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By B. J. Shaw, R. Kossowsky, W. C. Johnston

High purity (99,95) Ni-51 wt pct cr eutectic alloy was unidirectionalty solidified at rates of 0.1 to 8 in. per hr. The resulting material was characterized by large grains, approximately 0.5 mm in cross section and extending through almost the entire length of the specimen, parallel to the growth axis. The eutectic structure of specimens the growth at -1/3 The per hr consisted of a continuous nickel-rich phase and chrome -rich lamellae approximately 2 thick, spaced about apart. Specimens were tested in compression at temperatures ranging from —196 to 850"C over which range the 0.2 pet yield strength dp -creased from 160,000 p si to 35,000psi, respectively. Swaging to 40 pet reduction in area, followed by a 30-min anneal at 1000c to remove residual cold work, increased the 0.2 pet yield to 260,000 psi at -196°C, dropping to 35,000 psi at 850°C. The increase in strength was attributed to a residual cell structure. The strength of the alloy could be rationalized by the simple rule of mixtures if one assumed that additional strength is derived front a size effect characterized by is petch equation IN recent years there has been increasing interest in dispersion and second phase strengthening in materials needed for high-temperature applications. inm role of structure on the mechanical The of such alloys has been well established of such some extent accounted for theoretically. and to of how the strengthening mechanisms due to fibers and lamellae operate has been reduced to its fibers form by the fabrication of composites of strong rods unidirectionally aligned in a From work on tungsten-fiber-reinforced copper, for example, it was established that the "Rule of Mixtures" could explain the strengthening.12 " some what more sophisticated technique for introducing strong fibers into copper matrix was used by Hertzberg strong Kraft3 who unidirectionally solidified the copper-chromium eutectic. The use of unidirectionally fied eutectics has advantages in that there are no matrix-fiber wetting problems and fine fibers are automatically aligned and uniformly fiber However, one Is restricted to a specific volume fraction of the second phase. Nevertheless, even though the volume fraction is fixed, the rod or lamella thickness, , can be varied by controlling the freezing interface velocity. Alternatively, the grown material may be worked down by swaging or rolling. Embury and Fisher, " using this approach, drew down pear lite in iron and studied the mechanical properties iron and that the yield strength, oy, was properties.proportional They that d was the wire diameter. It could be inferred that was also proportional to but the work hardening had to be taken into consideration at the same time. By varying the growth rate of the cadmium-zinc lamellar eutectic, Shaw'1 showed that was proportional to without the introduction of work hardening and suggested that the lamellar interface itself contributed to the strengthening of the composite. In this investigation we have evaluated the mechanical properties of the unidirectionally solidified fec-bec eutectic Ni-Cr. This eutectic was selected because it presented the possibility was selected beca temperature, and high corrosion resistant alloy, and also represented a hard-soft phase combination with two completely different slip systems. Specimens were tested in compression and tension up to 850°C and a detailed study of the micro structure as a function of plastic strain and temperature was carried out by light and electron microscopy. It was shown that the composite strength tested in compression can be accounted for by the simple rule of mixtures if one allows for an additional term representing the effect of Intereprese EXPERIMENTAL PROCEDURE 1) Unidirectional Solidification. Fig. 1 is a schematic drawing of the apparatus used to produce 0.2 in. diam by 12 in. long alloy ingots. The crucible tube is alumina, containing the charge which has been is swaged, or machined to 0.195 in. diam. The lower end of the tube is immersed to 0 .195in in.d iam. The upper end is supported by a 10 mil nichrome wire which lowers the crucible mil nic hr the] wire at a prescribed rate. Surrounding the furnace is a graphite susceptor into which a control thermocouple is inserted. The furnace is insulated with fiberfrax and enclosed in a quartz tube. There is a sliding seal at the bottom around the crucible and one on the top so that an atmosphere may be used for the sample and suscep tor. The power for the furnace is supplied from a 10-kw, 450 kc generator. The skin depth (the skin depth at which the field falls to l/e of its value at the outer surface) for graphite (p = 10 (j-ohm-cm) is 0.1 in. at this fre-

Jan 1, 1970

ALTHOUGH the refining period of the heat is generally defined as starting after the charge has been completely melted, it may more properly be considered as beginning with the first efforts to facilitate the shaping up of the slag and the making of corrective additions for the control of slag or metal composition. Such actions may be initiated during the latter half of the lime boil. The early part of the refining period may, then, in essence overlap the latter part of the melting period. The primary aims of the refining period are: (1) to reduce phosphorus and sulfur from the steel bath to levels safely below the maximum contents specified; (2) to eliminate carbon to a specified level as rapidly as possible and still allow time for proper conditioning of the slag and attainment of the necessary bath temperature; and (3) to have the heat ready for tapping or furnace deoxidation, with slag in the proper physical and chemical condition, and with carbon and oxygen contents and the temperature of the steel at the proper levels for the composition and grade of steel being produced. The particular conditions that fulfill these aims are distinctly different, depending upon whether the steel is to be finished according to fully killed. semikilled, or rimming practice and also depending upon the carbon range specified. Regardless of the type of charging practice employed, the object of the refining period is to produce repeatedly the desired finishing and tapping conditions for the grade of steel being produced. The variations and proportions of raw materials used in the charge may cause some variations in the degree of control required during refining, but not in the method of control. The refining period can therefore be discussed from a viewpoint largely independent of charging and melting practice. SHAPING UP THE SLAG In the first helper's vocabulary, refining practice consists in

Jan 1, 1951

By ROBERT B. COONS

SELECTIVE SERVICE must meet three important demands for man power: (1) Activities concerned with production of war goods. (2) The armed forces. (3) Civilian activities and institutions the continuance of which are essential to maintaining the structure of our American democracy. In the above enumeration of demands I have placed everything, including most of our most prized possessions and activities, after the demand for men for war production and the armed forces. To establish an order between the latter two is difficult. For the time being, at least, the Selective Service policy is to make sure that we avoid the risk of "too little and too late." No soldier, sailor, or marine should be sent from these shores to risk his life without the assurance of having a gun, clothes, food, and medical supplies. Therefore, the premium is now being placed on man power for war production and in our process of selection no stone is left unturned to see that our agencies are fully informed of the needs of war production. Our procedures set up recourses for employers of war-production man power so that their activities need not be disrupted, at least not until they have had time to train replacements.

