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By George S. Rice

The A.I.M.E. Ground Movement and Subsidence Committee, proposed in 1920, held its first technical meeting in February 1923, under the able chairmanship of Mr. H. G. Moulton. The following list of papers and discussions, indicating the scope of the problems and relation to various conditions and method of mining, were given at that meeting by the distinguished mining engineers: J. Parke Channing, on Subsidence at Miami, Arizona; Howard N. Eavenson, on Mining an Upper Bituminous Seam after a Lower Seam Has Been Extracted; J. J. Rutledge, on Subsidence in Two Oklahoma Coal Mines; Benjamin F. Tillson, on Caving Cracks at the Franklin Mine, New Jersey; Dr. F. W. McNair, on the Dome Theory; William Kelly, on disadvantageous effects in Mining and Back-filling Working Upward a Steep-Pitching Iron-ore Bed; Eli T. Conner, on the good results of Back-Filling by Hydraulic Means in Preventing Destructive Subsidence in the Anthracite District; Thomas H. Claggett, on the merit of Systematic Pillar Drawing in Preventing Cracks in an Upper Seam; Henry H. Otto, successful results in the anthracite district in Mining Lower Seams before Upper Seams; Douglas Bunting, on Leading Factors Incident to Successful Mining of an Overlying Seam; Edwin Ludlow, on there being "less damage to buildings when there was complete removal of coal with complete packing than when room and pillar is used without extracting the pillars"; Edward O'Toole on "bumps" in eastern Kentucky mines, which he thought were the result of geologic stresses: H. A. Buehler, on Upheaval of Surface in an Illinois Case in Advance of the Face; and R. Dawson Hall, on The Mechanics of Subsidence from Mining. The author of this paper discussed various kinds of problems of ground movement and subsidence in both metal mining and coal mining; the production of great landslides by workings near an outcrop, as at Turtle Mountain, Alberta, Canada; and general

Jan 1, 1940

By P. G. Shewmon, F. N. Rhines

THE determination of the self-diffusion coefficient of magnesium has been made possible recently by discovery1-1 of a radioactive isotope, Mg28 having a half-life of 21.3 hr,1 and subject to manufacture in useful quantity. In the present research this material was condensed from the vapor phase upon a surface of high purity magnesium. The progress of diffusion of the tracer atoms into polycrystalline magnesium was followed by machining layers and measuring the change in the intensity of radiation as a function of the distance of each layer from the surface. The self-diffusion coefficient was found to be 2.1 X 10-8 sq cm per sec at 627°C, 3.6 X 10-9 sq cm per sec at 551°C, and 4.4 X 10-10sq cm per sec at 468°C; the activation energy is about 32,000 cal per mol. Experimental Procedure Since there was no other published measurement of a diffusion velocity in any magnesium-base material, is was necessary to employ a number of new experimental techniques. The short half-life of Mg28 made it necessary to complete the entire experimental procedure within three or four days. This meant that the work had to be done where a cyclotron was readily accessible and that all operations, prior to the diffusion heat treatment, had to be so designed as to minimize their time requirements. Unusual problems were imposed also by the chemical reactivity of magnesium, its high vapor pressure, and the fact that no satisfactory method for elec-trodepositing magnesium on magnesium is presently available. Finally, the machining and handling of the easily air-borne radioactive-magnesium chips involved certain health hazards, resulting in the need for further experimental restrictions. Preparation of Mg28 The Mg28 was produced in the Carnegie Institute of Technology syncrocyclotron by the neutron spallation of chlorine.5 his involved bombarding a 2 gram crystal of high purity NaCl with a beam of 350 mev protons for a period of 2 hr, after which the crystal was dissolved in warm water and the Mg28 was concentrated and purified by chemical means (see Appendix). About 50 microcuries of Mg28 thus were obtained in the form of magnesium oxinate (8 hydroxyquin-olatc?), which was ignited in air to produce MgO. This in turn was reduced to magnesium metal vapor, by the method of Russell, Taylor, and Cooper," in the vacuum apparatus shown schematically in Fig. 1. Here the essential part is a tantalum ribbon, slightly dished to receive the MgO. The ribbon, pre- viously outgassed at high temperature, is heated to about 1700°C by passing an electric current through it, whereupon tantalum oxide is formed, magnesium vapor is released almost instantaneously, and condensed partly upon the diffusion sample. Diffusion-Sample Preparation: Hot-extruded magnesium rod, 21/32 in. round was used in making the diffusion specimens. The magnesium analyzed as follows: 0.004 pct Al, 0.027 pct Fe, 0.040 pct Mn, 0.0004 pct Cu, 0.0002 pct Ni, and less than 0.01 pct Ca, 0.0004 pct Pb, 0.0011 pct Si, 0.001 pct Sn, and 0.001 pct Zn. A brief study of the crystal texture of this material revealed a sharp fiber texture with the (001) plane roughly parallel to the extrusion axis. Cylindrical samples 1/2 in. long by 5/8 in. were machined from this rod, the end faces dressed on 3/0 emery, and lightly etched with 20 pct HC1 in water. These samples then were annealed for at least twice the intended time of diffusion, at the intended diffusion temperature, in order to stabilize the grain structure at about 1 mm average diameter. The annealing treatments were conducted in argon in the same apparatus and in the same manner as the subsequent diffusion treatments, which will be described presently. Thus, a strain-free plane surface was produced, but there remained a layer of MgO which had largely to be removed before the layer of Mg28 was deposited. Most of this layer was taken off by two light passes over 3/0 emery paper. The balance of the oxide and a thin layer of metal were then removed by etching 5 to 10 min in 4 pct nital (4 pct HNO3 and 96 pct ethyl alcohol) made with absolute alcohol. There followed immediately three quick rinses in: 1-49 1/2 pct methanol, 49 1/2 pct acetone, and 1 pct formic acid, 2-50 pct methanol and 50 pct acetone, and 3-pure benzene. This procedure is essentially that of Sturkey.7 The resulting surface, which was of almost elec-tropolished brightness, remained plane and was free of cold work. It could be kept clean by storing under benzene, or in a desiccator; short exposure

