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By Dol Duwez, R. H. Willens

A technique is described by which metastable alloy phases can be obtained by very rapid cooling from the liquid state. The results obtained so far have lead to; 1) extension of solubility limits beyond their equilibrium values, 2) new phases not found under equilibrium conditions, and 3) amorphous alloys. MANY new nonequilibrium phases have been found in alloys rapidly cooled from the liquid state. The technique used in these investigations essentially consisted of propelling a small molten globule of an alloy against the inside surface of a rotating copper cylinder. Since these original experiments were performed, the technique has been greatly improved. The purpose of this paper is to describe in detail, for the first time, a simple and efficient apparatus for producing foils of alloys which are rapidly cooled from the melt and to summarize some of the observations made on these alloys. I) FAST COOLING APPARATUS In the original fast cooling apparatus used by Duwez, Willens, and Klement,' the alloy was melted in a graphite container having the shape shown schematically in Fig. 1. A shock tube was attached to one end of the graphite part to supply the pressure for ejecting the molten globule. The globule was received on the inside of a rotating cylinder located about 0.5 in. from the exit of the graphite container. The globule trajectory made an angle of about 15 to 25 deg with the tangent to the cylinder at the point of

Jan 1, 1963

By R. W. Guard, W. R. Hibbard

As part of a program to determine the deformation characteristics of pure metals, the tensile creep properties of high purity aluminum (99.994 pct Al) have been determined using a constant stress loading. The effects of prior annealing temperature, stress, and temperature were studied. These data have been examined on the basis of present-day theories. None of the methods was found to give an accurate representation of the data over all conditions studied. The structures of several specimens after creep were examined by optical and X-ray metallography. Marked changes in the grain size were found and it was substantiated that the magnitude of these changes was greatly influenced by the applied stress (or creep strain). The changes in fiber texture which occur on creep deformation are shown to be consistent with those observed on deformation at lower temperatures. UNDERSTANDING the properties of new mate-*-J rials under different experimental conditions must be based on considerable knowledge of the mechanisms involved in plastic flow and how to control them. Tension and creep tests have been carried out on a number of pure metals in order to document their deformation characteristics. It is hoped that a comparison of these data with theory will indicate those areas where work on mechanisms and their relation to metallurgical variables may be most fruitful. Since aluminum has often been used for studying the qualitative aspects of creep behavior, it was chosen for detailed study. The effects of annealing temperature, stress, and test temperature on the constant stress creep behavior were studied. Although most of the tests were made above one half the absolute melting temperature, a few tests were made at lower temperatures to give qualitative comparisons. Some specimens were examined metallo-graphically and by X-ray diffraction techniques after creep. Since only a limited number of specimens could be made from the available material, no effort was made to study detailed changes in sub-grain structure or other metallographic features. Servi and Grant3 nd Dushman et al.' have previously published studies of high temperature creep of high purity aluminum. In both cases, a great deal of emphasis was placed on the minimum creep rate.

Jan 1, 1957

By E. W. Enqelmann

DURING January, 1933, burlap or coco matting was placed in the bottom of launders handling various products of the flotation plant of the Magna mill of the Utah Copper Co., with the hope of increasing the total recovery of gold. This was soon followed by placing various materials, such as coco matting, cotton twill, and common 10-oz. burlap on the bottom of the main tailing launder. The burlap was found to be the most economical material to use. The test was first conducted in an old wooden launder, 40 in. wide and 2000 ft. long, with 10-oz. burlap fastened