Jan 1, 1942

By Howard Willey

Mining operations of the Charcas unit at present are limited to the Tiro General mine at Charcas, in the State of san Luis Potosi, Mexico. The Tiro General mine was first operated during the Spanish occupation of Mexico for rich silver ores in an oxidized zone along the outcrop of the principal vein. In depth the ore is a complex sulfide with widely varying proportions of sphalerite, argentiferous galena and chalcopyrite ; and until recent years, it was economically impossible to carry on mining otherwise than irregularly in sections of the veins richest in galena and chalcopyrite. The advent of selective flotation brought the orebody as a whole within the field of economic interest, and a flotation mill of 650 metric tons daily capacity was constructed in the year 1925. The mining of partly worked-out sections of the mine, as well as the very heavy ground in most of the stopes opened in virgin ore, presented an unusually difficult problem. This paper describes the so-called "filled top slice" stoping method finally adopted as the standard system. Physical and Geological Conditions The principal orebody of the mine is an oreshoot about 1400 ft ng in a fissure vein striking about east and west and with an average lip of 70" to the north. The footwall of the orebody is fairly cleancu and regular both longitudinally and vertically and generally shows a dell-marked post-mineral slip. The footwall rock varies from a fairly strong limestone to a broken, metamorphosed limestone which requires heavy timbering. In some sections it is an altered, crumbly porphyry, which swells badly and necessitates frequent renewal of drift and raise tirnber. The hanging wall is irregular and frequently an assay wall. The stopina width ranges from a few feet up to more than 90 ft.; it averages about 30 ft. For the most part the hanging-wall rock is a shattered and altered monzonite porphyry, nearly aways requiring heavy timbering. The orebody is greatly fractured by post-mineral movement, which usually followed the footwall and left it as a smooth surface frequently covered with a slippery clay gouge. Two well marked transverse faults

Jan 1, 1931

By H. C. Schultz, F. K. Middleton Hunter

Certain local conditions were known to govern in large measure the successful adaptation of liquid-oxygen explosives to the large-scale blasting at Chuquicamata. The wide variation in hardness of the rock at this mine makes necessary the use of several types of explosives. A locally manufactured, relatively cheap black powder is used in blasting the softer waste and capping material, where a thorough displacement breaks the ground sufficiently. Before the introduction of L. 0. X., an ammonia dynamite of about 65 per cent. strength was being used exclusively in the harder underlying orebody, where a strong disruptive as well as a displacement effect is required for breaking the ore. The L. 0. X., as developed for quarry work in the United States, has a practically pure carbon cartridge material, and the explosive has an extremely high rate of detonation, which should therefore cause it to develop usefully its full disruptive effect in hard ground. The individual blasts at Chuquicamata arc large, black-powder shots which dislodge masses of rock averaging 250,000 tons each, and dynamite shots which dislodge masses averaging 80,000 tons each. It was desirable, therefore, to attempt to displace with L. 0. X. the faster, higher-cost ammonia dynamite used in the smaller blasts. It was not considered practical to attempt to displace the low-cost black powder with 1,. 0. X., as estimated costs showed no probable saving if this were accomplished. Since it was desirable to continue shooting relatively large blasts for effective operation, it was recognized that larger storage facilities than had been in use would be needed for the liquid oxygen. Because of the difficulty of transporting and discharging large storage containers of efficient design, the better plan appeared to be storage and discharge of the liquid at the place of manufacture, and transportation of the filled soaking boxes to the blast. Present Liquid-oxygen Plant An experimental unit with a rated capacity of 75 liters per hour was erected during the latter part of the year 1926 to prove the effectiveness of L. 0. X. at this mine, its cost, and possible efficiency of large-scale storage of the liquid. With this experimental unit 200,000 tons of ore

Jan 1, 1928

By Donald B. Evans, Robert D. Pehlke

The solubility of nitrogen in liquid Fe-A1 alloys has been measured up to the solubility limit for formation of aluminum nitride using the Sieverts method. The activity coefficient of nitrogen decreases slightly with increasing aluminum content in the range of 0 to 4 wt pct Al. Based on a nitride composition, AlN, the standard free energy of formation of aluminum nitride from fhe elements dissolved in liquid iron has been determined to be: ?F" = -59,250 + 25.55 T in the range from 1600º to 1750ºC. The solubility of nitrogen in liquid iron alloys and the interaction of nitrogen with dissolved alloying elements in liquid iron have been the subject of a number of research investigations.' Most of this work, however, has been reported for concentrations well below those necessary for the formation of the alloy nitride phase. Data in the concentration region near the solubility limit of the alloy nitride, particularly for systems exhibiting stable nitrides, are important in evaluating the denitrifying power of various alloying elements. They are also useful in determining the stability of a given nitride if it is to be used as a refractory to contain liquid iron alloys. In view of the importance of aluminum as a deoxidizing agent in commercial steelmaking and the fact that its nitride, AIN, is a highly stable compound and has merited some consideration as an industrial refractory, the following investigation was undertaken. The use of the Sieverts technique provided a measurement of the equilibrium nitrogen solubility in liquid Fe-A1 alloys as a function of nitrogen gas pressure up to 3.85 wt pct A1 in the temperature range of 1600º to 1750°C. The values obtained by the Sieverts method were checked by means of a quenching method in which liquid iron was equilibrated with an A1N crucible under a known partial pressure of nitrogen gas, and the solubility of A1N in liquid iron determined by chemical analysis. EXPERIMENTAL PROCEDURE The theoretical considerations involved in determining the solubility product of a solid alloy nitride phase in liquid iron by measuring the point of departure of the nitrogen gas solubility from Sieverts law have been discussed by Rao and par lee.' The principal problem is to determine the variation of nitrogen solubility in an alloy as a function of the pressure of nitrogen gas over it with sufficient precision to establish the break point in the curve at the solubility limit of the alloy nitride phase. A fairly large number of data points are required to do this. A second problem is the determination of the composition of the precipitated solid nitride phase. This is necessary in order to define completely the thermodynamic relationships. The Sieverts apparatus used to make the nitrogen solubility measurements in this investigation is of essentially the same design as that described by Pehlke and E1liott.l The charge materials were Ferrovac-E high purity iron supplied by Crucible Steel Co. and 99.99+ pct pure aluminum. Recrystal-lized alumina crucibles were used, and were not attacked by the liquid alloys. The hot volume of the system which was measured for each melt ranged from 46 to 50 standard cu cm and was found to decrease linearly with decreasing pressure and with increasing temperature. The temperature coefficient of the hot volume at 1 atm pressure of argon gas was essentially constant for all experiments at a value of -6 X 10-3 cu cm per "C. The melt temperature was measured with a Leeds and Northrup disappearing filament type optical pyrometer sighted vertically downward on the center of the melt surface. The temperature scale was calibrated against the observed melting point of pure iron taken as 1536°C. The emissivity of all melts was assumed to be that of pure iron, taken as 0.43. The charge weights ranged from 110 to 140 g and the range of aluminum contents covered was from 0 to 3.85 wt pct. Aluminum additions were made as 12 to 15 wt pct A1-Fe master alloys previously prepared in the system under purified argon. The compositions of the master alloys were checked by chemical analysis and found to be in agreement with the charge analyses. Vertical cross sections of the master-alloy ingots were used as charge material for the equilibrations in order to minimize the effect of any segregation which might have occurred during solidification of the master alloys. Determinations of the solubility product of