Jan 1, 1955

By Leonard Austin

WHAT Colonel Dwight says regarding the treat-ment of oxidized ores1 holds true also of the silver-lead smelting operations in Utah. The ore sought for was such as would, with appropriate fluxes, yield slag, and "lead bullion," as the lead reduced from the ore and carrying its gold and silver, was called. No matte, and probably little or no speiss, was yielded, and hence there was nothing to roast, either of ore or matte. But, by 1880, when I first took hold in smelting, there was quite a production of matte at the works of the Ger-mania Smelting and Refining Co., Utah, because, by that time, ores containing some pyrite and galena were being smelted. This was due, as at the Grant Works, Denver, to the more attractive price paid for the treatment of such ores. The matte, containing about 5 per cent. copper, was accordingly heap-roasted and returned to the blast furnace for the recovery of its contained metals. By this time there had been built a long-bedded, hand-rabbled reverber-atory roaster with a hearth of about 40 by 10 ft. in size, and in this matte and ore, crushed at the sampling mill, was treated. When, in 1892, I took control of this works, called& now the Germania Lead Works, three other roasters had been added, but the prac-tice of heap-roasting continued. This had the merit of needing no equipment, and of doing good work, because the pieces that were imperfectly roasted went back upon the next roast heap. At this time, when some suitable lump ore was obtainable, I roasted in heaps, in a satisfactory way. By 1892, the Bruckner cylinder roaster had been installed, which, compared with the reverberatory roaster, reduced labor. As such a cylinder revolves, a talus of ore is formed within it and at the same time fresh surfaces are exposed to the air, but the trouble was that the air did not reach to the bottom of the cylinder. This we corrected by placing a steam jet at the fire-box end, to project the air down-ward upon this stagnant ore, thus increasing the speed and completeness of roasting without at the same time increasing dust formation. The firing, if skilfully done, gave a somewhat sintered product, but with certain ores a slight access of heat over the normal would cause accretions to form within the cylinder near the fire end. These could be cut off by running back the fire box and barring off the crusts. It was in 1895 that the Bruckner cylinders at the Arkansas Valley plant, Leadville, were giving unsatis-factory service and I was called in to investigate. The steam jet was put in use as at the Germania Lead Works, but we found that, due to the altitude (10,500 ft.), combustion was feebler than at sea level or even at 4000 to 5000 ft. Later it appears, as Colonel Dwight states, that R. D. Rhodes and Mots sought to increase the air supply by admission through perforated tiles, but the trouble was due to the air itself.

Jan 8, 1922

By P. E. Arnold, G. S. Ansell

RELAXATION in metals has been studied in detail by many workers in recent years.1-5 These studies have shown that there is an energy-loss peak observed in a metal placed in mechanical resonance at low frequencies which may be correlated with various metallurgical processes. These experiments have been largely used to study single-phase materials. In order to study the effect of a finely dispersed second phase in a metal matrix upon this phenomenon, the relaxation behavior of an aluminum-aluminum oxide SAP-Type alloy in both the fine-grained as-extruded and coarse-grained recrystallized conditions was investigated by the use of internal-friction measurements. The alloys studied, designated MD 2100, consist of a matrix of commercial-purity aluminum containing a finely dispersed second phase of aluminum oxide. The aluminum oxide is present in this alloy in the form of fine platelets approximately 130A units thick and several microns on edge. The mean free path betwen dispersed platelets is approximately 0.5 p. The grain size of this alloy is extremely stable at temperatures as high as the melting temperature of the aluminum matrix. In the as-extruded condition the grain diameter is several microns, while in the recrystallized condition it is several millimeters in diameter. The damping characteristics of the alloy samples were determined using a torsional-pendulum device. The internal-friction constant was determined for this alloy in both the fine-grained as-extruded and coarse-grained recrystallized conditions over the temperature range from 343" to 923°K at frequencies of 0.9, 1.3, and 1.8 cycles per sec. An internal-friction peak was observed in testing the fine-grained alloys which was not observed for the coarse-grained alloys. This peak, which might be associated with a type of grain-boundary relaxation, was observed at each of the three different test frequencies for the fine-grained sample. The temperature at which the relaxation peak occurred for each of the three different frequencies is shown in Table I. From these data an activation energy of relaxation for each pair of frequencies was determined by comparing the temperature shift of the relaxation peak with frequency between each of the test frequencies, assuming that an Arrhenius-type rate equation is applicable. The activation energy of relaxation determined from these data is also shown in Table I. The mean value of the activation energy was about 6 kcal per mole. The activation energy for the relaxation process determined in this investigation indicates that the relaxation associated with the grain boundaries in this aluminum-aluminum oxide SAP-Type alloy is quite a different process than grain boundary relaxation in single-phase aluminum alloys. In these latter alloys, the activation energy for relaxation has been found to be the activation energy for self-diffusion, approximately 36 kcal per mole1,2 Where the activation energy is the same as the activation energy for self diffusion, it has been proposed that the relaxation phenomena is dependent upon vacancy formation and motion. It is apparent therefore, that, in this aluminum-aluminum oxide SAP-Type alloy, the relaxation must be due to another type of atom transport. It has been shown previously in studies of the high-temperature, low-stress, steady-state creep behavior of as-extruded aluminum SAP-Type alloys, that the activation energy for steady-state creep is one that may be characterized by the nucleation of dislocations from the grain boundaries. It is proposed that the relaxation behavior observed here is due to a similar effect. In this case, the internal-friction peak is a resonance behavior due to the time-dependent nucleation of dislocations from grain boundaries in the sample. A process of this type would have an activation energy which is undoubtedly stress-dependent and of the form Q = Q, + (dQ/du)u