Jan 1, 1935

By H. A. Hoffman

Competition from an all-flotation plant, with demonstrated economies and efficiencies, plus a change in smelting contract and introduction of improved cyclones lead to conversion from gravity-flotation. Detailed descriptions are given of equipment installed and procedures used at St. Joseph Lead's Federal mill. Future plans include further quality control by instrumentation in all aspects of the mill operation. Also planned are improvements in materials handling systems. Competitive conditions will continue to dictate improvements and changes in the mill flowsheet. The advent of all-flotation mills in the Lead Belt was introduced by the Indian Creek mill in late 1953. This modern and efficient plant then became a pattern for the other mills in this area to re-evaluate their circuits in an effort to develop flowsheets that would improve operating conditions and metallurgy. The Indian Creek mill demonstrated that all-flotation would require considerably less operating and maintenance labor than the combination of tabling and flotation that was common in the Lead Belt at that time. Two significant changes occurred in recent years to allow all-flotation to be seriously considered in other Lead Belt mills. One was a change in the smelting contract which did not require gravity concentrate. Another was the development of cyclones which provided classification of the flotation feed in a very small space. Since the Federal mill was the largest concentrating plant in the Lead Belt it was felt that the greatest savings could be made by investigating the all-flotation possibilities at this mill. Interest was stimulated by the milling and ore dressing Depts. to determine if this mill would be converted without undue cost, provided the metallurgy could be improved. Accordingly, laboratory tests were initiated to learn what metallurgical benefit could be derived. Numerous tests were run which indicated that grinding to all-flotation would improve the tailing by as much as 0.02 pct Pb. This was quite significant when multiplied by the tonnage of ore treated. Projecting the added cost of power for extra grinding and flotation, and the additional flotation reagents required, plus additional new equipment that would have to be purchased, it would still add up to a considerable saving. The all-flotation mill would reduce man power by some 30 pct, and make a metallurgical improvement. Operating costs could be reduced bv 2$ per ton. The metallurgical improvement would amount to 4$ per ton, for a total of 6$ per ton of ore milled. An estimate of the cost of the conversion was set at $250,000. With the savings as estimated this could be paid off in about two years. On paper it therefore seemed attractive enough to justify a mill test. MILL TESTING One section of the Federal mill was made available for use as a separate test circuit. Cyclones and density controllers were borrowed from the Viburnum and Indian Creek mills. Denver flotation cells were obtained from the Desloge mill that was then shut down. Two 10-cell groups of Fagergren flotation machines, consisting of eight roughers and two cleaners in each bank, were segregated from the remainder of the plant. The 9x12-ft rod mill was continued as a primary grinding mill. The two 6%x12-ft mills on this section were converted from rods to balls, and the speed increased to 22.0 rpm. Cyclones were installed to close the circuit of these ball mills. The ground pulp from each of the ball mills was fed separately to its own bank of flotation cells so that two completely separated test circuits could be run in parallel. This test circuit operated on a three-shift basis from Dec. 22, 1959 to Mar. 21, 1960. The first few weeks were occupied in developing conditions for proper metallurgy and trouble-free operations. Results were rather erratic but as the ore dressing laboratory and the mill operators became more familiar with conditions they were able to obtain expected results, which could be duplicated day after day. The last five weeks of testing indicated the best results and are tabulated in Table I. During the first two weeks a Denver unit cell was used on No. 1 flotation circuit. Even though it recovered almost one half of

Jan 1, 1962

By E. W. Filer, L. S. Darker

ONE of the primary purposes of this investigation was to determine how far blast-furnace metal and slag depart from equilibrium, particularly with respect to sulphur distribution. In studying the equilibrium between blast-furnace metal and slag, there are two approaches that can be used. One method is to use synthetic slags, as was done by Hatch and Chipman;' the other is to equilibrate the metal and slag from the blast furnace by remelting in the laboratory. In the set of experiments here reported, metal and slag tapped simultaneously from the same blast furnace were used for all the runs. The experiments were divided into two groups: 1—a time series at each of three different temperatures to determine the t.ime required for metal and slag to equilibrate in various respects under the experimental conditions of remelting, and 2—an addition series to determine the effect of additions to the slag on the equilibrium between the metal and slag. An atmosphere of carbon monoxide was used to simulate blastfurnace conditions. The furnace used for this investigation was a vertically mounted tubular Globar type with two concentric porcelain tubes inside the heating element. The control couple was located between the two porcelain tubes. The carbon monoxide atmosphere was introduced through a mercury seal at the bottom of the inner tube. On top, a glass head (with ground joint) provided access for samples and a long outlet tube prevented air from sucking back into the furnace. The charge used was iron 6 g, slag 5 g for the time series, or iron 9 g, slag 7 % g for the addition series. This slag-to-metal ratio of 0.83 approximates the average for blast-furnace practice, which commonly ranges from about 0.6 to 1.1. A crucible of AUC graphite containing the above charge was suspended by a molybdenum wire in the head and, after flush, was lowered to the center of the furnace as shown in Fig. 1. The cylindrical crucible was 2 in. long x % in. OD. The furnace was held within &3"C of the desired temperature for all the runs. The temperature was checked after the end of each run by flushing the inner tube with air and placing a platinum-platinum-10 pct rhodium thermocouple in the position previously occupied by the crucible; the temperature of the majority of the runs was much closer than the deviation specified above. The couple was checked against a standard couple which had been calibrated at the gold and palladium points, and against a Bureau of Standards couple. The carbon monoxide atmosphere was prepared by passing COz over granular graphite at about 1200°C. It was purified by bubbling through a 30 pct aqueous solution of potassium hydroxide and passing through ascarite and phosphorus pentoxide. The train and connections were all glass except for a few butt joints where rubber tubing was used for flexibility. The rate of gas flow was 25 to 40 cc per min. As atmospheric pressure prevailed in the furnace, the pressure of carbon monoxide was only slightly higher than the partial pressure thereof in the bosh and hearth zones of a blast furnace—by virtue of the elevated total pressure therein. Simultaneous samples of blast-furnace metal and slag were taken for these remelting experiments. The composition of each is given in the first line of Table I. There is considerable uncertainty as to the significant temperature in a blast furnace at which to compare experimental results. This uncertainty arises not only from lack of temperature measurements in the furnace, but also from lack of knowledge of the zone where the slag-metal reactions occur. (Do they occur principally at the slag-metal interface in the crucible, or as the metal is descending through the slag, or even higher as slag and metal are splashing over the coke?) The known temperatures are those of the metal at cast, which averages about 2600°F, and of the cast or flush slag, which is usually about 100°F hotter. To bridge this uncertainty, remelting temperatures were chosen as 1400°, 1500" (2732°F), and 1600°C. For the time series the duration of remelt was 1, 2, 4, 8, 17, or 66 hr; crucible and contents were quenched in brine. The addition series were quenched by rapidly transferring the crucible and contents from the furnace to a close-fitting copper "mold." Of incidental interest here is the fact that the slag wet the crucible

