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By W. D. Robertson, W. L. Phillips Jr.

Stress-strain curves were obtained for single crystals of alpha brass in tension and in direct shear. Specimens were strained various amounts in a given slip direction, unloaded, and immediately strained in a second slip direction 60°, 120°, or 180&apos; from the original slip direction. Crystals strained in tension and direct shear had comparable critical resolved shear stresses and stress-strain curves. The density of slip lines in direct shear and in tension was essentially the same. The stress-strain curves obtained in shear were independent of initial orientation, choice of {111 } slip plane, choice of <110> slip direction, prior annealing temperature, and rate of cooling after annealing. There was no recovery after annealing for 4 hr at room temperature or 200°C; recovery was observed after 4 hr at 400°C. The crystals showed no asterism and mechanical properties were completely recoverable up to 20 pct strain. It was found that there is a barrier to slip in all latent close-packed directions, and that the magnitude of these barriers, evaluated at 3 pct strain, is proportional to prior strain and independent of the choice of latent direction in the {111} plane. The formation of Cottrell-Lomer barriers is discussed as a possible explanation for the hardening of the latent systems. AN idealized concept of plastic deformation indicates that a single crystal should yield at some stress that is dependent on crystal perfection and it should then continue to deform plastically by the process of "easy glide," which is characterized by a linear stress-strain curve and a low coefficient, ds/dE, of work-hardening. Hexagonal metal crystals generally conform to this ideal concept of laminar flow. In face-centered cubic metals the range of easy glide is always restricted in magnitude and it is strongly dependent on orientation, composition, crystal size, shape, surface preparation, and temperature. Since one of the principal differences between the two crystal systems, both of which deform by slip on close-packed planes, is the existence of secondary (latent) slip planes in the face-centered cubic crystals, it has been proposed that the transition from easy glide to turbulent flow, characterized by rapid linear hardening, is due to slip on secondary planes intersecting the primary plane.&apos;-.; However, the characteristic differences between individual face-centered cubic metals remain to be explained; in particular, it is not clear why the range of easy glide should vary so greatly in different metals and alloys similarly oriented for single slip. An investigation and comparison of different metals with respect to latent hardening on the primary slip plane should provide some of the information required to specify the necessary and sufficient conditions governing the transition from easy glide to turbulent flow. But, in order to accomplish this purpose, plastic strain must be produced by simple shear in a chosen plane and in a predetermined direction by some form of directed shear apparatus, the results of which must be correlated with the corresponding tension experiments. Two such experiments have been performed previously with zinc and with aluminum. Edwards, Washburn, and Parker" and Edwards and Washburn7 found that the strain-hardening coefficients in two latent directions in the basal plane of zinc were the same as in the primary direction. However, to initiate and propagate slip in either the [2110] or the [1210] direction, following primary slip in the [1l20] direction, it was necessary to increase the stress above that required to continue slip in the primary direction; when the direction of shear was reversed 180 deg plastic strain began at a much lower stress than that required to initiate slip in the original direction and the stress to propagate slip in the reverse direction was lower than the stress to continue slip in the forward direction, indicating a permanent loss of strain-hardening. Rohm and Kochendorfer observed softening in aluminum for all latent close-packed planes and directions. They also found that the critical resolved shear stress obtained from their direct shear apparatus was 50 pct lower than the value obtained from conventional tension tests, that the stress-strain curve was linear at 50 pct plastic strain, and that slip lines were not visible at strains less than 30 pct. At present it is uncertain whether these diverse results correspond to real differences in work-hardening characteristics of the close-packed planes of aluminum and zinc or to differences in experimental technique. In view of Read&apos;s analysis &apos;" of the stress distribution in the experimental arrangement of Rohm and Kochendorfer, there is some reason to question the significance of the latter results. In order to resolve this problem it is necessary to re-valuate the direct-shear technique and either repeat the previous measurements or investigate a third system. The latter choice seemed most likely to produce significant results with respect to work-hardening, and accordingly, it was decided to examine the hardening characteristics of the latent slip directions in alpha-brass. The choice of alpha-brass was dictated by the fact that easy glide is more extensive in this alloy than in any other face-centered cubic metal or alloy and, presumably, more nearly like the idealized hexagonal system. Experimental Procedure Crystals were made in graphite by the Bridge-man method in the form of cylinders, 11/2 in. diam and 8 to 9 in. long. Material for the crystals was 70/30 brass containing the following impurities:

Jan 1, 1959

By F. D. George, M. J. Salkind

Al3Ni whisker-reinforced aluminum was found to exhibit good Charpy impact toughness and little notch sensitivity even though its room-temperature tensile elongation parallel to the whiskers is only 2 pct. This impact behavior was maintained d liquid nitrogen temperature (-196"C). It is postulated that this behavior is due primarily to the presence of the continuous aluminum matrix which provides sufficient 10calized ductility in the vicinity of the crack tip to absorb considerable energy from the advancing crack. The impact behavior of Al-Alni was found to be quite anisotropic. Of six orientations studied, the transverse orientation having the notch normal to the whisker axis was found to exhibit the lowest impact energy, whereas the transverse orientation having the notch parallel to the whisker axis was found to exhibit the highest impact energy. A significant differnce was noted between the impact behavior of material containing needlelike whiskers and that containing bladelike whiskers. Only two of the six orientations studied exhibited complete fracture for the material containing needlelike whiskers. On the other had, most of the specimens containing bladelike whiskers exhibited complete fracture. It was postulated that the bladelike whiskers block transverse flow, thus reducing the amount of plastic deformation ahead of the crack tip. One of the more significant advantages of composite materials is the prospect of combining high strength with toughness. In general, toughness is associated with materials which exhibit considerable ductility and can deform plastically in the presence of a stress concentration. Very strong materials which resist plastic deformation generally exhibit low toughness. At first glance, then, it would appear as though strength and toughness are mutually incompatible so that useful engineering materials would have to be a compromise between the two. One approach to the problem of combining the high intrinsic strength of ceramics with the toughness of metals was to mix them together to form a cermet. Unfortunately, the toughness of cermets was found to be rather disappointing. Whisker reinforcement of metals, however, appears to be a more promising approach. It has been demonstrated that whisker-reinforced metals produced by unidirectional solidification exhibit enhanced strength due to the presence of high strength nonmetallic whiskers. The total strain capacity of these composites in the direction of fiber alignment is limited to that of the fibers, the matrix being unable to carry the load once the fibers have failed. A characteristic, then, of whisker composites is low ductility in the direction of whisker alignment, on the order of a few percent elongation. This low elongation, which is usually associated with brittle behavior, should not be taken as an indication of low toughness. Such a material can exhibit significant ductility in directions other than parallel to the fibers7 and can therefore possess significant intrinsic toughness. Toughness in a fiber-reinforced metal is derived from several mechanisms. The first is due to the toughness of the matrix itself. A continuous ductile metal matrix can act as an effective crack arrest medium by undergoing localized plastic deformation. Cracks initiated from the surface of the composite or from a brittle fiber failure must travel through the matrix before reaching another brittle phase particle. A second crack arrest mechanism peculiar to fiber composites is due to the fact that, as a crack travels through the matrix and approaches a fiber, the plastic deformation ahead of the crack tip will result in loading of the fiber. This causes the matrix shear strength in the plastic zone to be apparently higher, thus extracting more energy from the crack and diverting the crack at an angle to the original direction of propagation. A third crack arrest mechanism occurs in fiber composites which exhibit a weak bond between fiber and matrix. The idea was proposed by Cook and Gordons that if a crack propagating transversely in a fiber composite were made to turn and run along the fibers by decohesion of the fiber-matrix bond, then toughness would be imparted by the blunting of the crack tip and the creation of new surfaces. The last mechanism, interfacial decohesion, is commonly noted in naturally occurring fiber composites such as wood, bone, and bamboo, and has been observed in man-made composites such as glass fiber-reinforced resins,g silica fiber-reinforced aluminum," laminated steel," and tungsten and silica fiber-reinforced electroplated copper.&apos;&apos; The first mechanism, crack arrest by plastic deformation in the matrix, has been noted in tungsten wire reinforced cast copper." The purpose of this investigation was to quantitatively assess the toughness of a whisker-reinforced metal as a function of orientation. Previous investigation considered only cracks propagating nominally perpendicular to the reinforcement. In this investigation, crack propagation in three mutually perpendicular directions as well as three intermediate orientations was investigated. The system chosen for study was the unidirectionally solidified A1-A13Ni eu-tectic alloy which has a microstructure consisting of 10 pct by volume of A13Ni whiskers in a matrix of aluminum This material exhibits two different kinds of whisker morphology, depending upon the rate at which it is solidified.&apos; At low rates of solidification (less than 2 cm per hr) the whiskers are bladelike, whereas at higher rates of solidification they are