Jan 1, 1962

By J. Campbell

Long freezing range casting alloys are particularly susceptible to a type of porosity which is observed to form in layers parallel to the supposed position of the isotherms in the solidifying casting. Under favorable conditions (which appear to be typified by low-temperature gradients in the casting giving rise to a wide and more or less uniform pasty zone, and which arise from several factors, particularly: a) wide freezing range alloy, b) high thermal conductivity of metal, c) low thermal conductivity of mold, and d) high mold temperature3) layer porosity has been observed in many different casting alloys: copper,' aluminum, magnesium,' steels, and high-temperature alloys.3 Baker4,5 and later cibula6 argue that layer porosity occurs because of thermal contraction, in a manner analogous to hot tearing. In outline, the theory consists of the establishment of a coherent dendrite network by the impinging of dendrite tips. Subsequent shrinkage imposes tensile stresses on the network which tears perpendicularly to the stress, i.e., parallel to the isotherms. If these tears are not filled by the inflow of residual liquid then layers of porosity result. Baker7 attempted to test whether the porosity was the result of thermal contraction by casting test pieces in a mold designed to accentuate hot tearing. However, no significant increase in porosity was observed. This negative result of Baker's critical experiment appears to be substantiated by numerous observations, particularly the experiments by Lagowski and Meier8 on Mg-Zn alloys covering the range of zinc contents up to 30 pct Zn. These clearly reveal that the maxima for the incidence of hot tearing and layer porosity are well-separated, occurring at 1 and 6 pct Zn, respectively. Furthermore, the thermal contraction maximum occurred at 1 pct Zn, indicating that hot tearing is associated with contraction in the solid state, and not with porosity. These observations are further substantiated by the elementary consideration that the thermal contraction of the casting is likely to produce (if anything, since the temperature difference across casting of high thermal conductivity, such as aluminum and copper, is likely to be negligible) a compressive stress on the

Jan 1, 1969

By J. B. Newkirk, A. H. Geisler

Certain of the permanent magnet alloys provide ideal systems for the study of the kinetics of the precipitation reaction and the correlation of structure with properties. One such system, Cu-Ni-Fe, was found by Bradley1,2 to exhibit a coherent transition state in the precipitation process analogous to that reported for Al-Cu alloys somewhat earlier.3 The attractiveness of some perrnanent magnet alloys for study lies in the fact that vertical sections of the ternary phase diagram in certain regions of composition (Fig I) have as their prototype the binary Ni-Au diagram. Alloys of this type decompose into products that have the same crystal lattice type but only slightly different lattice parameters. The advantages that such alloy systems oA&apos;er for study over the usual in which an intermetallic compound is formed are many: 1. Since the precipitate has the same crystal strutture as the matrix, complex atomic movements are not required to form the new lattice. 2. Similarly, complex orientation relationships are not involved for both the matrix and the precipitate would be ex. petted to have the same orientation. 3, Small &,registry of the decomposition products at equilibrium (in contrast with Cu-Ag alloys) is conducive to extensive coherent growth in the transient state and thus the transition lattice can be detected by the usual X ray diffraction methods. 4. Finally, the relative quantities of precipitate and depleted matrix can be varied from 0 to 100 pet* thus permitting wide freedom for the study of the effect of cornposition on coherent growth and properties. In the Cu-Ni-Fe alloys of appropriate composition, the face-centered cubic precipitate and also the depleted matrix when first formed are coherent with the parent matrix.1&apos;2 The two have the same <Jo parameter as the original matrix but they are both tetragonal; the precipitate has an axial ratio c/a < I while that of the depleted matrix is c/a > I. When coherency is lost they assume the normal face-centered cubic structure with the depleted matrix having a lattice parameter greater than the original matrix and that of the precipitate less. Such a mechanism would also be expected for CU-Ni-CO alloys because of the similarity in constitution but this had not been demonstrated. The Present investigation was conducted on a CU-Ni-CO alloy. The constitution diagram and magnetic properties of these alloys have been fairly well established, however, no previous determinations of mechanism of precipitation and no correlation of structure with properties had been made. Thus, an alloy of this system Was chosen for a comprehensive investiga-

Jan 1, 1949

By T. C. Russell

The Conda phosphate mine, eight miles north of Soda Springs in Caribou County, Idaho, was opened up by the Anaconda Copper Mining CO. in 1920. Except for brief periods, during the 20&apos;s and early 30&apos;s, the mine has maintained a continuous production, and 2,100,000 short tons of phosphate rock have been shipped to the company&apos;s phosphate fertilizer manufacturing plant at Anaconda, Mont., or to independent processing plants on the Pacific Coast; a small tonnage of the rock has been shipped to the Hawaiian Islands. The Phosphoria formation on the Conda property consists of two, commercial-grade phosphate beds separated by 147 ft of black to brownish colored phosphatic calcareous shales interbedded with softer mudstones, clays, and occasional narrow seams of oolitic phosphate. The main lower phosphate bed in the series averaging 7.1 ft in thickness, is called the "foot-wall bed," which lies coriformably on the Wells limestone formation, the 1atter often containing irregular bands of chert. The upper or " hanging-wall bed" of phosphate rock averaging 7.2 ft in thickness, is overlaid by thick quartzite beds, locally called the " Rex chert" member in the upper portion of the Phosphoria formation. (Fig 1.) There are two anticlines on the property with axis striking approximately parallel to the mountain range beneath which extensive development on phosphate rock has been conducted in the past, and is now in progress. The phosphate beds have been eroded to a large extent from the tops of these anticlines, leaving at least three well-pronounced outcrops of the phosphate beds exposed within the boundaries of the Anaconda Copper Mining Cornpany&apos;s properties. At present, mining operations in the Conda No. 3 mine are confined to the two phosphate beds along the east flank of the easternmost anticline, where the dips on the beds vary from 50° to 60° east, thereby affording favorable conditions for the sublevel mining system now in use. Mining operations formerly were confined to the footwall or lower oolitic phosphate bed because of its higher phosphate and vanadium contents (32 pct P²O5 and 0.29 pct V2 O 5); this bed averages 7.1 ft in thickness. The oolitic portions of the upper bed were of satisfactory grade, but the shale and clay partings (Fig 2) diluted the mined rock and could not he separated economically by selective mining or by sorting. Experiments in beneficiating this rock were carried on for a number of years. Recently, a simple washing process was adopted, which gave a satisfactory grade of concentrates and a high recovery of P² O5. In 1947 it was decided to expand Anaconda&apos;s production of treble superphosphate and phosphoric acid by approximately 90 pct. This rock will be obtained from the footwall and hanging-wall beds, and the rock from the hanging-wall bed will be benefici-ated at -Anaconda.l In order to take advantage of the previous development on the 500 secondary haulage level, short crosscuts will be driven at approximately 950 ft intervals from the existing lateral drifts through the hanging-wall shale beds. From the inner end of each crosscut, short lateral drifts will he driven in both directions, so that four working raises can he put up on the dip of the phosphate bed at proper intervals along each of the lateral drifts. The mining operation on the footwall bed at Conda