Jan 1, 1953

By W. A. Tiller

SEVERAL authors1-6 have shown that, during solidification from the melt, the direction of formation of substructure boundaries depends upon the direction of heat flow and the rate of solidification of the metal. The most prominent of these observations was that a preferred orientation developed during the solidification of the columnar zone of an ingot which for face-centered-cubic metals was the <100> direction. Previous explanations1-&apos; given to account for this preferred orientation and the other boundary phenomena are all based on the premise that the phenomena are characteristics of the pure element. However, recent experiments by Rosenberg and Tiller7 have demonstrated that the preferred orientation in pure lead is the <111> orientation, and that the heretofore observed <100> orientation is due to the effect of solute on the mode of solidification of the metal. Teghtsoonian and Chalmers,4 studying striation boundaries in tin, and Chalmers and Rutter,5 studying corrugation boundaries in tin, showed that these substructure boundaries were aligned parallel to the axis of heat flow for slow rates of growth, and that the alignment varied from this direction as a function of the rate of growth. to approach the den-drite direction at high rates. Chalmers,6 studying the direction of formation of a grain boundary separating two crystals of different orientation, showed that at slow growth rates the boundary is parallel to the axis of heat flow, while at higher speeds it will deviate from this direction, sloping into the crystal whose dendrite orientation departs the most from the axis of heat flow. It is this phenomenon that allows certain crystallites in the chill zone region of an ingot to encroach on their neighbors and ultimately produce the preferred orientation of the columnar zone of the ingot. Since the previous explanations of this preferred orientation are unable to account for the recent observations,&apos; a new mechanism will be considered. This will lead to an explanation of the other substructure boundary phenomena as well. Investigations by Graf,8 Billig,9 Rsenberg,10 and others have demonstrated in a striking fashion that crystal growth takes place by the deposition of individual layers oriented along the close-packed planes of the material considered. This lamellar or

Jan 1, 1958

By P. K. Foster, A. McNabb

A consideration of the literature shows the inadequacy of Fick&apos;s Laws to describe the diffusion of hydrogen in steels below 400°C. These laws are modified an the assumption that hydrogen is delayed at fixed sites in the lattice. Approximate and exact solutions of the resulting nonlinear system are derived for simple geometrical shapes. The results qualitatively account for the observed anomalous behavior. Experimental methods for verifying the theory are suggested. 1 HIS paper presents a new analysis of the diffusion behavior of hydrogen in steel based on a physical model which supposes that hydrogen atoms wander in a random manner through the crystal lattice, but tend to get trapped or delayed at certain fixed sites uniformly distributed throughout the metal. These sites, which will be called traps, are regarded merely as potential wells of significantly greater depth than those encountered in regular regions of the crystal lattices and no assumptions are made concerning their nature or origin. The results of experimental studies of the diffusion of hydrogen in iron and steel have usually been reported in the literature in terms of a diffusion constant D derived under the assumptions that the hydrogen concentration C is governed by Fick&apos;s laws.1 Fig. I is a composite of published graphs of the man. ner in which the values of D, so derived, vary with temperature. It is convenient to consider this material in two categories; the high temperature results above 400°C, and the results at lower temperatures. The graphs 2, 3, 4, 5 in the first class lie within a factor of three of each other and are relatively consistent compared with the low-temperature values. There is an increasing divergence in values of D with decreasing temperature till at room temperature they are spread over three orders of magnitude. Small values of D have been obtained for work-hardened specimens.&apos; It is evident that D is a function of other variables besides temperature in this range and that these neglected variables are in some way connected with the work hardening experienced by the specimen. In view of evidence for an interaction between hydrogen in solution and dislocations9&apos;10 and adsorption on crack surfaces,&apos; some doubts must be entertained about the validity of Fick&apos;s laws and their associated physical model of noninteracting particles in random motion through the medium. More direct evidence of their inapplicability to the diffusion of hydrogen in steel was first produced by Darken and smith." Consider the permeation of hydrogen through a plate of thickness a under a boundary concentration Co at the ingoing, and zero at the outgoing, face. If Fick&apos;s first law1 is valid, the steady state flux P, through unit area is DCo/a. In addition, the concentration C varies linearly throughout and Qo, the mean quantity of hydrogen in the medium, is co/2. Compare Qo with Q1 the mean quantity required to saturate the same specimen to a uniform concentration G. In this case Ql = Co and hence the ratio

