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By A. S. Appleton, M. B. Bever, G. E. Dieter

A gold-silver alloy was deformed by explosive loading at shock pressures up to 510 kbars. The stored energy and hardness increased over the whole range of pressures; the largest rates of increase were observed between 120 and 150 kbars. In this range, markings rkavacteristic of defornation twins first appeared; higher pressures produced markings in all grains. These effects are compared with those of conventional deformation processes and are discussed in relation to probable structural changes. In recent years, increasing efforts have been devoted to the investigation of the effects produced in metals by the passage of high-intensity shock waves of explosive origin. By properly utilizing the energy released by the detonation of a high explosive, it is possible to generate pressure pulses of the order of 500 kbars and higher. (One kbar equals l0 9 dynes per sq cm or approximately 1000 atm.) The passage of a shock wave through a metal occurs at pressures which are very much greater than the yield strength. As the shock front passes a point in the metal, the pressure rises almost instantaneously, and continues to act at the point for a few microseconds. Thus, metals subjected to explosive shock loading experience a nearly instantaneous increase in pressure, and a subsequent release of pressure, which is almost as rapid. Under these conditions mechanical twinning and shear transformations occur readily. smith1 has investigated the metallurgical changes in copper and iron resulting from exposure to explosive shock waves. He found an appreciable increase in hardness in both metals. In copper, a hardness greater than that resulting from 95 pct reduction in thickness by rolling was obtained, yet in the explosive deformation, the thickness of the specimen decreased only a few percent. After explosive loading, the micro-structure of copper showed markings characteristic of mechanical twins. The amount of stored energy resulting from explosive loading is of interest. Measurements of the stored energy of cold work as a function of strain, temperature, strain rate, and composition have been made with gold-silyer alloys deforyed by rolling, orthogonal cutting,3 drilling,4 filing, wire drawing, and torsion. The investigation reported here was also carried out with a gold-silver alloy and its results can be compared with those for the deformation of this alloy by more conventional methods. EXPERIMENTAL PROCEDURES An alloy containing 82.6 wt pct Au and 17.4 pct Ag was purchased in several batches from Handy and Harman Co., New York, as annealed rod 1/4 in. dim. The rod was cold-rolled to a sheet approximately

Jan 1, 1962

By J. D. Miller, M. Misra

The processing strategy for the effective separation of bitumen from low grade (<l0 weight percent bitumen) Utah tar sands by a hot water process differs significantly from that used for the processing of high grade (> 10 weight percent bitumen) Utah tar sands. Excellent separations (coefficient of separation = 0.9) can be achieved for high grade Utah tar sands by intense hot water digestion followed by a modified froth flotation step. Such a technique is ineffective for low grade tar sands. In order to change the characteristics of the low grade tar sand an attempt was made to enrich the bitumen content of the feed to greater than 10 weight percent by recycle of bitumen concentrate to the digestion stage. However, the quality of the separation was not improved under these circumstances. Similarly feed enrichment by heat treating the low grade feed with recycled concentrate prior to digestion did not improve the separation. More successful separations of low grade Utah tar sands were finally achieved by modification of the viscosity of the low grade bitumen with controlled addition of diluent. These results of the hot water separation tests and variations in the quality of separation are interpreted in terms of the physical properties of the bitumen and the surface bonding forces operative at the bitumen-sand interface.

Jan 1, 1981

By F. E. Harris

It has been said that carbon is "ubiquitous" with reference to iron alloys. Certainly at temperatures where carbon and iron form the solid solution, austenite, it may be readily added to, or removed from, steel surfaces. Differences in concentration potential are the sole requirements for carbon flow. To measure the rate of carbon flow, a proportionality factor, D, is arbitrarily expressed in units of (length)2 X (time)-&apos;. If the term used for carbon concentration is weight Pet C, as is customary, then a factor must be found, changing this term to One of weight Per unit volume when the diffusion coeficient, D, is used in flow formulae. The determination of D values for carbon is complicated since D varies with the concentration itself. The Matano method has often been employed for systems involving a variant D. This method expresses all evaluation of unsteady flow whereby D is given a relationship with the numerical value of C-x slopes. The author contends that this solution is incorrect, except when D is invariant. The primary purpose of this paper is to support this contention. Here diffusion is controlled under two conditions of flow. The first part deals with the steady state; the second part considers unsteady flow under definite restrictions. Beginning with the fundamental concept, the development is continued until equations for C-x curves are obtained. The solution is then subjected to experimental data. It is realized that a great amount of reliable data is required for a rigorous proof. KO such research is claimed. Instead an attempt is made to set forth the physical significance of the diffusion mechanism, and particularly to express the factors which influence the flow of carbon in austenite. Of equal significance is the implication that gaseous media may be employed with reasonable accuracy in making these determinations. The Steady State Diffusion of Carbon in Au~tenite The fundamental experiment defining diffusion in solid metals may be readily performed for carbon in gamma iron.&apos; For this experiment a thin plate of medium carbon steel is chosen. The surfaces of this plate may be taken as two parallel planes which may be considered infinite for points well in the Center of the planes. These two planes are held at different concentrations of carbon at a constant temperature. This temperature, 1700°F for example, is one where the single phase: carbon in solution with gamma iron, exists. When these conditions are held for a sufficient time the concentration of carbon of the different points of the solid ment down towards its steady state value. At points well removed from the ends, the concentration will remain the Same along planes parallel to the surfaces of the plate.