Jan 1, 1950

By D. L. Martin

THAT small amounts of impurities have a harm-J- ful effect on the malleability of metals and alloys is well-known. One common type of em-brittlement involves the formation of a small quantity of eutectic at the grain boundaries, and is typified by sulfur embrittlement of nickel. Another example of eutectic embrittlement—sulfur embrittlement of cobalt—is described in this report. In the preparation of specimens for a study of Co-Pt alloys, it was observed that the hot swagabil-ity of the alloys appeared to be influenced by the grade of cobalt used as melting stock. The cause of the hot-shortness was not traced to any particular impurity, although sulfur was suspected.&apos; The damaging action of sulfur on the malleability of cobalt has not been generally recognized,&apos;; in spite of the fact that the Co-S phase diagram8 eveals the same basic conditions—low solubility and eutectic formation—responsible for sulfur embrittlement of iron and nickel.7, 8 Apparently sulfur embrittlement has not been a serious problem in the fabrication of cobalt alloys. One related factor is likely the limited commercial experience with high cobalt alloys, since the predominant use of cobalt has been in alloys containing less than 75 pet Co. A series of Co-S alloys was prepared and studied to establish the effect of sulfur on the hot working characteristics of cobalt. Specimens, 5/8 in. diam by 4 in. long, were prepared by vacuum melting in magnesium oxide crucibles and casting in a copper mold. Two grades of low sulfur electrolytic cobalt were used as the basic material for the study, one from Johnson, Matthey and Co. and the other from the International Nickel Co. Each contained about 99.5 pet Co and had a nominal sulfur content under 0.005 pet. The sulfur was added initially as cobalt sulfide powder. Later, some low sulfur alloys were prepared by diluting the high sulfur alloys with cobalt. Trouble was experienced in controlling the sulfur content. Apparently much of the cobalt sulfide powder was lost during melting, as most of the samples contained a lower sulfur content than was added. The alloys were evaluated for hot brittleness by heating to 1000°C in a hydrogen furnace and swaging in air. The results of these tests are summarized in Table I. All the alloys containing less than 0.008 pet S were successfully hot swaged to 1/4 in. diam. The bars containing more than 0.015 pet S could not be swaged because of the formation of intercrystal-line cracks similar to those illustrated in Fig. 1. Examination of the microstructure of the cast bars revealed cobalt sulfide eutectic at the grain boundaries, Fig. 2. The sulfide was not always continuous at grain boundaries in bars that were hot embrittled but, in general, the particles did form a network that could account for the brittleness above the eutectic temperature, 880°C. There is no question about the brittle nature of a specimen exhibiting a continuous sulfide network such as is shown in Fig. 2b, though a sulfide distribution similar to that in Fig. 2a is marginal. This particular bar cracked when hot-swaged. However, other bars with lower sulfur content but with some sulfide phase at grain boundaries were successfully worked. The reduction of area of a hot tensile test specimen was also found to be a sensitive indicator of sulfur embrittlement. The variation of reduction of area with sulfur content is shown in Fig. 3 for specimens fractured at 900°C in an evacuated capsule. The ductility of cobalt is greatly reduced when the sulfur content exceeds 0.005 pet. Similar results were obtained for alloys tested at 800°C, below the eutectic temperature. The upper sulfur embrittlement limit of 0.015 pet, Table I, agrees with the observation of Kalmus8 hat