Jan 1, 1964

By A. H. Rhoades, D. T. King, R. J. Gray

Tests and methods of detecting oxidized coal are studied. Particular emphasis is placed on the microscopically discernible changes that accompany the chemical and physical changes affecting the technological properties of coal during oxidation. Coal samples were used from the low-volatile Pocahontas No. 3 Seam, McDowell County, W.V., and from the high-volatile Cedar Grove Seam, Mingo County, W.V. Tests conducted include: carbonization, free-swelling index, phase inversion, froth flotation, Gieseler plasticity, oxygen by difference and by neutron activation, volatile matter, pH of coal slurries, alkali solubility, and electrostatic charge.

Jan 1, 1977

By J. A. Norden

MUCH has been written concerning the hoisting equipment of various mines -throughout the country, but most of the literature on the subject, if not all, describes equipment of extraordinary capacity and the small and medium-sized outfits have been neglected. The hoisting equipment here described is capable 'of handling about 1200 tons per day. It has not been worked, to capacity, but 600 to 700 tons, together with men and materials, have been handled in two shifts without any great effort. Only one shaft extends from the surface to the lowest levels of the mine; see Fig. 1. It is composed of three compartments, two of which are used for hoisting and the third for water, air, and electrical lines, and for sinking purposes. In 1909, this shaft was raised from the 1000-ft. (304-m.) level to the 700-ft. There a station was cut and an air hoist installed. At this time all mining operations were confined to the upper levels of the mine; that is; above the 700-ft. The. ore was-dropped to this level through chutes from the 300-, 400-, 500-, and 600-ft. levels and then lowered in cars on cages to the 1000-ft., which is the main haulage adit, the mill and railroad bins being about 3000 ft. from the shaft. Orebodies were, in due time, developed on the 1000-ft. level and below. Therefore, in 1913, the shaft was sunk to the 1150-ft. level and thereafter sinking was continued at regular intervals until the 1500-ft. level was reached. But, hoisting from the 1300-ft. level was a difficult, and slow process with the antiquated air hoist, so, in 1916, it was derided to raise the shaft to the surface and install a modern, electrically operated hoist. This was completed early in 1917 and the hoist was in operation in March of that year.

Jan 8, 1920

By H. E. Cook

The Ising model for the internal energy of a binary alloy has been used to obtain a general equation for the critical resolved shear stress of partially ordered crystals. The equation expresses the stress in terms of the Warren "alphas " and can be used to estimate the variation in strength with order without the assumption, present in the original formulation of this problem in terms of domain size, that order is complete within each domain and that the domains are of ungorm size and shape. In addition, it is the general equation, according to the Ising model, for strengthening by short-range order. Two applications of the equation are considered: One is an estimate of the variation in strength of CkAu with long-range order. The other is an estimate of the variation in strength of FeCo with quench temperature. Reasonable agreement is found with the variations reported in the literature. When the internal energy of an alloy crystal depends upon the distribution of solute, the strength of the crystal will also depend upon it because a portion of the applied stress for plastic deformation will be: where V is the volume of the crystal and E(E) is the energy change associated with the solute redistribution caused by the plastic strain, E. We expect T to equal zero for a crystal having a random arrangement of solute because the arrangement would remain random after plastic deformation. Likewise, we expect it to equal zero when the crystal is perfectly ordered because the motion of paired dislocations found in such crystals does not disrupt order. However, when short-range order exists or when long-range order is incomplete, plastic deformation will decrease the amount of order and additional work, proportional to the ordering energy, will be expended. Fisher' estimated T for crystals having short-range order by assuming an interaction energy between neighboring atoms and estimating the change in the number of unlike neighbors as a dislocation moved through the crystal. (His analysis was limited and several workers2"6 have since given more complete ones.) Fisher minimized the importance of a strengthening mechanism of this type for paired dislocations in a structure having long-range order. ~ottrell,' however, pointed out that T could be appreciable for ordered crystals having antiphase domains. He attributed the strengthening to the increase in surface energy of the domains as they were cut by paired dislocations. Ardley,' in his test of Cottrell's theory, found that r for Cu3Au crystals obeyed the equation: for 1 > t where 1 is the domain size, t is the domain wall thickness, and y is the surface energy of an antiphase boundary. His experiments represent the classic confirmation of the strengthening mechanism proposed by Cottrell. However, the assumptions involved in using Cottrell's theory are valid only for large domain size in CU~AU,~"~ i.e., when Eq. [2] reduces to: For small domains, ~linn~ has questioned Ardley's assumption that order was complete, and, indeed, Stoloff and ~avies" fpnd it incomplete until a size of approximately lOOA was reached. Even when the order within a domain is complete, it is not obvious how one determines the appropriate value for I in a structure where domains vary in size and are irregularly shaped. The purpose of this paper is to estimate T without restrictions upon the degree of order and domain shape. Our major assumption will be the use of a generalization of the model proposed by Bethe" (the Ising model) for the internal energy. This will in fact allow us to combine the theories for strengthening by short-range order and by antiphase domains into a single, general formalism. We will use the results to estimate the variation in strength of Cu3Au crystals with long-range order8 and the variation in flow stress of FeCo crystals with quench temperature.12'13 INTERNAL ENERGY For simplicity, we restrict our considerations to those binary solid solutions which can be described as an arrangement of atoms on a Bravais lattice. An atom site will be indexed by three numbers (PI, pz, p3) determined by the vector: from the origin fixed at atom (0, 0, 0) to the atom site where a', an, and a, are the lattice translation vectors. We write: For the energy of the crystal where pi(p) is the probability (either zero or one) of finding an atom of type i (i = 1, 2) at site (p), which is shorthand for (pl, pz, p3) and pj(p + r) is that for an atom of type j (j = 1, 2) at the site (p + r), which is shorthand for (pl + rl, The coupling parameter, resents the energy associated with the pair Pi(p), Pj(p + r). The crystal is assumed large enough so that surface effects can be neglected; therefore, trans-lational and inversion symmetry require the coupling parameters to obey the relations