Jan 1, 1948

By F. E. Harris

It has been said that carbon is "ubiquitous" with reference to iron alloys. Certainly at temperatures where carbon and iron form the solid solution, austenite, it may be readily added to, or removed from, steel surfaces. Differences in concentration potential are the sole requirements for carbon flow. To measure the rate of carbon flow, a proportionality factor, D, is arbitrarily expressed in units of (length)2 X (time)-&apos;. If the term used for carbon concentration is weight Pet C, as is customary, then a factor must be found, changing this term to One of weight Per unit volume when the diffusion coeficient, D, is used in flow formulae. The determination of D values for carbon is complicated since D varies with the concentration itself. The Matano method has often been employed for systems involving a variant D. This method expresses all evaluation of unsteady flow whereby D is given a relationship with the numerical value of C-x slopes. The author contends that this solution is incorrect, except when D is invariant. The primary purpose of this paper is to support this contention. Here diffusion is controlled under two conditions of flow. The first part deals with the steady state; the second part considers unsteady flow under definite restrictions. Beginning with the fundamental concept, the development is continued until equations for C-x curves are obtained. The solution is then subjected to experimental data. It is realized that a great amount of reliable data is required for a rigorous proof. KO such research is claimed. Instead an attempt is made to set forth the physical significance of the diffusion mechanism, and particularly to express the factors which influence the flow of carbon in austenite. Of equal significance is the implication that gaseous media may be employed with reasonable accuracy in making these determinations. The Steady State Diffusion of Carbon in Au~tenite The fundamental experiment defining diffusion in solid metals may be readily performed for carbon in gamma iron.&apos; For this experiment a thin plate of medium carbon steel is chosen. The surfaces of this plate may be taken as two parallel planes which may be considered infinite for points well in the Center of the planes. These two planes are held at different concentrations of carbon at a constant temperature. This temperature, 1700°F for example, is one where the single phase: carbon in solution with gamma iron, exists. When these conditions are held for a sufficient time the concentration of carbon of the different points of the solid ment down towards its steady state value. At points well removed from the ends, the concentration will remain the Same along planes parallel to the surfaces of the plate.

Jan 1, 1948

By Van Der Muelen P. A.

SOME time ago, the writer received from W. 0. Borcherdt, Manager of the, works of the Bertha Mineral Co. at Austinville, Va., several specimens of a dense yellowish slag-like material, containing cavities showing clear needle-like crystals, and representing a product formed by the fumes of zinc oxide and basic lead sulphate from the oxide furnace, attacking the firebrick lining of the flues. The matrix, which is of a greenish-yellow color, is made up chiefly of an amorphous glass, carrying numerous crystals, the latter being well-defined, clear, and transparent, but colored a very light yellow by small amounts of ferric oxide. A number of the crystals were carefully separated from the matrix and tested with the blowpipe. They have a fusibility of about 2, yield a globule of lead and a coating of lead oxide before the blowpipe on charcoal, and contain some zinc. Their hardness is 5 to 6. 1 Fig. 1. Under the microscope the crystals appear to be made up of a prism, with narrow faces, and a fairly large pinacoid, but unfortunately show no terminal faces (Fig. 1). Between crossed nicols they gave parallel extinction in. the three planes containing the crystallographic axes, and are therefore orthorhombic. The index of refraction is high. A number of the best crystals were measured on the reflection goniometer, the angles given below representing the average of measurements made on different individuals. mm = 46° 52&apos; mb = 66° 34&apos; a:b:c = 0.4334:1 :?

