as 65 pct iron were obtained. The high rate of silica extraction is related to a microcrystalline variety of quartz, since it is shown that the rate of extraction of silica from quartz is directly proportional to its surface area. Increasing dependence on foreign ore reserves makes the need for developing the technology necessary for treatment of our low grade ores even greater than it was at the time of World War 11, when much research was conducted on the extraction of alumina from clays. Representative of these were the studies carried on at the University of Illinois.' More recently, the U. S. Bureau of Mines investigated the production of alumina from anorthosite, and currently the aluminum industry is showing renewed research interest in this field. The studies reported here are part of a continuing research program based on the above concepts and aimed at the eventual development of processes for the treatment of low grade ores, particularly those of iron. The fact that large reserves 3 of low grade nonmagnetic taconite are contained in the iron formation of the Wisconsin Gogebic range have made this ore an important and attractive target for investigation. The idea of removing silica by caustic extraction is not new.495 The digestion in caustic solution of ground flint, diatomite, and other forms of chalcedonic silica is the basis for the production of soluble sodium silicates by the wet-process. Upgrading bauxites by the caustic extraction of silica has been investigated6 and is the subject of a German patent.7 Although mention is made by Roe' of the caustic extraction of silica from low grade Michigan and Wisconsin iron ores, and he lists a number of patents and references on the subject, recent work in the field does not appear to be extensive. As far as the author knows, there has been no work in this field on these particular ores. It is hoped that this paper will stimulate further investigation which will eventually lead to an econclmic means of processing these large low grade reserbes. TACONITES The taconites investigated in this study were from Minnesota and Wisconsin. That from Minnesota, a semi-taconite, Nas obtained from the Oliver Iron Mining Division, U. S. Steel Corporation, and represents a sample of an oxidized iron formation from their King Mine on the Mesabi range. The Wisconsin taconite came originally from the trench sampling of the U. S. Bureau of Mines, and represents a composite of the Norrie, Pabst, Yale, Plymouth, and Pence members of the Gogebic iron formation. Assays on these samples are given in Table I. A typical calcu1atr:d average analysis of the Wisconsin taconite is given in Table 11. Chemically, the Minnesota semi-taconite sample contains about 39 pct iron and 39 pct silica, while the Wisconsin taconite contains 30 pct iron and 53 pct silica, both on the dry basis.

Jan 1, 1962

By J. L. Potter

An inert-gas fusion technique was applied by the Bureau of Mines to the oxygen analysis of mixed-fluoride electrolytes used in electrowinning uranium and the rare-earth metals. Method development included: (1) Thermodynamic and experimental evaluation of the temperature required to quantitatively remove oxygen from a fluoride melt; (2) installation of a water and an acid trap to entrain the volatilized fluorides; (3) development of a suitable sample-preparation technique for the heterogeneous fluoride baths in which both pulverizing and pelletizing were necessary to achieve reproducible results; (4) comparison of platinum flux and dry crucible techniques, which showed that the use of platinum was not necessary. The accuracy of the method was evaluated by analyzing fluoride baths containing known amounts of oxygen added as the metal oxide. In the 0.05-to 0.5-percent range, the relative error was about ±5 percent.