Jan 1, 1957

By B. H. Kear, S. M. Copley

Stress-stvain curves are presented for Ni3Al (y&apos;) cvystals in several ovientations, deformed in tension and compression at constant displacement rate, at temperatures from 70° to 2000°F. Both the yield stress and wovk havdening increase with temperature, with the magnilude of the effect dependent on ovientation. The yield stress maximum occurs at 1500°F in [001], at 1400°F in [011], and at 1200°F in [111]. The suppression of the yield stress peak in [011] and [111] orientatiorzs is due to the onset of cube slip, rather than octahedval slip, a1 elerated temperatures. The temperature and orientalion dependence of work hardening in nominal single slip orientations corvelates with changes in the CRSS ratio for octahedral slip and cube slip, in agreement with a model for work hardening based on pinning of screw dislocalions by cross slip from an octahedral plane into a cube plane. It is concluded that the unique plastic properties of y&apos; have a decisive influence on both ductility and strength characleristics of y +y&apos; nickel-base superalloys. It has long been recognized that the strength of y + y&apos; nickel-base superalloys depends on the precipitation of the y&apos; phase [basically Ni3(Al,Ti)]. This paper presents new data on the strength characteristics of single crystals of simple y&apos; (Ni3Al), and forms the first step in a systematic program aimed at elucidating the mechanisms of hardening in the complex commercial alloys. 1) EXPERIMENTAL PROCEDURE Single crystals of off-stoichiometric NiA1 were grown from the melt under vacuum by a modified Bridgman method. The melt was poured into a preheated alumina mold and crystal growth was promoted from one end by gradient cooling. The crystals were homogenized by annealing in hydrogen at 2400° F for 72 hr followed by furnace cooling. Chemical analysis of samples taken from several crystals gave an average composition of 88.2 wt pct Ni. Spectrographic analysis gave as the principal impurities in weight percent— Si (0.02), Mg (0.01), Fe (0.02), Ti (0.002), Cu (0.008), and Co (0.03). Tensile specimens with specifications as in Fig. 1 were prepared by a series of operations involving electrical discharge machining, precision grinding, and electropolishing. Compression specimens with dimensions 1/4 by 1/4 by -3/4 in. were prepared in a similar manner, except for the initial shaping operation using a precision cut-off wheel/two-circle goniometer unit to give selected crystal orientations. Specimens were deformed in a Baldwin-Wiedemann testing machine with furnace attachment, using a strain rate of 5 x 10-4 sec-1. The strain measuring device consisted of extension arms attached to the tensile grips (or compression plattens) at one end and leading out of the furnace to an LVDT at the other. Temperature was controlled by a thermocouple placed in contact with the specimen. According to the known phase diagram for the Ni/A1 system,&apos; when an alloy of the specified composition is cooled from the melt, primary y (nickel solid solution) dendrites grow at the expense of the liquid phase, which becomes enriched in aluminum. At the eutectic composition the remaining liquid freezes as a two-phase mixture of y + y&apos; (Ni3Al). Upon further cooling, a solid state transformation occurs, involving the precipitation of y&apos; in the primary dendrites, and the complete transformation of the eutectic mixture to massive y&apos;. The as-cast structure consists, therefore, of y + y&apos; dendrites with interdendritic regions of massive y&apos;, i.e., transformed eutectic, Fig. 2. 2) DISCUSSION OF RESULTS 2.1) Stress-Strain Curves. Fig. 3 shows tensile stress-strain curves for crystals in orientations close to [001] deformed at temperatures from 70° to 2000°F. Both the yield stress and total elongation are strongly temperature-dependent. At 70°F, easy glide is absent, and the work hardening coefficient BIT - G/300. At T > 1500°F, the negative slope of the stress-strain curves is due to pronounced necking in the crystals. The yield stress maximum at 1500° F corresponds with a minimum in the ductility, Fig. 4. The extensive duc-

Jan 1, 1968

By F. B. Eiseman

IT is desired -to determine the effect of the extent of bank repairs on the final slag volume in acid electric steel-melting practice. It is understood that the repairs stud- TABLE I-Summary of Effect of Bank Repairs on Slag Volume [ ] ied here are necessary and the amount of sand added is that needed to maintain hearth and banks in a satisfactory condition. In this way the effect of repair materials on the amount of slag tapped would be found with a reasonable degree of accuracy. Ten heats were made for this study with careful attention to a uniform charge. The steel was the usual grade B and melting was carried out in a 3 1/2-ton top-charge Lectromelt furnace. Melting practice in all cases was the same-complete oxidation, with recarbonization by means of low-silicon pig iron.

Jan 1, 1947

By A. U. Seybolt

A FEW copper-zinc-base alloys meet die-casting requirements reason- ably well, although improvements are desired. Aluminum bronzes, high-tinbronzes and some copper-nickel-zinc alloys can be die-cast, accordingto Herb,1 but seldom are because of such factors as higher melting ranges and greater cost than certain of the brasses. Fox2 has summarized the copper-base die-casting alloys that were in commercial use in 1937 and has given the effects of different alloying constituents. Table 1 gives some of the properties of these alloys as reported by Fox. TABLE 1. Commercial Die-casting Brasses a Constituent Yellow Brass Low-silicon High-siliconb Brass Brass Nickel Silver Composition, Per Cent Cu 57-59 63-65 80 -81.5 42.0 Zn 40-42 33-35 13.5-16.0 41.0 Sn 0.5-1.5 Si 0.75-1.25 3.75-4.25 Pb 1.0 Ni 16.0 Properties Tensile, lb. per sq. in.. 55,000-60,000 65,000-70,000 85,000-95,000 85,000-95,000 Yield, lb. per sq. in.d.. 30,000-35,000 35,000-40,000 65,000-70,000 65,000-72,000 Elong., per cent in 2 in . 15-20 20-30 8-12 10-20 Brinell hardness 120-130 120-130 160-180 160 Specific gravity 8.47 8.50 8.15 8.45 Properties reported by Fox.2 b Trade name of Brastil, Doehler Die Casting Co., similar to Webert Alloy, 3,4 American Brass Co., and Tombasil Alloy,5 Ajax Metal Co. c Trade name Tinicosil, Titan Metal Manufacturing Co. Melting point (liquidus) of the yellow brass is given by Herb&apos; as 1650° F., of the high-silicon Brastil (with 4.5 to 5 per cent Si) as 1600° F., and of the nickel silver as 1675° F. d Criterion not stated.