Jan 1, 1963

By W. C. Winegard, C. Feng, C. Elbaum

SEVERAL investigations have been made concerning the effect of oxygen on the mechanical properties of titanium 1-6= In particular, the yield strength has received considerable attention. Finlay and snyder2 report a 0.2 pet strain offset yield strength if 49 kg per sq mm in titanium containing 0.1 pct 0 and 61 kg per sq mm in titanium with 0.2 Pct 0. These results are in good agreement with those of Jaffee, Odgen, and Maykuth3 who report values of yield strength

Jan 1, 1960

By Roger L. Brockenbrough

Steels available for mine-shaft applications are discussed, and the use of steel linings for round and rectangular shafts is reviewed. For rectangular shafts, frameworks constructed of square or rectangular steel tubes offer advantages. Also, corrugated steel sheeting provides a suitable alternative to timber lagging for spanning between the main shaft supports. For round shafts, self-supporting cylindrical steel liners, with circumferential stiffeners to prevent collapse, have been used to depths up to 6000 ft. Several large-diameter round shafts have been constructed with a concrete lining and an internal framework: of high-strength low-alloy steel tubes. It is concluded that in any new shaft construction steel designs should be investigated as economical alternatives to designs using other materials.

Jan 1, 1976

By H. C. Theuerer

GeC14 may be purified by extraction with HCI and chlorine. The process is as effective for the removal of AsCI:, as the more cumbersome distillation methods usually used for this purpose. GERMANIUM for semiconductor use contains impurities at levels no higher than a few parts in ten million. Material of this quality is obtained from highly purified GeC1, by hydrolysis to the oxide and reduction of the oxide in hydrogen. When purifying GeCl,, AsC1, is the most difficult impurity to remove. This is usually accomplished by multiple distillation procedures.1-3 AsC1, may also be removed from GeC1, by extraction with HC1.1-4 Reducing the arsenic to low concentrations is not practicable, however, because of the large number of extractions needed. This paper discusses a new method for the removal of arsenic from GeC1, by extraction with HC1 and chlorine. The method is rapid, leads to little loss of germanium and is at least as efficient as the distillation procedures currently being used. Theory of Extraction Procedures In the simple extraction of GeC1, with HC1, the following reaction occurs ASCl8G8C1 D AsCl3rc1 at equilibrium CA/Cn= K, where K is the distribution coefficient, and C, and C,, are the molar concentrations of AsC13 in HC1 and GeCl,, respectively. The materials balance equation for this reaction is VACA + vncn = VnC,, where V, and Vn are the volumes of HC1 and GeCl4, respectively, and C, is the initial concentration of AsC13 in GeC1,. From this it can be shown that for multiple extractions where C,, is the concentration of AsC13 in GeC14 after n extractions, and r is the ratio of V, to V,,. It is assumed that r is maintained constant, that equilibrium is established during each extraction, and that K is independent of the AsCl3 concentration. By saturating the system with chlorine, the following reaction occurs in the aqueous phase AsCl3 + 4H2O + Cl2 D H5AsO4 + 5HC1 at equilibrium K&apos; = ------------ ai - a4 h2u - aet2 where a is the activity of the various components. The effect of this reaction is to reduce the concentration of the AsC1, in the aqueous layer and, therefore, to promote further extraction of this component from the GeC1, layer. If the arsenic acid remains entirely in the aqueous phase, the net effect of this reaction is to promote the removal of arsenic from the GeC11. The materials balance equation for extraction with HC1 and chlorine with the foregoing reaction is, then, VaCC + VACA + VACn = VnCo where C,. is the molar concentration of H3AsO, in the HC1. With the added assumptions that the activities of AsC13 and H8ASO4 in the aqueous phase are equal to their molar concentrations, it can be shown that for n extractions Cn/Cu = (1/rkK + rK + 1) n where k - K1 a4h2o - acl2/aoncl. It can be seen by comparing Eqs. 1 and 2 that if k is large, the removal of AsC1, by HC1 extraction will be greatly improved by the addition of chlorine. Dilution of the HCI used in the extraction with chlorine would also favor the separation. This, however, would increase the loss of GeCl,, which is undesirable. Experimental Procedure Germanium prepared from oxide of semiconductor purity is n-type with resistivities greater than one ohm-cm. The resistivity is controlled by the donor concentration, which is —lo-: mol pct. Germanium prepared from material with added arsenic will have lower resistivity commensurate with the arsenic concentration. With such material, at arsenic concentrations above 10-1 mol pct the resistivity is controlled by the added arsenic, and effects due to other impurities initially in the oxide are negligible. In this investigation GeO, of semiconductor purity was converted to GeCl,, and -0.01 mol pct As was added. This material was used for the extraction experiments and the purification attained determined by a comparison of the resistivity data for samples of germanium prepared from the initial and purified GeC1,. A method for calculating the arsenic concentration from the resistivity data is discussed later. The details of the experimental procedures used are as follows: Two hundred and thirty cu cm GeC1, were prepared by the solution of GeO, in HC1, followed by