Jan 1, 1962

By H. C. Fiedler

A high degree of cuhe-on-edge grain orientation and good magnetic properties were obtained in Si-Fe strip processed from laboratory heats containing vanadium nitride inclusions. The higher the nitrogen content the greater was the restraint on normal grain growth and the greater was the ability to undergo secondary recrystal-lization. The degree of restraint in a heat containing magnanese sulfide inclusions was slightly greater than that in the lowest nitrogen vanadium nitride heat. The high rate of diffusion of nitrogen in the temperature range in which the texture is developed makes it necessary to retard the loss of the inclusions until the texture has been developed. MAY and Turnbulll have shown that to develop the cube-on-edge secondary recrystallization texture in Si-Fe it is necessary that inclusions, such as manganese sulfide, be present to prevent normal grain growth. They showed that the driving force for the growth of the secondary grains is inversely proportional to the diameter of the matrix grains, and that the function of the inclusions is to maintain a small matrix grain size. Fast3has developed cube-on- edge texture in Si-Fe by nitriding the hot rolled band. The silicon nitride thereby formed promotes secondary recrystallization during the anneal of the final gage strip. To obtain the best magnetic properties, the inclusions must be removed from the strip after the grain orientation has been developed. Nitride inclusions have an inherent advantage over sulfide inclusions in that the greater diffusivity of nitrogen as comared to sulfur permits the use of shorter times and or lower temperatures for the purification heat treatment. The purpose of the work to be described was to examine the usefulness of vanadium nitride inclusions in developing the cube-on-edge texture and to determine the magnetic properties of oriented strip made from heats containing these inclusions. A comparison is made with a heat having had iden-

Jan 1, 1962

By R. Janes, F. Everard

Pilot plant studies have been conducted on a variety of iron ores of differing composition and grain size to test their amenability to dry autogeneous grinding and dry magnetic concentration. A general description of the pilot plant and its equipment is given with particular reference to the Aerofall mill and the dry magnetic separators developed by the Ontario Research Foundation. Test results are reviewed in detail with emphasis on power consumption, mill speed, the use of ball charges, types of ores, moisture content, separator speeds, and design. In 1957 the Ontario Research Foundation installed a pilot plant (Fig. 1) for the study of dry autogenous grinding and dry magnetic concentration of iron ores. A 61/2-ft Aerofall mill was installed as the dry autogenous crushing and grinding medium. The Cavanagh fast drum and the Double Helix, two dry magnetic separators developed at Ontario Research Foundation, were also installed. Iron ore samples of 10 to 150 tons have been investigated. These ores varied widely in mineralogy and grain size. Taconite (-325 mesh), fine-grained magnetite (200 to 325 mesh), and medium-grained magnetites (65 to 150 mesh) have been treated with varying degrees of success. Lately, considerable research has also been conducted on the metamorphosed magnetite-hematite complexes of the Labrador Trough. Operational and metallurgical data have been compiled from these tests. The effects of ore type, air flow, mill speed, and ball charge on mill operation are discussed. Metallurgical data are also presented to illustrate the operation of the dry magnetic separators. PILOT PLANT DESCRIPTION Fig. 2 depicts the normal flowsheet used. Minus 6-in. ore from a vibrating feeder is fed to the 6%-ft Aerofall mill powered by a 50-hp 550-v induction motor. The main blower, a 25-hp 550-v fan rated at 7000 cfm, draws air through the mill. Finely ground ore is conveyed by the air stream to a horizontal classifier, where expansion and a change in direction cause the +I50 mesh fraction to fall onto a vibrating