Jan 5, 1917

By C. E. MacQuigg

In this paper it is impossible to more than touch on many of the commercial alloys of iron, chromium, and carbon, therefore the discussion is confined to the properties of some of the less well-known alloys with upwards of 20-per cent. chromium. The discussion has been based largely on the strictly engineering aspects of the alloys. Chromium has well-defined effects when added to the iron-carbon system. These effects depend on the amount of chromium added and on the composition of the iron-carbon alloy to which the addition is made, i.e. whether low- or high-carbon steel, cast iron, etc. In the case of the low-carbon steels, the chromium addition, when not in excess of several per cent., appears to exert an influence on the properties by its influence on the critical range. In the higher chromium alloys, the physical properties are influenced chiefly by the formation of new complexes, such as iron-chromium solid solutions and, with higher carbon contents, iron-chromium carbides of great hardness. Examination of the published data1 on the critical range phenomena of chromium-bearing steels up to several per cent. chromium indicates an agreement on the following points:

Jan 1, 1923

By C. E. MacQuigg

In this paper it is impossible to more than touch on many of the commercial alloys of iron, chromium, and carbon, therefore the discussion is confined to the properties of some of the less well-known alloys with upwards of 20-per cent. chromium. The discussion has been based largely on the strictly engineering aspects of the alloys. Chromium has well-defined effects when added to the iron-carbon system. These effects depend on the amount of chromium added and on the composition of the iron-carbon alloy to which the addition is made, i.e. whether low- or high-carbon steel, cast iron, etc. In the case of the low-carbon steels, the chromium addition, when not in excess of several per cent., appears to exert an influence on the properties by its influence on the critical range. In the higher chromium alloys, the physical properties are influenced chiefly by the formation of new complexes, such as iron-chromium solid solutions and, with higher carbon contents, iron-chromium carbides of great hardness. Examination of the published data1 on the critical range phenomena of chromium-bearing steels up to several per cent. chromium indicates an agreement on the following points:

Jan 1, 1923

By D. E. Peacock, B. Harris

The mechanical behavior of a niobium (columbium)TUNG alloy containing 20 wt pet Ta. 15 wt pet W, and 5 wt pct Mo has been studied in the temperature range 77° to 423°K. All specitrzens tested, apart from those into which oxygen was introduced deliberately, were fully recrystallized at 1500°C, had an average grain diameter of approximately 0.03 mm, and a combined carbon, ox-vgen. nitrogen, and hydrogen content of not not more than 250 ppm The meckatnical behavior of this alloy was found to be similar in seine respects to that of unalloyed bcc transilion metals. Both yield and flow stresses were sensililae to changes in deformation rate and both increased rapidly as the temperature was lowered below 150°C. A detailed examination revealed, however, that most of the temperature dependencc of the yield stress could be accounted for by the temperature dependence of the elaslic, modulus, whish is not true of the unualloyed metals. In lension at moderate strain rates, the trunsition fvom ducfile to hvittle behavior occurred just belour room teunperature bur incveasing the oxygen content from 190 to 200 pptn raised the transition temperature to about 4000K. TUNGSTEN and molybdenum have been found to be very effective high-temperature solid-solution strengtheners of niobium, but the amounts of these elements that can be added are limited if the alloy is to retain useful room-temperature ductility. It has been shown, however, that partial replacement of niobium with tantalum lowers the ductile-to-brittle transition temperature of such alloys and allows larger additions of molybdenum and tungsten to be made. Some of the high-temperature properties of niobium alloys containing these elements have been reported by Bartlett et al.,&apos; and the work presented here describes the low-temperature behavior of one of these, a solid-solution alloy containing, by weight, 20 pct Ta, 15 pct W, and 5 pct Mo. The elastic modulus, the temperature and strain-rate dependence of the yield and ultimate tensile stresses, and strain-hardening effects are discussed and compared with those of unalloyed niobium. EXPERIMENTAL MATERIAL AND PROCEDURE The material used in this investigation was produced from a 6-in.-diameter, double arc-melted ingot. This was can-extruded at about 1150°C to a 3-in.-diameter billet, and after annealing for 1 hr at 1345°C the billet was heated to 1315OC and part rolled and part forged to 0.5-in.-thick plate. The resulting material exhibited a cold-worked structure