Jan 1, 1957

By Robert Franke

(Butte Meeting, August, 1915.) IN view of the prominence which the conical mill has attained in the fine-crushing field within the few years since its introduction, the following comparison with its more mature forerunner, the Chilean mill, based on extensive tests, is submitted in the interest of the milling profession. Soon after designing the concentrating plant of the Miami Copper Co. in 1909, the Hardinge conical mill made its appearance in the milling forum. Its possibility as a suitable crushing device for the plant was well recognized, but in view of the lack of commercial demonstration, at the time, as to capacity, efficiency for desired product, and the still more uncertain factors of cost of maintenance and power consumption, it was deemed that the immediate adoption of this machine throughout the plant would be a hazardous undertaking. For these reasons it was decided to equip the majority of the imme diately required units of the plant with Chilean mills, the fine-crushing proficiencies of which were better known, and one section with Hardinge mills, to serve as a test unit for the guidance of future installations and replacements. Thereby, after 1.5 years&apos; operation with both types of mills, a thorough test as to metallurgical efficiency and cost economy has been obtained. The conical mill used in these tests is the 8-ft. Hardinge pebble mill, having a cylinder 22 in. in length. The cylindrical portion of this mill is lined with cast-iron liner plates, and the conical extensions with silex bricks bound together by cement. Each liner plate carries a projecting lifter, the function of which is to increase the height of drop of the lifted material. Danish No. 5 pebbles, obtained from the coast deposits of Denmark, are used for the grinding charge. The Chilean mill used is a fast-running, 3-roller, 6-ft. Saturn mill, with screens of 0.037-in. opening. The feed to these mills is the oversize of Callow screens having 0.029-in. openings, which follow rolls crushing to 0.5 in.

Jan 7, 1913

By Louise B. Freeman

Kentucky for the first time in its oil history passed the 10 million barrel mark. Of the total 10,019,641 bbl., 8,262,516 bbl. were produced in Western Kentucky, and Union County surpassed all others, with 4,056,142 bbl., or 40 percent of all the production for the state. There were 930 wells known to have been drilled during the year; 510 in Western Kentucky and 221 in the gas-producing area of Eastern Kentucky.

Jan 1, 1946

By Ernest Gayford

This is a nontechnical paper on flotation, subdivided under three general headings: (I) Definition of flotation; (2) what flotation is now doing in Utah; and (3) what is the future of flotation? Definition T. A. Rickard defines flotation&apos; as "the act or state of floating," from the French flottaison, water-line and flotter, to float. The dictionary defines flotation as "the science of floating bodies." The flotation process is a method of concentrating ores by frothing. Weinig and Palmer,2 define flotation as follows: What is the flotation process? Briefly, it consists in the agitation of finely divided ore in water containing bubbles of air or gas, a small amount of oil and, usually, other reagents, soluble and insoluble; under these conditions the small particles of native metals, sulfides, arsenides, antimonides, selenides and tellurides show a tendency to attach themselves to the films of the bubbles, and are thus carried to the surface of the water. The oxidized gangue minerals, such as quartz, feldspar, limestone, hematite, etc., show much less affinity for the bubbles, are easily wetted by the water, and either remain in suspension in the water, or sink to the bottom of the vessel. If the bubbles are sufficiently stable they can be removed, carrying their load of sulfide-mineral particles with them. Thus there can be effected a separation of the two classes of minerals from each other, assuming that the grinding has been sufficient to unlock all of the particles of different composition. The separation does not depend upon differences in specific gravity of the various minerals; in fact, the sulfides are usually heavier than the oxides, and some of the heaviest sulfide minerals are the easiest to float. A particle of mineral may be so large, however, that its weight will counteract its affinity for the film of the bubble. In most cases the ore must be fine enough to pass a screen having at least 48 meshes to the linear inch. Taggart3 defines flotation as follows: Flotation is a method of wet concentration of ores in which separation of mineral from gangue is effected by causing the mineral to float at or above the surface of a body of liquid pulp while the gangue becomes or remains submerged. The method

Jan 1, 1928

By Eugene R. Rice

(Canal Zone Meeting, November, 1910.) THERE are many methods for determining the meridian, but all of those in common use involve at least two separate observations, one for latitude and one for azimuth. Such observations made upon a south star at any hour are open to the objection of possible inaccuracy due to ignorance of the absolute refraction, and also to slow change in the altitude of the star when near the meridian. The method of observing a circumpolar star at elongation, besides requiring a separate observation for latitude, is open to the serious objection that clouds may obscure the star at the critical moment. Moreover, a tedious wait for the star to come to elongation is sometimes necessary. Many of us can recall long, cold, weary vigils, waiting for Polaris to reach elongation. For observing a circumpolar star at any hour, not only the latitude, but also the true time, must be known. This it is practically impossible to obtain, except in regions reached by the telegraph, and usually then one has to know the longitude also, in order to reduce "standard time" to "local time." The results obtained by this method, when the star is at culmination, are not very good, unless the true local time is absolutely known. The methods of obtaining the meridian from the sun, by means of a solar attachment, or by direct observation, while good, are not absolute, by reason of refraction, change in declination of the sun, and small change in vertical angle, when the sun is near the meridian. For these two methods, latitude, time, and approximate longitude have to be known. In the method here described, only one observation is needed, and from it azimuth, latitude, and sidereal time are computed. In other words, one can observe a circumpolar star-Polaris