Jan 1, 1962

By H. B. Probst

Mechanical twins were produced in zone-refined tungsten single crystals by explosive working at room temperature. These twins are parallel to (112) planes and have irregular boundaries rather than the classical plane twin boundaries. These boundaries aye grooved surfaces in which the grooves themselves are parallel to a <111> direction and the sides of the grooves appear to be par-allel to (110) planes. TWINS were produced in tungsten single crystals by explosive working at room temperature. These twins differ in character from any previously reported for tungsten; however, they are similar to those found in molybdenum after compression at -196°C.1 Deformation twins "resembling Neumann bands in ingot iron" have been observed in tungsten by Bech-told and Shewmon.2 This observation was made with sintered polycrystalline tungsten pulled in tension to fracture at 100°C and using a strain rate of 2.8 x 10-4 sec-1. More recently Schadler3 found deformation twins in zone-refined tungsten single crystals pulled in tension at -196"&apos; and -253°C. These tests were conducted using a strain rate of 3.3 x l0-4 sec-1, and the twin bands were found to be parallel to a (112) plane. Deformation twins in tungsten&apos;s sister metal, molybdenum, were observed by Cahn.4 These twins were produced by compressing small (0.7 mm) vapor-deproducedposited molybdenum single crystals at -183°C. The compression was performed &apos;by impact." By the use of precession X-ray techniques, Cahn was able to identify the twin plane as {112} and the shear direction as <1ll>. Mueller and Parker1 produced deformation twins in polycrystalline electron-beam-melted molybdenum by compression at -196°C. Their "loading rate" was 5000 psi per min which, judging from their stress-strain curve, corresponds to a strain rate of approximately 0.3 x 10-4 sec-1. These twin bands were found to be parallel to (1 12) planes; however, they differed in appearance from previously observed twins. In place of straight and parallel twin boundaries they were found to be irregular, jagged, and sawtoothed. The sides of the saw teeth were identified as (110) planes and irrational planes of a (111) zone. The twins observed in the present work in tungsten single crystals are similar in appearance to those of Mueller and Parker in polycrystalline molybdenum. The starting material used in this investigation was 3/16-in. diam commercial tungsten rod produced by powder-metallurgy techniques. This material was converted to a single crystal by the electron-bombardment floating-zone technique.= The process was carried out in a vacuum of 10-5 mm of Hg using a traversing speed of 4 mm per min. Segments (=2 in. long and 3/16 in. in diam) of two crystals (A and B) produced in this manner were studied. Crystal A received one zoning pass, while crystal B received two passes. The two crystals were explosively worked at Bat-telle Memorial Institute in the following manner. A 1/2-in.-thick layer of plastic was applied to the crystals to serve as a buffer in an attempt to prevent cracking. The composite, crystal and buffer, was then wrapped with 1/8-in.-thick DuPont sheet explosive EL506A2 and detonated in water at room temperature. Metallographic samples of the worked crystals were prepared, and back-reflection Laue X-ray patterns were obtained using unfiltered molybdenum radiation. RESULTS AND DISCUSSION Blasting the crystals as described above failed to prevent cracking. The crystals fractured into several fragments about 3/16 to 1/2 in. long; however, the fragments were of sufficient size to be useful for the subsequent study. The diamond pyramid hardness of the crystals after blasting was in the range 430 to 450 as compared with 340 for the as-melted material, which shows a definite hardening resulting from plastic deformation. These hardness values were obtained using a 1000-g load and taking readings only in sound portions of the crystals free of cracks. The crystals exhibited profuse twinning as shown in Fig. 1. No such structure is present in the as-melted condition. Most of these twins have jagged twin boundaries and are similar in appearance to those found in molybdenum by Mueller and Parker. The twins in both crystals were found to be parallel to {112} planes. This identification was made by using the conventional two-trace method. Subsequent efforts to describe these twins more fully were carried out on crystal A. If the longitudinal axis of crystal A is placed in the (001)-(011)-(Il l) basic triangle of the standard cubic stereographic projection, as in Fig. 2, then the two sets of twins shown in Fig. 1 are parallel to the (112) and (121) planes. Fig. 3 shows a schematic representation of a twin with jagged boundaries. This type of twin with a <111>

Jan 1, 1962

By E. L. Singleton

This Bureau of Mines investigation was initiated to study and establish some of the chemical and physical characteristics of the condensed Mno-Si02 system. To prevent oxidation of the manganous ion, I atmosphere of purified helium was used in the furnaces. Solidus-liquidus curves and invariant points were established from melting-point determinations and were supplemented from data obtained by the static-quenching method. Experimental findings and data are for the intermediate compounds of tephroite and rhodonite with their respective eutectics represented at 25.5 and 37.2 weight-percent silica. Tephroite melts congruently at 1,347° C., and rhodonite melts incongruently at 1,286° 8.. A metastable transformation was determined to exist at the 1,347° C. isotherm, the congruent melting point of tephroite. A composite X-ray-diffraction pattern was formulated for synthetic rhodonite. This investigation contributes fundamental data leading toward a better understanding of the more complex slag systems.