Jan 1, 1969

By E. W. Stewart, G. P. Conard, J. F. Libsch

The effects of several additives upon the reduction characteristics of hydrogen-reduced ferrous formate are described. The various additives inhibit sintering of the reduced iron particles by apparently different mechanisms. The magnetic properties of the low density compacts produced from the resulting ultra-fine iron powders were improved markedly. THE permanent magnetic characteristics of ultra-fine iron powder prepared by various means have been a subject of considerable interest and experimentation in the past few years. When such particles are small enough to show single domain behavior, they possess&apos; 1—permanent saturation magnetization, and 2—high coercive force. In the absence of domain boundaries, the only magnetization changes in a particle occur through spin rotation which is opposed by relatively large anisotropy forces. With decreasing particle size, the coercive force tends to increase to a maximum and then decrease because of the instability in magnetization associated with thermal fluctuations. Kittel&apos; has calculated the critical diameter at which a spherical particle of iron can no longer sustain domain boundaries or walls to be approximately 1.5x10-&apos; cm. Stoner and Wohlfarthr in England and Neel4,6 in France have shown from purely theoretical calculations that the high coercive force expected from single domain particles is dependent upon crystal anisotropy, shape anisotropy, or strain anisotropy contributions. Further work by Weil, Bertaut,&apos; and many others has contributed much to the understanding of fine particle theory. Neel and Meikeljohn" have demonstrated that a decrease in particle size below a critical value of approximately 160A leads to a quite rapid decrease in coercive force because of the prevention of stable magnetization by thermal agitation. Lih1, working with powders prepared by the reduction of formate and oxalate salts of iron, has shown the marked influence of powder purity upon magnetic properties. Maximum coercive force was obtained in powders of approximately 65 pct metallic iron content while the maximum energy product, (BxH) occurred in powders of 85 pct metallic iron content. Careful consideration of the preceding theoretical considerations and experimental results has led to the manufacture of permanent magnets from ultra-fine ferromagnetic powders by powder metallurgy techniques. Such work has been done by Dean and Davis," the Ugine Co. of France, and Kopelman." The aforementioned work of Kopelman and the Ugine Co. was concerned somewhat with the effect of various additives upon the properties of hydrogen-reduced ferrous formate. Virtually no work, however, has been published on the effects of additives on the reduction rates of metal formates, although unpublished work by Ananthanarayanan16 howed promise of improved energy product in ultra-fine iron compacts prepared by the hydrogen reduction of a coprecipitated mixture of magnesium and ferrous formate. After consideration of the preceding information, it was hoped that a better balance between the metallic iron content and particle size of the reduced iron powder could be accomplished by a prevention of the attendant sintering of the partially reduced iron powder during the reduction reaction. It appeared possible that magnesium oxide might interpose a mechanical barrier between adjacent iron particles and prevent their sintering together, while metallic cadmium and metallic tin would interpose a liquid barrier which might accomplish the same purpose. The degree to which these materials were effective in accomplishing the foregoing objective and the experimental details associated with the work are reported in the following sections of this paper. Experimental Procedure Preparation of Formate and Oxide Mixtures: To obtain ferrous formate of reproducible reduction characteristics, a slight modification&apos; was made in the technique of Fraioli and Rhoda." A supersaturated solution of ferrous formate was mixed with an equal volume of 95 pct ethyl alcohol and the formate crystals precipitated by stirring and screened to —325 mesh. These crystals were in the shape of elongated hexagons, approximately 4x10 micron in dimension. Various preparations of such ferrous formate, designated as lot 111, were reduced for 2 hr, yielding ultra-fine iron particles of exceedingly reproducible size, metallic iron content, and magnetic properties. The magnesium and cadmium formates were prepared by the reaction of dilute formic acid with their respective carbonates, while the tin formate was prepared by the reaction of dilute formic acid with stannous hydroxide. To evaluate the effect of metallic formate additives in intimate mixture with the ferrous formate, varying amounts of magnesium, cadmium, and tin formates were coprecipitated with the latter. The designations of these materials and their chemical compositions are given in Table I. Due to the differing solubilities of the various formates in aqueous media,