Jan 1, 1969

By J. H. Smith, H. W. Paxton

ALTHOUGH many structural and kinetic investigations have been made for alloys of iron and nickel, only meager data exist from thermodynamic investigations. The purpose of this note is to estimate the free energy of the Fe-Ni solid solutions from thermodynamic data available for ternary alloys containing iron and nickel. The lack of a description of the thermodynamic behavior for the Fe-Ni system has required the structural and kinetic analyses of the system to assume some form of solution behavior, usually regular, e.g., the mar-tensite transformation analysis of Kaufman and Cohen, 1 consistent with the limited thermodynamic data. Indications that this system could exhibit ideal solution departures might have been suggested by the large deviations from additivity rules observed in the density and lattice-parameter measurements of Jette and Foote2 who interpreted this in terms of possible solute-solvent interactions. Later Turkdogan et al. 3 and more recently Ward and wright 4 found a minimum in the graphite solubility in liquid Fe-Ni solutions near the concentration of FeNi3 with deviations from linearity persisting at all concentrations. This was interpreted by Ward and wright4 to indicate negative heats of solution and was suggestive of short-range ordering. The infinitely dilute activity coefficient of carbon (?oC) was also observed by smith5 to pass through a maximum near the FeNi3 concentration in Fe-Ni solid solutions. Recent investigations of the liquid solutions over the entire concentration range by Zellars et a1.' and Speiser et a1.," using vapor-pressure determinations, revealed both negative departures from Raoult's law and a nonregular solution behavior. The solid alloys have been studied by Oriani 8 and Kubaschew-ski and von Goldbeck6 employing gaseous H2/H2O equilibria with Fe and FeO. Both investigations were in substantial agreement, indicating very small departures from ideality. However, Oriani observed the formation of Fe3O4 (instead of FeO) at XFe= 0.441 which severed the equilibrium and precluded experimental investigation of the nickel-rich alloys. Heat-capacity and heat-content measurements have been evaluated by Montgomery10 and found generally unsatisfactory for gleaning thermodynamic information. This is due to the unknown final states of the alloys caused by the interference of the martensite transformation on cooling iron-rich concentrations and superlattice formation, magnetic transformation, and the varied heat treatments used by investigators of nickel-rich concentrations. As an alternative to the experimental difficulties, indirect estimates of the solid-solution behavior have been made by Fleischer and Elliott11 and Smith et a1.12 From their measurements of the solubility of Fe-Ni alloys in liquid lead, Fleischer and Elliott calculated the nickel activity (aNi) (and integrated for aFe) by assuming: 1) liquid lead has no solubility in solid Fe-Ni alloys, 2) Henry's law is obeyed throughout the liquid lead-rich phase (0— 12 at. pct Nil, and 3) Henry's law constant is independent of relative iron and nickel concentrations. The estimate of Smith et a1.12 was obtained

Jan 1, 1964

By Werner Engelmaier

Constant-strain rotating-bending fatigue tests were conducted on 2024-T3 aluminum alloy constant-strain McAdams-type specimens in ultrahigh vacuum, 10-lo Torr, and in atmospheric air. In the elastic strain range the ratio of vacuum-to-air fatigue life varied from about 10 at a maximum bending stress of 37 ksi to near unity at the endurance limit. After 10 pct of the fatigue life, intergvanular microcracks appeared on the surface which did not appreciably propagate further until the last 5 pct of the fatigue life, where trans-granular cracks propagating first in slip-plane cracking and then in the stress-dominated mode led to failure. No reduction in residual tensile strength resulted from the fatigue of the specimens short of fracture. The mechanism governing the fatigue life operates between the occurrence of the intergranular microcracks and the initiation of the trans granular cracks. MORE than forty years ago, Mc Adam' and Haigh2 published the first systematic studies showing that the fatigue properties of metals were greatly affected by environments. Gough and sopwith3 found in a later study that the fatigue life of metals subject to corrosion can be substantially increased by reducing the atmospheric pressure. This and their later work4'5 was, however, done in a vacuum of only 10~3 Torr. Subsequent studies6-' at a vacuum of 10- Torr showed that water vapor is the primary agent affecting the fatigue properties of aluminum alloys. Only recently was ultrahigh vacuum used for fatigue studied.l Various theories have been put forward to explain this phenomenon. Wadsworth and Hutchings12 postulated that cracks form very early in the test and that the chemical attack by the corrosive components of the atmosphere at the root of the cracks enhances the speed of the crack propagation. They also noted that chemisorbed layers of gas on the fresh crack surfaces prevent cold welding of the crack and make the separation irreversible. Ham and Reichenbach, on the other hand, reported that their specimens showed no cracks after a run in vacuum, even though the runs were long enough to have caused the specimen to fracture in atmospheric air. They also reported that in argon at 0.14 Torr the fatigue life was about 5 times longer than at 7 X lo-' Torr. Jacisinll reported that fatigue tests in dry nitrogen showed results close to those obtained in ultrahigh vacuum. The present experiment was designed to determine the extent to which cumulative fatigue damage, i.e., the accumulation of length of fatigue cracks, reduces the residual static tensile strength of an aluminum alloy in both ultrahigh vacuum and atmospheric air and to obtain fatigue-life data for this aluminum alloy at various strains. It was also hoped that information ex- tracted from these data might support one of the previously mentioned theories. 1) EXPERIMENT Test Specimens. The material tested was commer-cial 2024-T3 aluminum alloy. In addition to aluminum, this alloy contains approximately 4.4 pct Cu, 0.5 pct Fe, 0.5 pct Si, 0.6 pct Mn, 1.5 pct Mg, plus smaller amounts of other elements.13 Some typical mechanical properties of this aluminum alloy are listed in Table I.'~ The material was used in the as-received condition, i.e., solution-treated and cold-worked. Mc Adam-type1' constant-stress specimens and notched fatigue specimens were machined from 4 -in. -diam rods, Fig. 1. The critical section of the McAdam-type samples was polished with a 45-deg spiral motion to a No. 8 microfinish. The notch in the notched specimens was machined on a lathe with a forming