Jan 1, 1962

By E. A. Gulbransen, K. F. Andrew

Weight loss measurements were made using a sensitive microbalance operating in a high vacuum system. The Langmuir equation was used to Calculate the vapor pressures of the several metals and alloys. Aluminum lowered the vapor pressure of i9,on in a 5.4 Al-94.6 Fe alloy, and of iron and chromium in a 4.8 Al-21.5 Cr-73.7 Fe alloy. The influence of oxide films formed on the alloys on the effective vapor pressures of the alloys was also studied. These studies were used to aid in the inte9,pretation of the high temperature oxidation of alloys based on iron, chromium, and aluminum. RECENT studies on the oxidation of chromium1 and the heat resistant alloy 5 Al-22 Cr-73 Fe showed transitions in the rate of oxidation at 900o and 1050oC respectively. The transition for chromium occurred at a temperature where the rate of evaporation of chromium from oxide-free surfaces equalled the rate of chromium atoms reacting with oxygen. This paper presents new vapor pressure studies on iron, chromium, and the specially prepared alloys 5.4 Al-94.6 Fe, 21.9 Cr-78.1 Fe, and 4.8 Al-21.5 Cr-73.7 Fe. The ternary alloy is similar in basic composition to the patented heat-resistant commercial alloy known as Kanthal. The binary alloys were studied to show the individual effects of aluminum on the vapor pressure of iron and of iron on the vapor pressure of chromium. The purpose of the proposed studies was to test the influence of metal volatility on the oxidation behavior of heat-resistant alloys based on iron, chromium, and aluminum. Since oxide films formed on the metal may limit metal transfer to the surface, the influence of oxide films on metal volatility was also studied. LITERATURE A) Vapor Pressure. The vapor pressure of iron has been studied by Jones, Langmuir, and Mackay,&apos; Dornte and Nrton. Edwards. Johnston. and Ditmar. and McCabe, Hudson, and Paton. Stull and SinkeT have calculated a heat of sublimation at 298° K of 99.83 kcalper g atom. The vapor pressure of chromium has been reported by Bauer and Brunner,&apos; Speiser, Johnston, and Blakburn, Gulbransen and Andrew,&apos;&apos; Vintaikin,o McCabe, Hudson, and Paton, and Kubaschewski and Heymer.12 Good agreement was obtained except for the early work of Bauer and Brunner.&apos; Stull and Sinke7 calculate a heat of sublimation at 298°K of 95.0 kcal per g atom. Vapor pressure measurements on aluminum have been made by Brewer and Searcy,13 Bauer and Brunner,aand Farkas.I4 Stull and Sinke,7 giving Brewer and Seary&apos;s&apos; data the most weight, derive a heat of sublimation of 77.5 kcal per g atom at 298 oK. B) Method. Two methods15 are used for measuring the vapor pressure of metals: 1) The Langhuir free evaporation method, and 2) the Knudsen effusion method, In the Langmuir method, used in the present work, the vapor pressure of the metal P is given by the equation: Here M is the molecular weight of the vapor species. T is the absolute temperature. (dw/dt) is the rate of sublimation in g per sq cm per sec and a is the condensation coefficient. a is a measure of the efficiency of condensation of molecules striking the metal surface from the vapor. If condensation results from each collision a is unity. This coefficient has been found to be unity,a, le for metals. These results establish the general validity of the Langmuir free evaporation method as applied to metals. EXPERIMENTAL A) Vacuum Microbalance Method. A modification of the Langmuir free evaporation method was used. Strip specimens were suspended from a sensitive microbalance operating inside of a high vacuum system. For alloys, microbalance methods17 must be used on large area samples at relatively low temperatures to minimize composition changes. The