Jan 1, 1939

By David T. Peterson

Calcium metal was found to deoxidize thorizcm at 1000° to 1200° C. The reaction kinetics were determilled and related to the diffusion coefficients of oxygen in thorium. The solubility of oxygen in thorium, the minimum oxygen concentration, and the diffusion coefficient were determined from 1000° to 1200°C. This firocess results in the lowest oxygen concentrations zohich have been reported for thorium metal. FOR many years it has been known that calcium metal will reduce thorium oxide to thorium metal. This reaction has been the basis for several methods of preparing thorium metal. From the equations giv-by Kubaschewski and vans, &apos; AF" for the reaction Cao, + Tho,(,) - CaO(,, + Th(,) was calculated and found to be -3.4 kcal at 1000°C, -2.5 kcal at llOO°C, and -2.0 kcal at 1200°c. Thorium is very slightly soluble in liquid calcium, and the solubility of calcium in solid thorium is very low. Consequently these metals would be in essentially their reference states. If thorium containing oxygen were equilibrated with liquid calcium between 1000° and 1200°C, the oxygen content of the thorium would have to be below the solubility limit in thorium. Oxygen is one of the impurities most difficult to remove from thorium and is the most abundant impurity in metal prepared by almost all known methods. Fortunately, oxygen does not have a large influence on the properties of thorium because the solubility in solid thorium is very low. EvenT in thorium containing 100 ppm of 0, particles of thorium oxide can be observed in the microstructure. In view of the incompatibility of thorium oxide and liquid calcium and the low solubility of thorium oxide in thorium, the deoxidation of thorium by this method was investigated. For thorium containing an amount of oxygen well in excess of the solubility limit, the reaction should proceed in the following sequence. The oxygen content of the thorium matrix near the surface would be depleted by the diffusion of oxygen to the surface. At the surface, the oxygen would react with calcium to form calcium oxide. To maintain equilibrium within the thorium, thorium oxide would dissolve to keep the matrix saturated. Consequently, the thorium-oxide particles would disappear first at the surface and then the particle-free rim would grow in thickness. If the rate-controlling step were the diffusion of oxygen through this layer of thorium which was growing in thickness in direct proportion to the amount of oxygen removed, the well known parabolic time law should be observed. If the oxygen concentration at the surface of the thorium and at the inner surface of the deoxidized rim were known, the diffusion coefficient of oxygen in thorium could be calculated from the parabolic rate constant. EXPERIMENTAL PROCEDURE The thorium metal used in this study was prepared by calcium reduction of ThF, by the method described by Wilhelm.&apos; The analysis of this metal is given in Table I. The carbon was determined by combustion, the oxygen by the HC1-insoluble residue method, nitrogen by the Kjeldahl method, and the other elements by emission spectroscopy. A section of this ingot was hot rolled at 600°C to 1/4 and 1/8-in. thick plates. Specimens approximately 7/8 in. square were cut from these plates, and all surfaces of the specimens were cleaned and smoothed by filing with a clean file. Individual specimens were placed in 1-in. diam by 2-in.-long tantalum capsules. Approximately 1 g of clean, high-purity calcium was placed in the capsules and an end closure arc-welded in place. The tantalum capsules were sealed in Inconel crucibles to protect the reactive metals from oxidation. The entire loading procedure was done in a glove box filled with pure argon. The loaded crucibles were placed in a muffle furnace, controlled within 2OC of the desired temperature, for a measured length of time. After the specimen had cooled to room temperature, it was sectioned perpendicular to the large faces and through the mid-point of two of the sides. The sectioned specimen was mounted and polished through Linde A abrasive. The rim which was free of thorium-oxide particles could be clearly observed microscopically as mechanically polished. Twenty measurements of the thickness of the rim were made at equally spaced points far enough from the end of the

Jan 1, 1962

By Hans Lundberg

BASED upon an instrumental improvement, a new development has taken place in the art of electrical prospecting, and some remarkable results have already been obtained with regard to potential exploration. In order to visualize the importance of this development, it is deemed advisable to review briefly the fundamental facts about potential surveys. Potential exploration may be carried out qualitatively or quantitatively. Qualitative investigations are made by determining and plotting on a map points of equal potential, whereby any anomalies are revealed, without, however, much clue to their magnitude. Quantitative investigations determine the variations of potential or potential drop, and thus show not only the location of the anomalies, but also their magnitude. Figs. 1 to 6 illustrate the influence of simple types of ground inhomo-geneities, assuming one effective exciter potential only. Such a condition can be closely realized by connecting an electric current source to two electrodes, one of which, is located at a great distance. Assuming uniform ground resistivity, the resultant potential distribution may be represented by concentric spheres. Any change from the normal condition causes a characteristic distortion of the spheres, which becomes different for different types of resistivity variation. The series of Figs. la to 6a illustrates schematically results of qualitative investigations and series 1b to 6b results of quantitative investigations. Figs. 1 and 2 picture the well-known case of local resistivity variations normally encountered in ore prospecting. Figs. 3 and 4 show the reactions caused by more or less vertical resistivity contacts and Figs. 5 and. 6 refer to the problem of ground-water and bedrock investigations where the resistivity contact is horizontal or nearly so. It is evident from Figs. 5a and 6a that qualitative measurements do not permit an identification of such general geological features as widespread horizontal strata, because the resultant contraction or expansion of the equipotential circles at the surface cannot be recognized without quantitative determinations. On the other hand, qualitative measurements are well suited for the exploration of local or lateral resistivity