Jan 1, 1965

By S. F. Shaw

The Sierra Mojada mining district is situated in western Coahuila, about 8 km. east of the Chihuahua state line, and about one-half way from the northern to the southern extremity of the state. It is at the terminus of the Mexican Northern R. R., 125 km. northeast of Escal6n, Chihuahua; also about, 240 km. due west of Monclova, Coahuila. The altitude is approximately 1500 m. above sea level. The Sierra Mojada valley is about 10 km. long, from east to west, with a width of 1 to 2 km. It is approached from the east through the Puerto del Oro, where the Mexican Northern R. R. enters the valley; the slope from west to east is gentle. The Sierra Mojada, of which about 300 m. is an almost vertical wall, bounds the valley on the south side; on the north side, the slope to the crest of Sierra Planchada is more gradual, rising only 200 or 300 m. above the valley. Water is relatively scarce in the district, and there are no running streams. The rainy season, usually beginning at the middle of June, lasts through July, and occasionally into August or September. In some years the rains fail entirely. The slope of the ground is such that nearly all the water immediately runs off. The arroyos along the flanks of the mountains are not very deep, but in heavy rains, sometimes approaching cloudbursts, a tremendous volume of water rushes down them, carrying large boulders. A certain amount of seepage collects in the agglomerate, lying below the conglomerate, and is retained in the local fractures. Some shallow wells have been sunk in this agglomerate, and one well over 150 m. deep was sunk on the Volcan ranch, supplying about 76 1. (20 gal.) per min. A considerable supply of water is collected in large earth reservoirs in and below the town of Esmeralda. In ordinary years this supply will last until January or February, after which the Volcan well has to be depended on until the next rainy season. Vegetation is scarce, aside from scanty scrub oak and other brush in the mountains, and a few mezquite, locust, pepper, and cottonwood trees

Jan 1, 1923

By S. F. Shaw

The Sierra Mojada mining district is situated in western Coahuila, about 8 km. east of the Chihuahua state line, and about one-half way from the northern to the southern extremity of the state. It is at the terminus of the Mexican Northern R. R., 125 km. northeast of Escal6n, Chihuahua; also about, 240 km. due west of Monclova, Coahuila. The altitude is approximately 1500 m. above sea level. The Sierra Mojada valley is about 10 km. long, from east to west, with a width of 1 to 2 km. It is approached from the east through the Puerto del Oro, where the Mexican Northern R. R. enters the valley; the slope from west to east is gentle. The Sierra Mojada, of which about 300 m. is an almost vertical wall, bounds the valley on the south side; on the north side, the slope to the crest of Sierra Planchada is more gradual, rising only 200 or 300 m. above the valley. Water is relatively scarce in the district, and there are no running streams. The rainy season, usually beginning at the middle of June, lasts through July, and occasionally into August or September. In some years the rains fail entirely. The slope of the ground is such that nearly all the water immediately runs off. The arroyos along the flanks of the mountains are not very deep, but in heavy rains, sometimes approaching cloudbursts, a tremendous volume of water rushes down them, carrying large boulders. A certain amount of seepage collects in the agglomerate, lying below the conglomerate, and is retained in the local fractures. Some shallow wells have been sunk in this agglomerate, and one well over 150 m. deep was sunk on the Volcan ranch, supplying about 76 1. (20 gal.) per min. A considerable supply of water is collected in large earth reservoirs in and below the town of Esmeralda. In ordinary years this supply will last until January or February, after which the Volcan well has to be depended on until the next rainy season. Vegetation is scarce, aside from scanty scrub oak and other brush in the mountains, and a few mezquite, locust, pepper, and cottonwood trees

Jan 1, 1923

By F. J. Norton

THE object of this investigation was to make a comprehensive study of the degassing of molybdenum in order to determine how rigorous a treatment was necessary to completely, remove sorbed gases from molybdenum electrodes in vacuum tubes. Some work has also been done with tungsten, nickel and carbon. As a logical development of this work it has been shown that the gas is present throughout the body of the metal and a study has been made of the solubility of nitrogen in molybdenum and tungsten and the rate of diffusion of nitrogen through molybdenum has been calculated. Tests were made on molybdenum from all the commercial sources and no difference was discovered in the nature of the gases present, the amounts or the ease of removal. The reason for this was apparent when a study was made of the manner in which gases are absorbed by gas-free molybdenum. It is necessary to heat molybdenum to 1760° C. in a vacuum of the order of 0.001 micron for a time which varies lineally with the thickness, in order to obtain a condition in which no further gas is evolved by the sample. A sample so degassed can be handled and sub-sequently assembled in a tube and then degassed readily. The gases obtained from molybdenum are carbon monoxide and nitrogen, the nitrogen being the more difficult to remove..