Jan 1, 1962

By Dexter C. Hatch

At MacIntyre Development of the National Lead Company, Taha s, New York,, the flotation plant was set up to recover ilmenite from the finer size fraction of the ore that cannot be efficiently treated in the main gravity-magnetic separa¬tion process. It was later expanded to handle the reground middlings from the tables wetherill magnetic separators. The ilmenite-magnetite ore is ground to minus 20 mesh in five 6 x 12 ft. rod mills in closed circuit with DSM screens. The minus 20 mesh screen undersize is pumped to four parallel sections each consisting of two rougher wet-magnetic separators and one cleaner separator for magnatite removal. The screen undersize from the fifth section is distributed to all four sections. The magnetite removed in the roughers is pumped back to the cleaners and the cleaner magnetite is dewatered in rake classifiers and carried by belt to the winter plant or the stockpile area. The nonmagnetic sands from rougher and cleaner magnetic separator are sized for table feed in eight pocket hydraulic sizers. The slime overflows from the Crocketts, the sizers, and the magnetite rakes are collected and pumped to three-inch cyclones for thickening and desliming. The cyclone underflow is the principal flotation plant feed.

Jan 1, 1962

By D. R. Rathburn

Jan 1, 1962

By Sara Jane Boles

In recent years the demand for products of greater refractoriness has placed an ever-increasing emphasis on ceramic materials, including the metallic oxides. Magnesia (MgO) is one of the most important of these oxides, exhibiting, as it does, high electrical resistivity, high slag resistance, and a melting point of 2,800° C. However, magnesia has a tendency to hydrate in the presence of water and to volatilize above 1,500° C. in certain kiln atmospheres and has a comparatively low resistance to thermal shock. Because of these disadvantages, the previously listed advantages inherent in this material have been largely overlooked, and research on magnesia has lagged behind that on oxides such as alumina and zirconia. This bibliography has been prepared in an effort to present to Government and industry a comprehensive picture of the prospects for greater utilization of magnesia as a refractory material in future research. To provide as selective and accurate a collection as possible, the references included cover magnesia in a pure state, not as an additive or in combination with other materials. However, several references discuss the effect of minor impurities (less than 5 percent of the total) on the properties of magnesia, as these papers are considered to be of special importance. A few references to articles on forming techniques are also included, as they are valuable additions to the overall treatment of the subject. The processes used in obtaining and refining the raw materials are adequately covered in earlier publications and are excluded. A number of references are omitted as being of questionable value in enhancing the cumulative study of pure magnesia as an ultra-high-temperature refractory material.