Jan 1, 1931

By P. Marier, T. R. Ingraham

When cylindrical powder compacts of nickelous oxide (NiO) are heated in an equilibrated stream of SO3, SO,, and 02, in the temperature range 500°to 800°c, tlickelous suljate (NiSO4) is formed as an adherent layer on the oxide. The reaction is diffusion-controlled, with an activation energy of 13 ± 3 kcal per mole. When cylindrical powder compacts of NiSO4 are heated in a stream of dry nitrogen in the temperature range 1000 0to 11500C, NiO is formed at a well-defined interface between the sulfate and oxide. The interjhce migrates into the sulfate at a constant rate at a constant temperature and gas flow. The reaction rate increases with increasing gas flow and decreases with increasing partial pressure of SO3 in the gas stream. Resolution of the partial-pressure data with a Lang-itzliir Adsorption Isothern suggests that about 80 pct of the NiO interface is covered with SO3. The heat of adsovption is about 68 kcal per mole. The activation energy of the decomposition process is 61 ± 3 kcal per mole. MOST of the work reported on the formation and decomposition of nickel sulfate is related to thermodynamics.1-3 No quantitative work has been reported on the decomposition process. The only kinetic work reported on the formation is that by Fletcher and shelef.4-6 whose main purpose was to study the effects of alkali metal sulfate additions on increasing the rate of nickel sulfate formation. They found that, in the absence of an additive, only small amounts of sulfate were formed and the kinetic data were difficult to interpret. However, they suggested that the sulfa-tion of nickel oxide is a diffusion-controlled process for which the activation energy is approximately 17 kcal per mole.6 In this paper, both the formation and decomposition reactions will be examined; and based on the effects of temperature, flow rate, interfacial area, and partial-pressure of sulfur trioxide, mechanisms and activation energies will be suggested for both processes. EXPERIMENTAL Material. The nickel source material used in all experiments was Baker and Adamson Reagent Grade NiSO4. 6H2O, for which the following analysis was supplied by the manufacturer: C1, 0.001 pct; NO3, 0.005 pct; Co, 0.02 pct; Cu, 0.005 pct; Pb, 0.002 pct; Fe, 0.001 pct: insol, 0.005 pct. The anhydrous sulfate was prepared by heating the hydrate at 420°C in a muffle furnace for 5 hr. Nickel oxide was prepared by decomposing the sulfate at 950°C over a period of 10 hr. Method. The technique used for measuring the rates of formation and decomposition was developed earlier in these laboratories.7-8 The method is based on the observation that the kinetic parameters of a reaction can be established in a flow system, with specimens prepared by compacting powder to a uniform pellet shape. The results are identical with those established with solid polycrystalline specimens or single

Jan 1, 1967

US 4,133,866-Selective recovery of the bound sodium content of red mud obtained in the production of alumina by the Bayer process The red mud is mixed with aqueous ferric sulfate, the resulting suspension stirred intensively at a temperature of 15-85°C and adjusted to a pH value of from 4.4 to 4 6, and the solids are removed. The clarified solution of sodium sulfate can be used directly for the leaching of additional bauxite T Lakatos, M Miskei, J Szolnoki, F. Toth, and L Revesz, assigned to Aluminiumipan Tervezo es Kutato Intezet, Almasfuzitoi Timfoldgyar, and MTA Geokemiai Kutatolaboratorium. Jan. 9, 1979. 3 pp (423-208). Filed: 10¬28-77 (846,588) Priority: Hungary, 10-29-76 (AU 364). US 4,145,398-Continuous digestion of bauxite with aqueous sodium hydroxide, with higher throughput in existing plants or the construction of smaller plants with equivalent capacity The ore suspension at a solids concentration of 1-6% by weight and temperature of 200-300°C is flowed through a digestion tube or nest of tubes at a velocity of preferably from 2 to 5 m/s and under a pressure of from 10 to 200 atm Heat is supplied by a fluid heat carrier flowing in countercurrent in a concentric outer tube. Preferably, some of the red mud is recycled to the digestion operation. L. Plass, assigned to Vereinigte Aluminium-Werke A.G Mar 20, 1979. 5 pp. (423-121) Filed: 2-27-76 (754,749) Same: British 1,437,548, dated May 26, 1976 Same Canadian 1,008,253, dated Apr 12, 1977. US 4,146,573-An aqueous slurry of red mud, formed in the Bayer process production of alumina from bauxite, can be solidified by treating the red mud with a described quaternary ammonium salt, continuing mixing until the red mud has set up to a rigid mass, and recovering the solidified concentrated red mud J Kane, assigned to Nalco Chemical Co Mar 27, 1979 4 pp (423-82). Filed 8-2-78 (930,251).

Jan 1, 1980

Chairman James F. Kemp :—I call upon Prof. Albert Sau-veur to open the general discussion on the subject of sound steel ingots. Albert Sauveur, Cambridge, Mass.:—I believe that I have the privilege, this instant, of opening one of the most important, significant and far-reaching discussions ever held before this Institute. I believe that our talk this morning will be heard far and wide, not only on this side of the water, but also on the other side. Everywhere, in short, where steel is manufactured. I welcome the opportunity of expressing my mind in regard to the production of sound steel ingots, a subject about which I entertain Rome very decided opinions. I shall not attempt to discuss the relative merits of the various processes that have been described. I shall, on the contrary, confine myself to a general consideration of the important questions before us. So intensely do I feel regarding the production of sound steel ingots that I have put my remarks on paper in my desire to present my views. I have always remembered my astonishment, not to say dismay, some twenty years ago, when I beheld for the first time a steel ingot, a rail steel ingot, that had been split open from top to bottom. There was the pipe! There was an enormous cavity extending from a short distance from the top to nearly one-third of the length of the ingot; and when I was told that manufacturers seldom discarded more than one-tenth of the total length of the ingot it became evident to me that a large proportion of piped, and therefore, defective, or at least weak and dangerous, rails were manufactured; in fact, probably one rail out of six, nearly 17 per cent., of dangerous rails.