Jan 1, 1932

NEW MEMBERS The following list comprises the names of those persons who became members during the period of May 10, 1917, to June 10, 1917. ANDERSON, JAMES P.,-Mgr. of the Mines of the Ringwood Co., 50 Church St:, New York, N. Y. BAKER; THOMAS C., Mine Supt., Cia. Santa Gertrudis, S. A. Pachuca, Hidalgo, Mexico. - BARCUS, W. J.. E., Min. Engr., Mining and Metallurgical Dept., General Chemical Co., 25 Broad St., New York,. N. Y. . BENNETT, GEORGE N.,.Min. Engr., Butte & Superior Mining Co., 616 West Gold St., Butte, Mont. BROCKMANN, GUILLERMO, Banker, Gmo. Brockmann & Co., Room 3115, 120 Broadway, New York, N. Y. BROWN, CLYDE L Mining, Box 703, Goldfield, Nev. BRUNSKOG, CARL W., Draftsman, Consolidated Arizona Smelting Co., Humboldt, Ariz. BURRELL,. OSSIAN C Mgr., American Zinc Co. of Tenn., Mascot, Tenn.

Jan 7, 1917

By Frank H. Riddle, Wilfrid R. Foster

GENERAL treatment of the various minerals of importance in refractories appears in the chapter entitled "Refractories" elsewhere in this volume. The present chapter is restricted to a discussion of minerals of the sillimanite group and brings up to date the excellent information contributed by Prof. Paul F. Kerr to the first edition (1937). Since the appearance of that edition, the status of the group has changed some- what. Kyanite remains the preferred source material for mullite refractories but total consumption of kyanite has increased considerably.85 The exigencies of World War II forced an increased dependence on domestic sources and led to an intensification of the search for higher-grade deposits of kyanite and allied minerals. The first discovery of massive kyanite similar to that of India has been reported from Georgia.37 British East Africa has joined India as a substantial supplier of our imported kyanite, but that from India continues to hold preference.85 During World War II, prices of both domestic and foreign grades reached peaks unparalleled since the earliest years of the use of kyanite and as yet have shown no tendency to return to prewar levels. Topaz, by virtue of the deposit outlined in South Carolina, merits inclusion in the group.20,36,95 Large andalusite deposits, which threaten to rival our one large domestic occurrence, have been found in Russia.69,88 Sillimanite has not yet attained an important position among these useful minerals because of the lack of accessible deposits of high-quality material in adequate supply.37,50,58 Tests by the Bureau of Mines have indicated the possibilities of economically beneficiating low-grade sillimanite and kyanite.105.106,140 Government, university, and industrial

Jan 1, 1949

By P. G. Chamberlain, E. R. Podnieks, R. E. Thill

Although published data on the physical properties of rock are voluminous, information is often lacking on the environmental conditions under which such data were acquired. Efforts are frequently directed to improve specimen tolerances and preparation procedures; but investigators often overlook giving the rock environment equally careful control during the testing program. Generally, tests are conducted at existing laboratory room conditions, and the prepared rock specimens are frequently, if not most commonly, air-dried for various lengths of time before testing. The standard testing atmosphere recommended by the American Society for Testing & Materials (ASTM)1 is 73.4°F and 50% relative humidity. To maintain a rock at 50% relative humidity for testing purposes, however, requires special equipment and preconditioning procedures, as this study demonstrates. Relatively small variations in the moisture content of a specimen, for example, due to the coolants or lubricants used during specimen preparation, can cause significant variations in the physical properties measured. Such moisture variations may occur in the rock specimen even after it is air-dried, since laboratory humidity conditions commonly fluctuate from day to day. For these reasons, this study emphasizes procedures for preconditioning and maintaining a controlled environment during testing. Although the effects of moisture or temperature on rock properties have previously been studied, their combined effect on rock properties is unknown. In this study, uniaxial compressive strength, Young&apos;s and stiffness moduli, and longitudinal wave velocity were determined and compared under controlled conditions of temperature, moisture, and pressure for 11 environments considered to be of particular interest in laboratory, in-situ, and even simulated lunar environments. The following environments were selected for this program: -250°F under dry, 50%

Jan 1, 1972

By H. F. Yancey, O. L. Furse

For several years the Bureau of Mines at its Northwest Experiment Station, in cooperation with the Mines Department. of the University of Washington, has been studying the breakage and degradation of coal. The first phase of the study was devoted to the determination of the friability of many coals of various ranks and comparison of various methods for estimating friability.&apos; A study of the relative ease or difficulty with which various coals are reduced to the fine size required for use as pulverized fuel followed the completion of this work. Baltzer and Hudson2 list twelve research organizations in the United States, two in England, one in Germany and one in Canada that are reported to be engaged on this problem; showing the general appreciation of the need for a simple method of estimating the grindability of different coals. Hardgrove,3 ho has advanced a method for estimating grindability, points out that pulverizer tests of different coals are incomplete and unsatisfactory. He compares such tests to that of a boiler test made without knowledge of the calorific value of the coal. Frisch arid Holder4 also stress the same point. They state that,