Jan 1, 1969

By W. W. Stephens, W. J. Kroll, H. P. Holmes

THE only two methods for producing commercial quantities of malleable zirconium, up to now, have been using magnesium reduction of the anhydrous chloride under a neutral gas, and using purification of raw zirconium by the iodide dissociation method on a hot filament. The purity of the metal obtained by the latter process is about the same as that resulting from the chloride reduction, with the exception of the oxygen content, which may be about 0.05 pct lower in the iodide metal. Even traces of oxygen have a strong hardening effect on zirconium. Since, in the iodide process, the impurities, Si, Al, Fe, Ni, and Mg in the raw zirconium used, are carried over, it would appear uneconomical to use this method of refining solely to eliminate the traces of oxygen, unless very soft metal is desired. One important step to improve the iodide method, namely, dissociating pure iodide made from carbide and recycling the iodine, which would change this refining process into a method for extracting zirconium from the ore, has not yet been made. The Bureau of Mines, by using the chloride reduction, wanted to produce quantities of a reasonably pure and malleable metal at low cost for large-scale industrial use. This aim has been achieved, and a pilot plant permitting production of 600 lb of malleable zirconium per week will be described (fig. 1). Briefly, the Bureau of Mines process consists of reducing purified gaseous anhydrous zirconium chloride with fused magnesium under a noble-gas atmosphere. The reaction product, magnesium chloride, and any excess magnesium metal present are removed from the sponge zirconium in the next step by fusion and evaporation in a good vacuum at about 925°C. In this process, care is taken to keep air out of contact with the hot metal, which otherwise would contaminate the product with oxygen and nitrogen. Both these impurities embrittle zirconium even when present in an amount as low as 0.1 pct. A number of previous reports1-3 describe the method and the various improvements that finally led to a workable process. The major steps made were the production of large quantities of carbide, which is the raw material for producing the chloride, its chlorination with reasonable efficiencies, and the elimination of iron trichloride contained in the raw chloride, as well as that of the zirconium oxide which is always present in this product. The physical nature of the anhydrous chloride, which sublimes at 331°C at atmospheric pressure and melts at 420°C under a pressure of 25 atm, made it necessary to provide a special safety device on the purification and reduction vessels in the form of a lead-alloy seal, permitting escape of excess gases if pressure tended to build up. The main difficulties encountered in the reduction and in the following step, salt separation in a vacuum at elevated temperature, were caused by the material from which the reaction pot was constructed—iron. This metal reacts with zirconium at about 940°C with formation of a eutectic. The last step, salt separation by evaporation of the magnesium and magnesium chloride in a vacuum, is quite unconventional and has not been used before on such a scale. It is only due to the improved construction of high-vacuum pumps, especially oil-diffusion pumps, that such a method could be used. The various steps of the Bureau of Mines process, as described in the general outline above, may be summarized as follows: (1) production of the carbide, (2) chlorination of the carbide, (3) purification of the raw chloride, (4) reduction of the pure chloride with fused magnesium, (5) separation of excess magnesium and magnesium chloride in vacuum at elevated temperature, and (6) melting of the sponge obtained. Production of Carbide The arc furnace, described in a previous report,' was improved both to reduce the graphite consumption caused by the burning of the bottom plates and to concentrate the heat in order to obtain better power efficiency. This was achieved by providing the bottom with graphite plates entirely embedded in refractory bricks, the contact with the current being made with three water-cooled copper plugs. Figs. 2 and 3 show the arrangement. The crucible, made