Nov 1, 1910

By D. C. McLean

This report summarizes the work that has been done during the past several years in adapting resins for use as auxiliaries in mine roof support. The resins were applied in two ways: 1) by injection into the strata, and 2) as a bonding agent for roof bolts and reinforcing bar. The Explosives and Mining Chemicals Department of the American Cyanamid Co. has worked during this period in cooperation with the Roof Control Research Group of the U.S. Bureau of Mines, the Pattin Manufacturing Co., the J. H. Fletcher Co., the Homestake Mining Co., the U.S. Steel Corp., the National Mines Corp. and the Pocahontas Land Corp. in an effort to create resin formulations and methods for applying them as a practical and sate type of roof support for mining areas particularly where conventional support is inadequate, yet expensive. This, work has involved much pioneering in a field where theory, speculation, and pure mythology predominates, and little basic engineering data is available. It is strange butt true that, despite the importance of roof control both from an operational and safely standpoint, there is scarcely a mining&apos; company in this country that has an engineer, or anyone, assigned to the study of roof support problem, except temporarily--after a bad roof fall. The responsibility for improving roof control methods seems to have been placed entirely upon the shoulder, of the USBM, various State departments of mines, and individual roof bolt manufacturing; companies. It was in cooperation with the USBM that Cyanamid first developed resins for mining use.

Jan 1, 1964

By J. Pinto, F. Galasso

THE current emphasis in preparing boron fibers by reduction of gaseous boron compounds on a resistively heated metal wire substrate has renewed interest in the borides of those metals which have relatively high melting points and are available as fine wires. A knowledge of the structures and properties of the borides, which are formed when boron diffuses into the metal core during boron deposition, can be of assistance in the understanding of the boron fiber formation process and the fiber properties. Many of these borides are well-known and their properties have been measured. However, when an unidentified boride is found in the core, it may be difficult to establish its composition because of the small amount of material available, the preferred orientation effects on the reflections in its X-ray pattern, and the possible overlap of X-ray reflections if several borides are present in the core. For example. the proper indexing of the X-ray pattern of WB4, which was formed in the tungsten substrate core during boron fiber formation, was accomplished only after small single crystals of this boride were grown and X-ray precession investigations were conducted.&apos; This note presents the results of a study of the phases formed in the core when tungsten, tantalum, and molybdenum metal wires were used as substrates in the boron fiber preparation process with particular emphasis on the identification and characterization of a higher boride of molybdenum analogous to WB,. Boron was deposited on resistively heated stationary 0.0012-in.-diam tantalum, tungsten, and molybdenum wires at 1050°C for various times up to 60 sec using boron trichloride and hydrogen as the reactant gases. After 60 sec of boron deposition the fibers were approximately 0.006 in. in diam. Examination of photomicrographs of fiber cross sections showed that the boron had diffused nearly to the center of the tungsten and molybdenum cores in 15 and 30 sec, respectively, and only halfway to the center of the tantalum core in 60 sec. X-ray diffraction photographs of the fibers indicated that it was also after 15 and 30 sec deposition times that the tungsten and molybdenum metal reflections, respectively, had disappeared from the X-ray patterns of the fibers. The patterns of the boron fibers produced using tantalum wire as a substrate showed that amorphous boron, TaB2, and tantalum metal were present after a few seconds deposition time and remained even after deposition times of 60 sec. Until a deposition time of 15 sec was reached, the tungsten substrate fibers contained amorphous boron,273 6WB, W2B5, and WB4 as well as tungsten metal, while the molybdenum substrate fibers contained amorphous boron, MoBa, Mo2B5, and molybdenum metal for deposition times up to 30 sec. Just before the molybdenum metal pattern disappeared, a pattern similar to that of WB, appeared, suggesting that a phase, MOB,, isomorphous with WB,, was present in the fiber. This same pattern was obtained from the product formed by heating a mixture of molybdenum metal and excess boron powder in a boron nitride crucible at 1960°C in an argon atmosphere. As was the case with the WBn pattern, this pattern could best be indexed on the basis of a hexagonal unit cell rather than the tetragonal unit cell Chrktien and Helgorsky reported for ~0~4,~ see Table I. The unit cell parameters for MoB4 were calculated to be a, = 5.214A, co = 6.358A. Assuming the space group P63/mmc and positions5 2M01 in 2b and 2MoII in 2c found for tungsten in WB~,&apos; a logical structure for MOB, was determined using geometrical considerations to place the boron