Jan 1, 1934

By A. B. Kinzel

INCLUSIONS of nonmetallic matter have long been recognized as objectionable in steel. A complete theory of the effect of inclusions, which is consistent with that held today, was outlined in Howe&apos;s early work on the metallurgy of iron and steel. This, by analogy with wrought iron, assumes that the observed difference in properties between specimens with and across the direction of rolling is due to slag enclosures. The fact that wrought iron shatters in ballistic test is taken as an indica-tion of the effect of inclusions on the resistance to shock. Since that time, the development of the metallurgical microscope has shown the discrete nonmetallic inclusions in the iron matrix. Better resolution has, brought out the great number of inclusions, and the availability of good microscopes in steel mills and laboratories has constantly drawn more attention to these inclusions. This recent emphasis on inclusions has resulted in studies as to their nature, mode of formation and methods of elimination, such as the work of Wohrman, Dickenson, Herty, and Schenk. In addition to the published works; many investigations which have not been published&apos; have been carried out by private laboratories and have resulted in the application of specifications intended to limit inclusions in many qualities of steel. Nevertheless, a clear understanding of the quantitative effect of inclusions on the physical properties of steel has been lacking. It is the specific purpose of this study to determine the quantitative effect of inclusions on the physical properties of steel that determine its behavior under dynamic stress. The study has shown that a quantitative relation between counted inclusions and impact strength does exist in normalized steels, but &apos;that factors other than readily visible inclusions are equally important. Furthermore, the present commercial rating of inclusions is unreliable with respect to counted inclusions or dynamic tests, and this study indicates that the tensile-impact test is more reliable as a measure of quality.

Jan 1, 1931

By J. B. Reed, T. A. Read, H. Rosenthal

Although the season cracking of brass has been a subject of experimental investigation for more than thirty years, the mechanism that is responsible for this phenomenon is still obscure. While at- tempts to elucidate the stress-corrosion cracking of some alloys have been relatively successful, the principal accomplishments made in the studies of the season cracking of brass have consisted of improved techniques for the fabrication of articles of alpha brass, which reduce the danger of season-cracking failure in service. The primary purpose of the present paper is to collect the published experimental data which appear to be of importance to the development of an adequate theory of the mechanism of the season cracking of brass. Some of the possible mechanisms which have been proposed will also be discussed, together with some promising avenues of future attack on the problems. Several excellent survey papers on season cracking are available, including the recent ones by Croft and Sachs(1)2 and by Gibbs(2). The principal facts concerning season cracking, as presented in these papers, may be summarized as follows. The season cracking of alpha brass is a special type of stress-corrosion failure, which may occur in atmospheres containing ammonia, air, and water vapor. The stress causing failure may be either the