Jan 1, 1951

By Gilbert Santoro

In this study tantalum carbide filaments of various compositions in the fcc region were prepared by heating a tantalum wire in a measured amount of hydrocarbon vapor. Such properties as tensile strength, transverse-rupture strength, microhard-ness, lattice parameter, electrical resistivity, and magnetic susceptibility were measured as a function of carbon content. Some of these properties showed a maximum or a minimum between a carbon-to-tantalum molar ratio of 0.80 and 0.85, the composition range at which the color changes from metallic gray to gold. The recent literature has shown that in the large homogeneity range for the fcc phase of the Ta-C system there is a marked variation for such properties as microhardness,' electrical resistivity, ' thermodynamic properties,z'3 lattice parameter and superconductivity. In addition to the technological interest of these variations within a single phase, important theoretical benefits may ensue from a continuous investigation of properties vs stoichiometry in tantalum carbide and other refractory defect compounds, for example the effect of the metal-metal distance and crystal structure upon bond formation and electronic structure. Whether there is a similar variation of the tensile strength is of practical importance. Of theoretical interest would be the knowledge of how the magnetic susceptibility varies with carbon composition. Both of these properties, as well as the transverse-rupture strength, were determined for tantalum carbide filaments in the fcc phase region. The lattice parameter, the electrical resistivity, and the microhardness were also investigated and compared with values appearing in the literature. EXPERIMENTAL PROCEDURE Material Preparation. Tantalum carbide specimens of various carbon content were prepared by statically carburizing high-purity tantalum filaments in measured quantities of pure hydrocarbon gas. The filaments, which were 10 mil in diameter and 20 or 40 cm long, were heated by their own resistance at temperatures from 1800" to 2200°C using alternating current in some cases and direct current in others. Tantalum wire from two sources was used. One had a reported purity of 99.96 wt pct Ta. The ingot from which this wire was drawn had been electron beam-melted as the final step in its purification. The reported purity of the other wire, which was prepared by a powder metallurgical process, was 99.88 wt pct Ta. The impurities of both tantalum sources are listed in Table I. Spec-trographic-grade toluene or research-grade propane was used as the source of carbon. The apparatus for the carburization of the filaments is shown schematically in Fig. 1. The system was evacuated to 1 x l0-' mm of Hg when using the electron beam-melted tantalum and to less than 1 p when using the less-pure tantalum. Neither the difference in the base vacuum, nor in the hydrocarbon gas, nor in the tantalum filaments resulted in any detectable difference in the properties studied in this work. However, only the carbides prepared from the higher-purity tantalum were used in the magnetic-susceptibility determinations. Once the base vacuum had been reached, the system was flushed with the hydrocarbon and re-evacuated. For any desired composition of the carbide, hydrocarbon gas was allowed to leak into a constant-volume flask to a predetermined pressure. These pressures were measured by a Cartesian diver-type mercury gage with a range from 0 to 20 mm and with a scale expanded to nine times. The hydrocarbon gas was allowed into the reaction tube and the filament was quickly raised to the reaction temperature. The slack in the filament due to thermal expansion was taken up by drawing out the movable electrode with a screw mechanism. The filaments were kept at temperature from a few minutes to 200 hr. In the majority of cases the heating time was 6 hr. The reaction tube was cooled by cascading water on its outer surface. By means of an ammeter and a voltmeter the electrical resistance at the reaction

Jan 1, 1963

By D. E. Etter, J. E. Selle

The Pu-Ce phase diagram was determined by differential thermal analysis, metallography, and elechm-nricroprobe analysis. The dingram is chararterized by a eutectic with extensive solid solubility in the cubic Phases of both cerium and plutonium. No intermediate phases were found. Cerium is soluble in e plutonium to 16.0 at. pet Ce at 626OC nnd in d plcltoniurn to 23.0 at. pet at 613 "C, decreasing to 17.5 at. pet at room temperature. No solubility in the a, ß, or ? phases was jound, and the mininum cerium required to stabilize 5 plutonium to room temperature is 3.2 at. pet. The maximum solubility of plutonium in 6 cerium is 19.5 at. pet at 721OC, and the maximum soluhility of plutonium in ? cerium is 34.5 at. pet. Invariant points in the system are: a) eutectic at 626oC, L16.5 = E Pu16.0 + y Ce65.5; b) peritectoid at613oC, e Pu13.5 -y Ce65.5- d Pu23.0. AS part of a program aimed at the determination of the phase equilibria in the Pu-Ce-Cu ternary system, preliminary investigations were made of the three binary systems. A survey of the Pu-Ce binary system by differential therma1 analysis indi- cated several areas of disagreement with the published diagram,' primarily in the shape of the liquidus surface. Consequently, a thorough investigation of the system was undertaken, and this report presents the results of the study. EXPERIMENTAL PROCEDURE Three methods of investigation were used: differential thermal analysis (DTA), metallography, and analysis with electron-microprobe X-ray analyzer (EMX). The EMX analysis was particularly useful for the determination of solvus lines. The DTA method was most useful for the determination of the liquidus curves. Metallography complemented both of these techniques. Materials. The cerium metal used for most of this work had a freezing point of 805°C. This material showed 15°C premelting, and was found metallographically to contain some unidentified in~lusions.2 The temperature of premelting is defined as the point at which the DTA curve breaks away from the base line, analogous to a curve obtained from a solid-solution alloy. Several compositions were prepared near the cerium end of the diagram with higher-purity material which had a freezing point of 800°C. etallographic analysis showed this material to be relatively free of inclusions and only 8°C premelting was observed. Major impurities were found by spectrographic

Jan 1, 1964

By J. L. Whitlock

An attached growth aerobic biological treatment process has been developed at Homestake Mining Co.'s Lead operation which not only oxidizes free and complexed cyanides, including the stable iron complexed cyanides, but also thiocyanate, and the oxidation byproduct ammonia. Through the employment of a mutant strain of bacteria which has been gradually and specifically acclimated to the waste, these potential pollutants are mineralized to relatively harmless sulfates, carbonates, and nitrates. The resultant effluent, through toxicological testing, has been shown compatible with the receiving stream, which serves as a cold water marginal trout fishery.