Jan 1, 1962

By A. L. Mincher, W. F. Sheely

Mechanical properties of columbium have been studied over the temperature range of -196 to 1093oC. The decreased strengthening influence of cold-work at temperatures below ambient has been interpreted in terms of the Peierls-Nabarro effect. Maxima in the rate of strain hardening observed during tensile testing in the range 250-600°C. have been correlated with interstitial impurities to indicate the temperature ranges at which carbon, oxygen, and nitrogen, respectively, are responsible for strain aging. THE growing need for structural materials for use above the useful service temperatures of the iron-, nickel-, or cobalt-base alloys has caused the refractory metals to be considered as potential engineering materials. These metals, which include columbium, tantalum, molybdenum, and tungsten, are called refractory because the lowest melting point among them,that of columbium, is about 1000°C higher than the average melting temperatures of conventional high-temperature alloys. They are all body-centered cubic transition metals and, as such, their mechanical properties have basic characteristics which distinguish them from the face-centered cubic metals. For example, all show a much steeper rise in strength with decreasing temperature below room temperature than do the face-centered cubic metals, and their mechanical properties are strongly influenced by interstitially dissolved impurities. In order that these new metals may be used efficiently, it is necessary that their characteristics of behavior be fully known. In this paper, the mechanical properties of columbium will be examined over a wide range of temperatures. In particular, the influences of cold-work and individual species of interstitial impurity atoms on mechanical properties will be described, and basic mechanisms which may control the observed characteristics will be explored. EXPERIMENTAL The material used in this investigation was Union Carbide Metals Co. columbium roundels consolidated to four 4-in. diam ingots, three by consumable-electrode arc melting and one ingot by electron beam melting. Impurity contents of the ingots and methods of ingot conversion and treatment are summarized in Table I. The only metallic impurity occurring in any significant quantity was tantalum at about 0.1 pct. Iron, silicon, titanium, and zirconium were each less than 0.015 pct; boron was 1 ppm or less. This should have no appreciable influence on properties. The electron beam melted material, being the purest, will be used as the basis for comparison in the discussions to follow. Tensile tests were conducted from-196 to 1093oC, on both cold-worked and fully recrystallized arc-melted and electron-beam melted columbium using standard 1/4-in. diam, 1-in. long gage length test specimens. A strain-rate of 0.005 in. per in. per min was employed until the 0.2 pct yield strength was achieved and then the strain-rate was increased to 0.05 in. per in. per min for the balance of the test. Samples were protected in an inert atmosphere at tests above 300°C. The tensile properties obtained on the electron-beam melted columbium, E, in both the cold-swaged and recrystallized conditions are given in Fig. 1. The yield strength data of Dyson, et al.,&apos; obtained on recrystallized electron beam melted columbium and the tensile strength data reported by Tottle2 on powder metallurgy columbium are included in Fig. 1. The material used by Tottle had been purified by vacuum sintering. There is excellent agreement between Dyson&apos;s data and those obtained in the present investigation. The tensile strengths obtained by Tottle were slightly greater than those obtained in this investigation on electron-beam melted columbium but varied with temperature in a similar manner. Tottle&apos;s data showed a maximum in tensile strength near 500°C, as did our data on electron-beam melted material, and also showed a small maximum at 300°C. The significance of these maxima will become evident later in the discussion. The tensile properties of cold-swaged and recrys-tallized arc melted columbium are plotted in Fig. 2. It was found that the properties of the recrystallized arc-melted columbium from all three heats showed very close agreement except at temperatures between about 500" and 800°C. A reason for this range of disagreement will be suggested in the discussion. The generally good agreement, however, attests to the ability of cold-working and subsequent recrystal-lization to erase the effects of the three different primary breakdown procedures and to produce nearly equivalent structures in the samples derived from the three different heats. wesse13 reported tensile data on columbium having interstitial impurity contents between those of the

Jan 1, 1962

By Rodney P. Smith

The rate of motion of the boundary between a single-phase a-iron region and a two phase a-iron plus ?-iron, or a-iron plus cementite region has been measured on decarburization at several temperatures between 500" and 865°C. These data, together with data for the carbon content of a-iron at the boundary, yield the diffusivity of carbon in a-iron. The activation energy for carbon diffusion is 19.8 kcal per mole for the temperature range —50° to 150°C and increases to an average value of 23.0 kcaL per mole for the temperature range 727" to 865°C. AS part of an investigation of the diffusivity of carbon in iron using a steady-state method,&apos; the diffusivity of carbon in a-iron was determined at the temperatures 802" and 851°C. The diffusion constant thus obtained was larger, by nearly a factor of two, than that predicted from the combined results of stanley2 and of Wert.3 It seemed desirable, therefore, to continue the investigation. Since the temperature range in which the steady-state method can be conveniently used is limited, we have chosen a decarburization method, based on the laws of diffusion in metal accompanied by a phase change.4,5 If the initial carbon content of the Fe-C alloy is such that two phases coexist at the decar-burizing temperature* and decarburization is car- ried out such that the surface is maintained at substantially zero wt pct. C, the carbon distribution after a time, t, will be as shown in Fig. 1. The boundary between the single-phase and two-phase regions moves from y = 0 to y = x in the time, t, where x is proportional4 to tl". If the initial carbon (content of the sample is Ci, and CB is

Jan 1, 1962