Jan 1, 1969

By P. W. Gilles, B. D. Pollock

THE pioneering work of Steinitz1 and Steinitz, Binder, and Moskowitz2 has shown conclusively the existence at high temperature of two additional phases in the molybdenum-boron system and thus brings to a total of six the number of structures appearing in this system. To the structures Mo2B, MOB, and Mo2B5 they have added MO3B2, a new -MOB form, and have shown that MOB,, which has the same range of composition as Mo2B5, is only a high temperature structure of the latter. This solid solution, interestingly enough, includes neither of the compositions corresponding to the stoichiomet-ric compounds, MOB, or Mo2B5, but rather at all temperatures has intermediate values of composition. These workers have also, in the course of their work, measured melting points, transition temperatures, eutectic and peritectic points in the system and have shown that Mo3B2, because of its dispro-portionation at low temperature to Mo2B and MOB, is stable only in a limited high temperature range. During the course of the present work on the vaporization properties of the molybdenum-boron compounds, a few transition temperatures were observed. When the report of the other workers appeared, it was decided to repeat, in part, their study of the system. As a result, considerable evidence has been obtained that substantiates the specific kinds of melting processes they report as well as the general features of their diagram. However, a marked difference was found between the temperatures they report and the ones observed in this study, with the latter being higher. The purposes of this paper are to present the evidence obtained in this laboratory that verifies their diagram of the system, to give some important temperatures in the system, to compare them with those previously published, and to seek an explanation of the difference. Samples The metal starting material was 400 mesh molybdenum powder with a purity stated by the manufacturer to be 99.9 pct. The initial treatment, designed to remove volatile contamination, consisted of heating in a vacuum for 10 min to a temperature of from 800" to 1000°C during which a loss of 0.3 to 0.4 pct occurred. An assay following this treatment showed it to be 99.4 pct pure, with the principal impurity probably being oxygen. The boron starting material was obtained from the Cooper Metallurgical Laboratories and the Fair-mount Chemical Co. as 325 mesh powder with manufacturers&apos; analyses of 99 pct or better. Initial treatment consisted of heating in molybdenum in a vacuum at about 1700°C for 10 min. During this time a loss of 3.5 pct occurred. An assay following this treatment showed the different samples to have purities ranging from 95.5 to 99.0 pct with iron and carbon as the principal impurities. Following the initial treatment, the elements were combined to form stocks of Mo2B and MOB by heating pressed mixtures in a vacuum to 1100" to 1200°C to accomplish reaction and to 1500" to 1900°C for a few minutes to evaporate the more volatile impurities. Analysis of the two compounds for boron by a modification of the method of Blumenthal3 and for molybdenum by the lead-molybdate method indicated them to have purities greater than 99 pct. The individual samples to be studied had compositions in the Mo2B-MOB range and consisted of mixtures of the stock compounds. Procedure As is usually the case in high temperature work the selection of containers for the samples posed some problems. For vapor pressure studies tantalum crucibles, allowing little contact with the pressed samples, were used and some of the observations made during these experiments are pertinent to the study of the phase diagram. Most of the experiments, however, were performed in graphite containers, as were those of the previous authors. Two kinds of spectroscopic grade graphite crucibles were used. One was a % in. cylinder, 3/4 in. high, containing seven 3/16 in. holes drilled 1/2 in. deep into which were packed samples of the different mixtures weighing 250 to 500 milligrams. The other, consisting of separate crucibles, was prepared by drilling 3/16 in. holes, 1/2 in. deep into 1/4 in. graphite rods % in. long. The 7/8 in. cylinder was heated directly by induction while the small crucibles were packed in a tantalum heating element for induction heating. All heating was done in a high vacuum system in which the pressure was generally less than 1x10-5mm and never rose above 2x10-5mm when the samples were hot. The general pattern of the heating in graphite was to heat rapidly to a temperature somewhat below the desired one, then to raise the temperature slowly. The samples were held for 2 to 5 min at the maximum temperature, which in all cases was far higher than that needed to produce reaction. The short time was employed to reduce possible contamination by the crucible material and to reduce composition changes that would occur because of vaporization. After examination following the heating, the samples were reheated to a higher temperature. Temperatures were measured with a Leeds and Northrup disappearing filament optical pyrometer, certified by the National Bureau of Standards, by sighting through a window at the top of the vacuum