Jan 1, 1985

By G. S. Ansell, J. Weertman

The creep behavior of an aluminum alloy hardened with a finely dispersed phase of aluminum oxide was investigated. The as-extruded alloy shows an approximate steady-state creep in which the creed rate depends exponentially on the applied stress. The activation energy of creeb is abbroximately 150,000 cal per mole. The recrystallized alloy shows no steady-state creep. ONE method of improving the creep resistance of a metal is to introduce a finely dispersed second phase into the metal matrix. The improvement of the creep resistance has been qualitatively explained by assuming that the dispersed second-phase particles act as obstacles to dislocation motion. If the main effect of second-phase particles is simply to hinder dislocation motion then it is possible to derive a high-temperature creep equation for a dispersion-hardened alloy in a straightforward manner. In the Appendix of this paper such an equation is derived from a creep model which works very well for pure metals. Recently, F. V. Lenel has fabricated, for the first time, powder extrusions of aluminum-aluminum oxide in a large-grained recrystallized form. This alloy, designated as MD 2100, consists of a fine dispersion of aluminum oxide plates in a matrix of commercial purity aluminum. A considerable amount of investigation has been carried out concerning the microstructure and physical properties of this alloy.&apos; ) The aluminum oxide is present in the form of flakes 130A units thick and 0.3 u on edge. They are dispersed in the aluminum matrix with an average spacing of approximately 0.5 jx. The spacing varies in the range of 0.05 to 1.5 µ. The alloy structure is extremely stable at high temperatures. For this reason the alloy offers a unique opportunity for a fundamental study of creep of a very finely dispersed two-phase alloy. Lenel supplied specimens in both the unrecrystallized and recrystallized condition. This paper reports high-temperature creep experiments carried out on these specimens. The results obtained were rather unexpected. No steady-state creep was observed in the recrys-tallized material. In fact, after some transient creep which takes place upon loading, the creep rate is essentially zero ( < 10-8per min). If the second-phase particles acted solely as obstacles to the motion of dislocations, measurable steady-state creep would be expected. Since none is observed it appears that the main effect of the fine dispersion in the recrystallized material is to inactivate the dislocation sources themselves, rather than hinder the motion of dislocation loops created at these sources. EXPERIMENTAL DETAILS Specimens were tested in wire form, 0.087 in. in diam for the as-extruded alloy, and 0.035 in. in diam for the recrystallized alloy. These samples were held in friction-type wire grips; a gage length of 2.5 cm was used for all the creep tests. The specimens were held at 600°C in the test apparatus for at least 15 hr prior to each test. The tests were run under the condition of constant loading and, since the creep strains were small, can be considered as constant stress tests. The temperature of testing was held constant within 3°C. Elongations were measured with an optical cathetometer which was capable of measuring strains as smaIl as 0.00012. This allowed the measurement of strain rates as low as l0-8&apos;per rnin. In addition to the creep tests optical micrographs were made in order to determine both the grain size and microstructure of these materials. RESULTS Fig. 1 shows a few typical creep curves obtained from the as-extruded material. The elongations were somewhat erratic, but each curve shows a region of quasi-steady-state creep from which an approximate steady-state creep rate can be obtained. In general the higher the stress at a given temperature, the greater the total elongation before fracture. The lower the applied stress, the longer is the region where the creep rate is almost constant. Summary data from the creep tests of the as-extruded material are listed in Table I. The steady-state creep data of the as-extruded material for a range of stresses at a constant temperature follow a creep equation of the type creep rate = K&apos; = A exp (&) [11 where A and B are constants, k is Boltzmann&apos;s constant, T is the absolute temperature, and a the stress. The standard error of estimate of the data received is less than one order of magnitude. As shown in Fig. 2, if one compensates the creep-rate data for the effect of temperature over the range of test temperature, the steady-state creep data roughly follow a creep equation of the type Temperature compensated creep rate = K* = A exp

Jan 1, 1960

By J. J. Lillie

Sublevel stoping was first developed in the Michigan iron mines many years ago. Since that time this method, and modifications with long hole drilling, have been used in a number of non-ferrous mines and have been described in various papers and articles. With a few exceptions, the operations where sublevel methods have been applied are producers of large daily tonnages from ore bodies of considerable size. In selecting mining methods for small properties or relatively small detached ore bodies, sublevel methods often have been overlooked. The method has been used success- fully in relatively small operations at Copper Canyon, Nevada, and, more recently, in mining small ore bodies at Darwin, Calif. As a result of this experience, we believe that a review of the general procedure, the advantages noted, and the results obtained will be of interest to many operators of relatively small mines.

Jan 1, 1949

By P. L. Allsman

A method of analyzing blasting action indicates that major cost savings are possible by revising practice and bringing the classical blasting formulas up to date; difficult problems such as taconite and throw-breakup can be attacked by engineering Denonation pressure — the peak pressure developed by the explosive reaction; "shatter blasting." Average detonation pressure — the average pressure over the time the reaction continues; "heave blasting." Radial presswe — the stress in a radially expanding sphere about the detonation. Corresponds to the diminishing peak pressure. Lateral stress - the stress in a circumferential direction, induced by outward movement of the rock away from the detonation. Limiting stress or Slim— the rock property at which failure will occur in the case at hand; may be tensile or compressive strength, or combinations. Recent developments in explosives technology, following the advent of nuclear explosions, have led to a rather complete understanding of their action. A survey was made for the purpose of uncovering any knowledge which might be applicable in the mining and quarrying industries, the principal users of explosives. Although no revolutionary techniques have become apparent, much basic data pertaining to blasting — fortunately not classified — have been developed by recent research, from which a good general understanding of the process can be derived. It is hoped this explanation of the scientific principles governing explosive action, together with a proposed analysis of blasting practice, will further the development of mining engineering. NATURE OF THE REACTION: The phenomenon of explosion, termed detonation, is in reality a rather complex chemical reaction, and as such is completely explainable by physical and chemical laws. Detonation is characterized by high temperature and pressure, extreme rapidity — often being complete within one microsecond — and most importantly by formation of a shock pulse which accompanies the reaction zone. As with any chemical reaction, there is a critical value of temperature and pressure below which detonation can not occur; this is termed the "critical point". Whereas an explosive substance will decompose slowly at ordinary temperature, with the formation of gases which readily dissipate; at elevated temperature the reaction is considerably speeded. If pressure is suddenly applied at some point in an explosive medium, adiabatic compression results, and the temperature is locally raised. When the temperature becomes high enough the decomposition will be so rapid that the gaseous products do not have time to dissipate, but contribute to a further build-up of pressure. This, in turn, furthers adiabatic temperature rise over a widening area, and with any heat generated by an exothermic reaction, causes a rapid increase in temperature. Both temperature and pressure are spontaneously built up in this manner until the critical point is reached, resulting in detonation. The values of pressure and temperature necessary to create detonation are established by the unusual nature of the process. If temperature alone is raised above the critical point, without sufficient increase in pressure, deflagration or "low-order detonation" occurs. In the true, or "high-order detonation", the shock pulse resulting from the violent decomposition becomes an integral part of the reaction, and itself aids in increasing the detonation