Jan 1, 1945

By T. G. Digges, C. L. Vold, M. R. Achter

A study was made of the effect of the growth conditions on the perfection of single crystals of niobium (columbium). Dislocation densities, determined by means of double-crystal diffractometer measurements , were not greatly affected by the method of crystal preparation but could be reduced by annealing treatments. However, the size, sharpness, and tilt angles of the substructures, observed with X-ray reflection macrograph, were sensitive to variations in growth procedures as well as to subsequent thermal treatments. Although the dislocation density was the same in both types, there were more low-angle bound-aries in crystals grown by zone melting than in those prepared by strain anneal. Mechanisms to account for these observations are discussed in terms of dislocation movements. A planned study of the structure-sensitive properties of refractory metals required the use of single crystals of a high degree of structural perfection and, for ease of handling, of large cross section. It appeared that the strain-anneal technique could satisfy both of these requirements. First, crystals grown in the solid state have been reported to be more perfect than those obtained from the melt.&apos; Second, the diameters of rods which may be produced by zone melting should have a theoretical limit determined by specific gravity, thermal conductivity, and surface tension, while the diameter of strain-annealed rods is limited only by practical considerations. Previously it was shown that niobium (columbium) single crystals of 1 in. diam2 may be grown by strain anneal, compared to the 0.5 in. maximum diameter achieved by zone melting, as reported for molybdenum by Belk.3 The current research was undertaken to investigate and optimize the effect of various process variables on the perfection of 1/4 and 1/2-in.-diam niobium single crystals grown by strain annealing and to compare their perfection to those grown by zone melting. Characterization of these crystals was more conveniently accomplished by means of X-ray than by metallo-graphic techniques. EXPERIMENTAL PROCEDURE Specimen Preparation. Zone-melted crystals of 1/4 in. diam were produced by the standard electron-beam zone-melting technique. The swaged and cleaned rods were outgassed, in the solid state at a temperature near its melting point, at a rate of 12 in. per hr, and single crystals were grown by making two molten passes at 2 in. per hr. By maintaining a zone length of 4 to % in., very uniform single crystals several inches long were obtained. For the strain-annealed crystals, an induction heater was used, in preference to other types of heating, to take advantage of the good penetration of large sections. A five-turn coil, 1 in. long, operating at 10 kc and powered by a motor generator, was contained in a vacuum chamber. The rod, suspended from the upper end, was raised through the coil for both recrystallization and crystal growth. In preliminary work single crystals of the same material were also grown with single and multiturn coils powered by a 450-kc generator. A vacuum of 2 X 10-6 Torr was maintained at temperatures up to 2400°C. Starting with electron-beam-melted ingots of 21/2 in. diam, the analysis for which is given in Table I, the material was cold-swaged to the desired cross section of 1/4 and 1/2 in. diam and then recrystallized. The rods were then strained in a tensile machine and converted to single crystals by passing through the induction coil. As with zone melting, control of orientation is possible by the use of special procedures. Other investigators, see for example Williamson and smallman,4 have reported that orientation control may be achieved by a bending technique. In the present work the strained rod is partially lowered through the coil to start the growth of the crystal. Then it is removed and bent at a point in the poly crystalline portion. Finally, it is returned to the chamber and growth is continued "around the corner". This procedure has certain limitations. If the bending operation exceeds the critical strain, recrystallization may take place. Also, the amount of bending which can be imparted to the rod is limited by coil geometry, and up to now has been 10 deg. However, by repeating the bending and growing operations it should be possible to attain any desired orientation. In preparation for X-ray examination, single crystals were sectioned and planed by means of the spark-erosion technique. To obtain the maximum reflected intensity, the (110) plane was exposed for examination. They were then etched 3 to 5 min in a mixture of con-

Jan 1, 1967

By B. D. Crawford, S. A. Falconer

ONE of the outstanding achievements in connection with this country&apos;s war efforts has been the ability of our mining industry to supply from domestic sources many of the minerals of strategic importance that formerly were obtained principally from abroad. In order to meet the war-born demands for these scarce minerals, it has frequently been necessary to develop special methods for treating ores and waste products hitherto considered too low-grade to be workable; and to improve the efficiency of older beneficiation processes. Important in this respect have been the recent technological advances in the field of froth flotation of nonsulphide minerals. Because of the refractory nature of many of these domestic ores, and, in many cases, the limited available technical data regarding their treatment, much research work has been necessary. The following examples describe the procedures and reagents used, and the results obtained, in certain laboratory flotation investigations conducted by American Cyanamid Company&apos;s engineers at the Cyanamid Ore Dressing Laboratory on ores containing such minerals as scheelite, manganese oxides and carbonate, ilmenite, brookite, kyanite, garnet, spodumene, mica, feldspar, celestite, fluorite, chromite, corundum, and cassiterite. In presenting these data, we wish to point out that many of the minerals listed have previously been tested, and their amenability to flotation reported, by other investigators-notably those of the United States Bureau of Mines. In some instances the procedures and reagents used in the treatment of some of the following described ores follow rather well-established lines, and with one or two exceptions, the reagents used were well known. However, many of the ores tested did not respond well to simple conventional procedures and it was necessary to adopt special methods of conditioning and desliming, reversal of the usual order of floatability of some of the minerals, multiple cleaning, etc., in order to secure separations. Except where otherwise noted, all numbered and trade-marked reagents mentioned in this paper are marketed by the American Cyanamid Co. or the American Cyanamid and Chemical Corporation. TUNGSTEN ORES Tungsten minerals, vitally important in the war industries of the United States, rank high in the list of those we formerly had to import in order to supply our needs. Most of our domestic ores of tungsten contain scheelite as the valuable mineral. Today there are in the neighborhood of twelve tungsten operations in this country where flotation is used as the main or accessory form of benefication. It has, of course, been known for some time that scheelite and other tungsten minerals respond to treatment by flotation.