Jan 1, 1954

By L. Delisle

This work represents the first step of an attempt to test the applicability of the electron microscope to the study of subgrain structures in copper. Observations on annealed and deformed single crystals and polycrystalline samples of copper are described. IN the course of study of the structure of fine tungsten wires and tungsten rods with the electron microscope, well defined subgrain structures were observed. The size, size distribution, and orientation uniformity of the etch figures varied widely in different samples. Figs. 1 and 2, electron micrographs of a tungsten wire and of a tungsten rod, respectively, are illustrations of the difference in size and size distribution of the etch figures in different samples of the same metal. The observed differences, as pointed out in a previous paper,&apos; appeared to be related to the heat and mechanical treatments of the samples. They were also consistent with the results reported in the literature on the mosaic structure of metals.&apos; For that reason a program of research was initiated in an effort to obtain more systematic evidence of the possible relation of heat and mechanical treatments to the subgrain structure of metals as observed in the electron microscope. The purpose of this paper is to present observations made on the effect of cold work on the subgrain structure of copper. Procedure Starting Materials: Copper was the metal studied because it can be obtained in a high degree of purity, much information is available in the literature on its properties and its response to cold work and heat treatment, it shows no allotropic change, and it is sufficiently hard to be handled without great difficulty. Two groups of specimens were used: 1—single crystals cast from spectroscopically pure copper and 2—polycrystalline samples of oxygen-free high conductivity copper. Single crystals were studied because it was hoped that the elimination of a number of variables, such as grain boundaries, orientation differences, degree of purity, would simplify the problem and perhaps permit a better understanding of the phenomena that would be observed. The polycrystalline samples were designed to give a general picture of the changes considered. The single crystals were made of copper which analyzed spectroscopically to better than 99.999 pct Cu. They were cast in vacuum, by the Bridgman method, in crucibles made of graphite with a maximum ash content of 0.06 pct. The mold design is shown in Fig. 3. It permitted casting crystals of the size and shape required for the experiments, so that the danger of introducing cold work in the original samples by cutting or other machining would be eliminated. The polycrystalline samples were pieces, 3/4 in. long, cut from a rod of oxygen-free high conductivity copper, % in. in diameter. A flat surface, 1/4 in. wide, was milled along the rods, polished, and etched. The samples were then annealed in vacuum at 850°C for 1 hr. Polishing and Etching: Work previously done on tungsten,&apos; polished mechanically and etched chemically," had shown that: 1—the general appearance of the etch figures of a given sample was not altered by repeated polishings and etchings under similar conditions; 2—variations in the time of etching and the concentration of the etchant changed the definition of the etch figures, but did not alter their general size nor orientation distribution within the limits of observation. Further work confirmed the reproducibility of the subgrain structures observed in, 1—single crystals and polycrystalline samples of copper when polishing and etching were repeated under similar conditions, and 2—specimens of tungsten and polycrystalline copper when electrolytic polishing and etching were substituted for mechanical polishing and chemical etching, respectively. On the strength of these observations, it was felt that, if conditions of polishing and etching were kept constant, changes observed in the subgrain structure of a sample upon deformation and annealing would be attributable to such treatments. For that reason the conditions of polishing and etching were kept as constant as possible. The single crystals were polished electrolytically in a bath of orthophosphoric acid in water, in the ratio of 1000 g of acid of density 1.75 g per cc to 1000 cc of solution, under a potential drop of 1.6 to 1.8 V. Electrolytic polishing was selected to prevent the formation of distorted metal in polishing. The same samples were etched by immersion in a 10 pct aque-

Jan 1, 1954

By W. A. Thomas

Steam is, and doubtless always will be, the basic power in the anthracite industry, either directly applied through engines and pumps or electrically. The rapidity with which electric power is being applied to the mining and preparation of anthracite leaves little doubt as to its utility and economy. There is practically no operation, except possibly the drilling of hard rock, that has not been successfully electrified and the matter of drilling is handled economically with electrically driven compressors and the standard compressed-air drills. Conservation and the seemingly ever-increasing cost of production, justify careful consideration of the possible results of the more extensive use of electric power in the industry. It is not planned to discuss, herein, the relative economies of individual applications but to consider the relative economy and flexibility of steam and electric power. The reports available for the year 1920 indicate a production of slightly over 80,000,000 tons of anthracite, of which 8,843,500 tons were used for power and heating purposes; in other words, over 11 per cent. of the production was used at the mines. Some of this was used to generate electric power at the mines, about 160,000,000 kw-hr., while 150,000,000 kw.-hr. was purchased from the public utility companies. One large producer, who is buying some electric power and generating some, used over 13 per cent. of the production for power and heating at the mines. Another producer, where considerable electric power is generated on the properties, is using less than 9 per cent. of the output for power and heating. One of the largest producers has a fuel consumption of over 15 per cent. of the output, besides which considerable power is purchased. A careful study of the field indicates that steam-operated plants use upwards of 13 per cent. of the production for power and heating, while electrically operated plants use about 1 per cent. for heating; so that, for steam-power purposes at least 12 per cent., or 268.8 Ib., are used for power out of each ton produced. In the complete electrification of anthracite mining operations, no set rule can be given for the power requirement, in kilowatt-hours per ton, as conditions vary widely in the matter of pumping, ventilation, and transportation, but the following cases are given as a basis of determining a range and a possible average power requirements:

Jan 1, 1922

By W. A. Foster

NINETY years after the Riddle nickel deposit N was discovered in Oregon in 1864, Hanna Coal & Ore Corp. began mining operations. Until 1954 much prospecting and preliminary development work had been done on the property, but no ore had been shipped other than for metallurgical testing. The deposit is being explored by churn drilling and trenching, and a few test shafts have been put down for the purpose of studying the ore in place, determining volume and moisture factors, and gathering bulk samples for pilot plant and smelter tests. In churn drilling, 6-in. casing is driven down 2 or 3 ft behind the drill bit and bottomed at each 5-ft interval. All the sludge for each cased 5-ft interval is dumped through a splitter and one eighth is saved and analyzed. Drillholes are stopped after going through the ore zone and penetrating fresh peridotite in which the nickel content is less than 0.5 pct.

Jan 8, 1957