Jan 1, 1961

By Emmanuel P. Papadakis

Ultrasonic velocity measurements have been made to study the preferred orientation in cube-textured copper. Methods applicable to thin specimens were employed since the specimens were necessarily of sheet material. The measured velocities in various directions in the sheet differed from the corresponding values in single-crystal copper by 1 to 6 pet. The distribution of the deviations indicated that the align-ment of the (001) planes with the rolling plane was better than the alignment of the [100]and [010] directions with the rolling and transverse directions. Ultrasonic pole figures (velocity us orientation) are shown to be useful in the study of preferred orientation. THIS paper describes one set of experiments in a continuing study of preferred orientation in worked metals. This study has been undertaken to investigate the fundamental properties of metals when used as propagation media for ultrasonic waves. Many such materials are of current or potential use in ultrasonic delay lines. Fundamental studies on ultrasonic propagation parameters such as velocity, attenuation, and diffraction (beam spreading) are of importance in the design of delay lines, in the development of nondestructive testing methods, and in the study of materials themselves. Preferred orientation in worked poly-crystalline metals influences all three above-mentioned parameters, and hence is of particular importance. When polycrystalline metals are subjected to mechanical working, they develop textures dependent upon their crystal structure and the symmetry of the working operation.&apos; The texture consists in the alignment of the crystallographic axes of the grains in preferred directions with respect to the symmetry axes of the working operation. Since the grains are elastically anisotropic, the elastic moduli of worked metals are anisotropic. Hence the velocities of elastic waves in worked metals depend on the directions of propagation and polarization. The worked metal may be thought of as taking on the elastic symmetry of a single crystal: so it possesses the same number of independent elastic moduli as the crystal class it simulates. In general, a worked metal does not adopt the crystalline symmetry of its own grains. For instance, most rolled sheet becomes effectively orthorhombic while all bar stock and wire develop hexagonal symmetry. However, certain metals with cubic crystal structure develop a cube texture upon rolling and annealing.= Nearly perfect alignment of [100]-type directions with the rolling direction, transverse direction, and rolling-plane norma1 can be achieved in certain fcc metals and alloys. These cube-textured rolled metals provide an excellent opportunity to test preferred orientation by means of elastic waves, since a worked metal with 100 pct cube texture would have elastic moduli identical to the moduli of its constituent metal. It is the purpose of this paper to present the results of an investigation upon cube-textured copper. Ultrasonic waves were used. The methods of measurement and the experimental results on the effective moduli will be given. The ultrasonic measurements will be shown to complement X-ray pole figures for the determination of preferred orientation in worked metals. EXPERIMENT To study cube - textured material, it was necessary to use thin-sheet material since a severe reduction in gage (95 to 99 pct) is necessary to produce cube texture. Special ultrasonic methods were needed to investigate the thin material at megacycle frequencies. A) Materials. The cube-textured material tested was a copper alloy containing 1 pct Zn. Specimens already measured for Young&apos;s modulus4 by Alers were kindly supplied by him. The specimens were slabs 3.00 by 0.25 in. cut from sheet 0.047 in. thick. The orientations of the long axes of the specimens with respect to the rolling direction were taken in 15-deg steps from 0 to 90 deg. B) Measurements. Two distinct experiments were performed to measure the phase velocity in these specimens. One measured the shear wave velocity for propagation in the 0.25-in. direction and polarization in the 3.00-in. direction. The other measured the velocity of both shear and longitudinal waves propagating in the thickness direction in the sheet. 1) Plate-Mode Measurements. The velocity of the zeroth-order shear mode5 was measured in the 0.25-in. direction in each strip. The specimens were ground thinner over half their length to assure that the first-order shear mode would be cut off below 6 Mc per sec, leaving the zeroth-order nondispersive shear mode as the only propagating mode. Piezoelectric ceramic transducers of 5 Mc per sec resonant frequency poled in their long direction were solder-bonded to the edges of the thin part of the slabs as in Fig. 1 after these edges had been made flat and parallel by fine grinding. These transducers produced waves polarized in the 3.00-in. direction and propa-

Jan 1, 1967

By Yves Dardel

INTRODUCTION SINCE the first determination of Dumas1 in 1880, many authors have tried to measure the solubility of hydrogen in solid aluminum, or at least the amount of dissolved gas in it. However, the interpretation of the results which have been obtained is still difficult. Sieverts,2 then Baukloh and Oesterlen,3 during their gassing experiments could not determine any solubility of hydrogen in solid aluminum. On the other hand, Portevin, Chaudron and Moreau,4 leaving the determination of the hydrogen solubility beyond the scope of their experiments, measured only the amount of gas that they could extract by high voltage positive ion bombardment and found up to 151 cm3 of gas per 100 g of metal. Winterhager,5 by repeated vacuum extraction during severe cold rolling, extracted up to 161 cm3 per 100 g. In both series of experiments, the extracted gas contained chiefly hydrogen with a small amount of nitrogen, carbon monoxide, carbon dioxide and methan. Later, Schmidt and von Schweinitz6 as well as Chaudron and Moreau7 showed the importance of the adsorbed layer of hydrogen, the extracted quantities being proportional to the surface and not to the weight of the sample, when its cleaning was not perfect. In earlier experiments, Steinhauser8 extracted from more massive samples nothing but a little amount (< 0. 5 cm3 per 100 g) of hydrogen, carbon monoxide and methane. Thus, according to these experiments the quantity of dissolved gas is probably very small and the effect of the surface could falsify the results of the extraction. However, owing to the care taken by Chaudron and his coworkers, it was clear that all the hydrogen extracted could not come from the superficial layer, or that the links which bound hydrogen to the surface were so strong that the usual method of cleaning could not destroy them. After the main parts of the experiments reported here had already been carried out, Eborall and Ransley9 published the results which they obtained with an analysor having an accuracy of 0.03 cm3 per 100 g, while that of the usual apparatus was only about 0.2 cm3 per 100 g. During all their experiments the adsorbed layer would have been a difficulty, for the value of the adsorbed hydrogen was approximately equal to that of the dissolved amount. [ ] Since always keeping the same adsorbed layer is very difficult, an error in the correction for the adsorption can be made when using the apparatus of Eborall and Ransley, as well as the earlier apparatus,

Jan 1, 1948