Jan 1, 1914

By Emma Smith, R. W. Guard

INVESTIGATION of the nickel-rich end of the Ni-Zr system has been prompted by an interest in the effect of small amounts of zirconium in high temperature alloys. Hansenl presents a hypothetical diagram based on the work of Allibone and Sykes,2 who investigated the system up to 44 atomic pct (55 wt pct) Zr by metallographic means. Since the alloys they used were melted in Alundum crucibles they were probably contaminated with appreciable amounts of aluminum. They found two compounds which they called Ni3Zr and Ni4Zr. Hayes, Roberson, and Paasche3 identified a compound NiZr (50 atomic pct Zr) with a melting point of 1470°C. Such a high melting compound is not compatible with the observation of Allibone and Sykes2 hat a eutectic is formed near 50 atomic pct. The alloys containing up to 60 atomic pct Zr were melted in an inert atmosphere in a noncon-sumable electrode arc furnace. Analysis of most of the alloys indicated negligible loss of zirconium. The alloys were examined in the as-cast condition and also after annealing for 6 hr at 1175°C (or 1000°C for the alloys between 25 atomic pct and 45 atomic pct). Metallographic specimens were etched using mixtures of HF-HNO3-H2O or acetic acid- HN0,-H,O. The specimens for the solidus determinations were wrapped in molybdenum foil and sealed in evacuated quartz tubes. Specimens to be heated above 1300°C were enclosed in zirconia tubes inside the quartz to prevent reaction with molybdenum. The solidus determinations were carried out by heating the specimens at various temperatures for a few minutes and then examining the interior structure metallographically to determine at what temperature melting began. The 150 mesh powders for X-ray analysis were annealed in an evacuated quartz tube for 2 hr at 540 °C to remove cold work. Alloys with 22.5 atomic pct Zr and 44.4 atomic pct Zr required annealing at 700 °C for complete recovery. The grains of both of these alloys were soft and rather ductile. Both Debye-Scherrer film patterns and spectrometer traces were made for each alloy using filtered copper radiation. Results and Discussion The presence of a substantial amount of second phase in an alloy with 1.1 atomic pct Zr indicated that the solid solubility of zirconium in nickel is somewhat less than 1 atomic pct. The a0 value for the face-centered-cubic matrix in the same alloy was equal to that of pure nickel, so that the solubility must be very small. This observation is as expected from the large atom size difference. Annealed specimens of alloys with 15.0, 16.7, 22.5, 28.6, 44.4, and 59.4 atomic pct Zr showed. micro-structures that were essentially single phase. When

Jan 1, 1958

By H. R. MacMichael

IN the Chihuahua district of Mexico the first smelting was that inaugurated by the early Spaniards for the production of silver bullion. The ores treated were high in silver and lead. Silver-lead bullion was first produced and the lead then cupelled to waste, with the slag produced running from 5 to 10 per cent in lead and about 25 to 40 per cent silica. The ore was mined by peon labor, often being carried out of the mine on the backs of the men, and then transported by burros. Furnaces were of primitive construction, adobe or rock being used in the earlier period and some iron later when it became available. Blast was originally supplied by bellows manually operated. Such smelting was carried on to a greater or lesser extent until the latter part of the last century, and so extensive was it that many hundred thousand tons of leady slag remained to be treated in modern furnaces. In 1908 a smelter was placed in operation at Chihuahua by the American Smelting & Refining Co. At that time the ore was practically all oxidized and by a little selection, self-fluxing mixtures could be made, but with an average lead content usually under 10 per cent and sometimes as low as 7 per cent. The bullion produced would carry from 150 to 300 oz. silver per ton. The slag made approximated 30 per cent SiO2, 42 per cent FeO, 21 per cent CaO, and perhaps 3 per cent Zn. The ores varied from hard, coarse material which was passed through a crusher, to a considerable quantity of fines which had to be smelted as it came, as crushing the coarse was the only preparation for smelting.

Jan 1, 1933

By D. T. Peters, C. R. Cupp

Aging of commercial 18 pct Ni maraging steel and of related binary, ternary, and quaternary alloys has been studied by electrical resistivity, X-ray diffrac-tion, and hardness measurements. The aging process is in three stages: 1) recovery of martensite; 2) two precipitation reactions; 3) formation of nickel- rich austenite. The main objective of this work was to discover the nature of the Co-Mu interaction. Addition of cobalt to the Fe-18 pct Ni-5pct Mo alloy results in acceleration of the pvecipitation reaction by increasing the super-sat~lration 0f molybdenum. The cobalt-containing al- loys show no incubation period for the precipitation reaction, but the alloy without cobalt shows an initial slow reaction. These results are interpreted in terms of precipitation on dislocations. At low aging temperatures, the presence of cobalt leads to the appearance of a second type of precipitate which is a particularly effective hardener. Cobalt was found to retard the formation of austenite. Overaging is a combination of classical overaging and the formation of austenite in the structure. he- activation energy for the precipitation reaction determined from resistivity ,measurements is 42.8 kcal per mole and the growth of the precipitate is found to obey at law at high tenzperatures and a tU3 law at low temperatures. HE mechanism of strengthening of the 18 pct Ni maraging steels has been studied extensively since 1962.&apos;-? The strengthening is due to precipitation hardening of the martensitic matrix. The main precipitate is an inter metallic compound involving molybdenum, but there is disagreement about its identity.

Jan 1, 1967

By N. A. Tiner, Saara Asunmaa

The early stages of nucleation of vacuunz-deposited gold coatings on electropolished surfaces of pure nickel and binary alloys of Ni-A1 and Ni-Ti have been studied, employing carefully controlled temperature and vacuum conditions. The preferential nucleation of gold on slip-plane edges on the crystal surfaces gave rise to a very pronounced decoration effect which was used in studying the morphology of the pain boundaries, etch pits, and slip planes on crystal faces. Characteristic surface patterns were observed with local dimensional variations. Most pronounced geometric patterns were ohserved in the pain boundaries of nickel and on the crystal faces of Ni-A1 alloy. The nucleation behauior of gold indicates contamination on the Ni-T1 alloy and the getter properties of titanium are presented as a tentative interpretation for the detected contamination. The markings and imperfections on cleavage surfaces of crystals have long been observed by optical microscopy.1,2 Surface-replica techniques are also used to detect the smallest steps and structural details on crystal surfaces by electron microscopy. Recently, Bassett3-5 and Sella, Conjeaud, and Trillat 6 have shown that, when gold is deposited onto a rocksalt cleavage surface, there is preferential nucleation at steps and slip-plane edges on the crystal surface. This gives rise to a very pronounced decoration effect which is invaluable for revealing the lattice steps on a cleavage surface. According to Bassett,3 gold atoms arriving during vacuum evaporation at the crystal surface have a certain mobility on the surface after arrival, particularly at elevated temperature. If a significant

Jan 1, 1964