Jan 1, 1956

By A. U. Seybolt

The solubility limit of oxygen in columbium has been determined in the range between 775&apos; and 1100°C by means of lattice parameter measurements and microscopic examination. The solubility is a function of temperature and varies, in the range given above, from 0.25 to 1.0 pct O, respectively. BECAUSE of the marked deleterious effect of oxygen upon the mechanical properties of some of the transition metals, it is desirable to know something about the solubility of oxygen in these metals. The brittleness caused by oxygen in solution is particularly marked in the case of the group VA elements, vanadium, columbium, and tantalum. The solubility of oxygen in vanadium has already been reported in an earlier paper,&apos; and Wasilewski2 has given a value (0.9 wt pct) for the solid solubility of oxygen in tantalum at 1050°C. Brauer3 in 1941 investigated the Cb-0 system up to Cb2O5, but made no real effort to investigate the extent of oxygen solubility in the metal. He made the observation, however, that this solubility must be less than 4.76 atom pct (0.86 wt pct) oxygen. This estimate was made from X-ray diffraction results on the alloys CbO, CbO, and CbO; all alloys consisted of the terminal (Cb) solid solution plus CbO, but the last alloy containing 4.76 atom pct 0 showed only three very weak CbO lines. It is surprising that Brauer, by examining only three alloys, arrived at an estimate of the solubility which agrees very well with the results to be reported herein. Experimental Procedure A columbium strip obtained from Fansteel Metallurgical Products was cut into strips, 0.020x1/2x2 in. Two holes, about 3/16 in. in diameter, were made near the ends of the strips in order to hold them against a flat steel block for mounting in a General Electric X-ray spectrometer for lattice parameter measurements. The same holes were used to hang the specimens inside a fused silica vacuum furnace tube which was part of a Sieverts&apos; gas absorption apparatus. The apparatus and method of adding oxygen gas has been previously described.1 According to the supplier, the columbium obtained had the analysis given in Table I. After degreasing the samples, approximately 0.001 in. was etched from each side of the samples in order to remove possible surface impurities from the last rolling operation. For this purpose the following cold acid pickle was found satisfactory: 8 parts HNO3, 2 parts H2O2 and 1 part HF. Various Cb-O compositions were obtained up to 0.75 wt pct O by the gas absorption and diffusion technique. After the sample had absorbed all the oxygen gas added at 1000°C, an additional 24 hr was allowed for homogenization. This treatment appeared to be adequate, as shown by the linearity of the lattice parameter-composition plot. More concentrated alloys were prepared by arc melting mixtures of Cb and Cb2O5 since it was very time-consuming to make Cb-0 alloys in the neighborhood of 1 pct O, or over, by the diffusion method. When the flat strip specimens were used, they were ready for the X-ray spectrometer after cooling from the Sieverts&apos; apparatus. The cooling rate obtained by merely allowing the hot fused silica furnace tube to radiate to the atmosphere (when the furnace was lowered) was sufficiently fast to keep the dissolved oxygen in solution. Arc-melted alloys were reduced to —200 mesh powder in a diamond mortar, wrapped in tantalum foil, sealed off in evacuated fused silica tubes, and then heat treated as indicated in Table 11. The fused silica tubes were quickly immersed in cold water without breaking the tubes after the heat treatments. The tantalum foil prevented reaction between the fused silica and the sample; there was no reaction between the powdered samples and the foil at 1000°C, but some trouble was experienced at 1100°C. At this temperature level a reaction between the sample and the foil was sometimes observed, which resulted in erroneous parameter values. Experimental Results Hardness Tests: Since most of the X-ray samples were in the form of flat strip, it was convenient to obtain Vickers hardness numbers as a function of oxygen content. Compared to the V-O case,&apos; oxygen hardens columbium much more slowly, presumably because of the larger octahedral volume in colum-bium (about 12.0 compared to 9.3Å3 in vanadium), hence, requiring less lattice strain for solution. The plot of VHN vs wt pct O is shown in Fig. 1.