Jan 1, 1944

By M. I. Jacobson, A. S. Yue, A. E. Vidoz, F. W. Crossman

An equation governing the concept of constitutional supercooling under the combined effect of concentration and temperature gradients was used to produce platelike Al-CuAl2 eutectic composites for mechanical properties studies. Compression specimens were prepared from a single-colony Al-CuA12 eutectic composite ingot, 2 in. in diam and 12 in. long. The specirrzens were cut such that the platelets were oriented parallel, 45 deg, and perpendicular to the compression direction. Since the ingot was of eutectic composition, The aluminum-rich matrix could dissolve 5. 7 wt pct Cu in solid solution, and therefore could be strengthened by precipitation hardening. Specimens were tested at room temperature and elevated temperatures in the unidirectionally solidified, solution-treated, and solution-treated plus aged conditions. The results were compared with those for the conventionally cast and extruded specimens. For the controlled material, the highest strengths were obtained with platelets oriented parallel to the compression axis. In the unidirectionally solidified condition, 0.2 pct offset yield strength was 32,000 psi; however, this was increased to 59,000 psi by solution treatment, and further increased to 90,500 psi by solution treatment and aging. The attainment of high compressive strengths in the Al-CuAl2 eutectic composites was interpreted in terms of the buckling of elastic CuAl2 platelets in the plastically deformed a aluminum matrix. SINCE the discovery of high-strength whiskers,&apos; scientists and engineers have made significant progress toward incorporating these whiskers into metallic matrices, forming composites for basic studies and structural application. The general procedure is to produce the whiskers first and then to bind them together with a ductile matrix. The production of whisker-reinforced composites requires tedious handling techniques,, particularly when it is desired to align the whiskers unidirectionally. Furthermore, the interfacial bond between the whisker and the matrix is frequently poor3 so that the resulting composite has strengths lower than expected. These disadvantages are generally true for any metallic composite produced by physically mixing the components. It is possible to eliminate these shortcomings by growing whiskers directly in the matrix material by eutectic solidification.4-8 In eutectic solidification, the matrix phase and a whisker phase are grown approximately simultaneously from a liquid of the same overall composition at the eutectic temperature. If the solidification process is controlled by varying the freezing rate, the temperature gradient, and the impurity content, platelike or filamentlike whiskers are produced parallel to the growth direction. The morphology of the grown-in reinforcement, i.e.. plates or rods, generally depends on the volume fraction9 of the dispersed phase present in the eutectic mixture. Since the unidirectional eutectic solidification is a one-step process, i.e., the liquid-solid transformation process, an excellent interfacial bond between the matrix and whisker is obtained. An additional advantage is that no special handling technique for whiskers is needed. In recent years, many investigators10-13 have studied the effects of growth variables on the micromorpholo-gies of binary eutectic alloys produced by controlled solidification. The study of their mechanical properties was initiated by Kraft and coworkers14-16 who found that the strength of cast A1-CuA12 eutectic alloy can be increased threefold by unidirectional solidification. In the A1-AL3Ni system, a strength of 50,000 lb per sq in, was reported for the unidirectionally solidified eutectic alloy, a value five times higher than for conventionally cast material. Thus, the unidirectionally solidified eutectics can be used as fiber-reinforced composite materials. In this paper, we shall first use an equation17 as a guide for the production of eutectic composites in general and the Al-33 wt pct Cu eutectic in particular. Experimental data supporting the theoretical prediction are given. Second, the compressive properties of the grown A1-33 wt pct Cu eutectic were thoroughly investigated in terms of platelet orientations, thermo-mechanical treatment, and temperature. The experimental data are interpreted in terms of a buckling model of fibers in elastic fiber-plastic matrix metallic composites. EXPERIMENTAL PROCEDURE Crystal Growth. The following experimental procedure was adopted for the production of controlled microstructures in the A1-33 wt pct Cu eutectic alloy. The controlled solidification was accomplished with a movable resistance-wound radiation furnace. Fig. 1 is a schematic drawing of the solidification apparatus. A water-cooled chiller was placed into a degassed high-purity graphite crucible containing the charge. Rubber stoppers wrapped with aluminum foil were used to seal both ends of the quartz tube through which a dried argon atmosphere was passed under a slight positive pressure. At both ends of the quartz tube, radiation shields were used to minimize heat loss. The quartz tube was held in place by two steel clamps and the furnace was drawn vertically by means of a steel cable against the steel truss which permits the furnace to move without touching the tube. The drive mechanism consisted of two pulleys, a counter weight.

Jan 1, 1969