Jan 1, 1955

By J. B. Clark

The oil industry has long recognized the need for increasing well productivity. To meet this need, a process is being developed whereby the producing formation permeability is increased by hydraulically fracturing the formation. The "Hydrafrac" process, as it is now being used, consists of two steps: (1) injecting a viscous liquid containing a granular material, such as sand for a propping agent, under high hydraulic pressure to fracture the formation; (2) causing the viscous liquid to change from a high to a low viscosity so that it may be readily displaced from the formation. To date the process has been used in 32 jobs on 23 wells in 7 fields, resulting in a sustained increase in production in 11 wells. INTRODUCTION Need For Process Although explosives, acidizing, and other methods have long been used, there still exists a need for artificial means of improving the productive ability of oil and gas wells, particularly for wells which produce from formations which do not react readily with acids. This paper discusses the development of a hydraulic fracturing process, "Hydrafrac", which shows distinct promise of increasing production rates from wells producing from any type of formation. The method is also considered applicable to gas and water injection wells, wells used for solution mining of salts and, with some modification, to water wells and sulphur wells. Requirements of Process In considering such a possible process, it appeared that certain requirements must be met. Some of these are as follows: A. The hydraulic fluid selected must be sufficiently viscous that it can be injected into the well at pressure high enough to cause fracturing. B. The hydraulic fluid should carry in suspension a propping agent, such as sand, so that once a fracture is formed, it will be prevented from closing off and the fracture created will remain to serve as a flow channel for oil and gas. C. The fluid should be an oily one rather than a water-base fluid, because the latter would be harmful to many formations. D. After the fracture is made, it is essential that the fracturing fluid be thin enough to flow hack out of the well and not stay in place and plug the crack which it has formed. E. Sufficient pump capacity must be available to inject the fluid faster than it will leak away into the porous rock formation. F. In many instances, formation packers must be used to confine the fracture to the desired level, and to obtain the advantages of multiple fracturing. Development of Process As a necessary step in the development of this process, it was deemed advisable to determine if the Hydrafrac fluids were actually fracturing the formation or whether these special fluids were merely leaking away into the surrounding formation. To determine this, a shallow well, 15 feet deep, was drilled into a hard sandstone. Casing was set, the plug drilled, and the well deepened in the conventional manner. A fracturing fluid dyed a bright red was used to break down the formation. Sand mixed with distinctively colored solids was injected into the well with the fracturing fluid to prop open any fracture made in the formation. A simulated gel breaker solution dyed a bright blue was then pumped into the well to determine if the gel breaker would follow the first solution. The results are shown in Figure 1. It was noted that a fracture was formed about the well bore, that the propping agent was transported back into the break, and that the breaker solution did actually follow the fracturing gel out into the fracture. While it is realized that this shallow well test is probably not exactly equivalent to a deep test, the results were interpreted as being a definite indication of what happens down the hole during a Hydrafrac job. Of interest in this connection is an investigation reported by S. T. Yuster and J. C. Calhoun, Jr.&apos; This study, re~orted after the Hydrafrac work was under way, presents some excellent field data supporting the theory of fracturing a formation with hydraulic pressure. METHOD Steps of Hydrafrcu: Process Figure 2 shows a simplified cross-sectional view of a well treated by one version of the process. The first step, formation breakdown, is done with a viscous fluid, usually consisting of an oil such as crude oil or gasoline, to which has been added a bodying agent. Due to availability and price, war-surplus Napalm has been used in the majority of experiments to date. Napalm is the soap which was used in the war to make "jellied gasoline". The next step consists of breaking down the viscosity of the gel by injecting a gel-breaker solution and then after several hours, putting the well back on production. Figure 3 shows diagram-matically, a typical field hookup. The oil or gasoline is unloaded into the 10 bbl. tank shown on the left rear of the truck. This base fluid is picked up by the mixing pump and pumped through the jet mixer, where the granular soap is added. Next it goes into a small mixing tub, from which the high-pressure pump takes suction. The solution is then pumped into the well. The breaker solution is then taken from an extra tank and is displaced into the well immediately following the gel. When required, additional trucks may

Jan 1, 1949

By J. B. Clark

The oil industry has long recognized the need for increasing well productivity. To meet this need, a process is being developed whereby the producing formation permeability is increased by hydraulically fracturing the formation. The "Hydrafrac" process, as it is now being used, consists of two steps: (1) injecting a viscous liquid containing a granular material, such as sand for a propping agent, under high hydraulic pressure to fracture the formation; (2) causing the viscous liquid to change from a high to a low viscosity so that it may be readily displaced from the formation. To date the process has been used in 32 jobs on 23 wells in 7 fields, resulting in a sustained increase in production in 11 wells. INTRODUCTION Need For Process Although explosives, acidizing, and other methods have long been used, there still exists a need for artificial means of improving the productive ability of oil and gas wells, particularly for wells which produce from formations which do not react readily with acids. This paper discusses the development of a hydraulic fracturing process, "Hydrafrac", which shows distinct promise of increasing production rates from wells producing from any type of formation. The method is also considered applicable to gas and water injection wells, wells used for solution mining of salts and, with some modification, to water wells and sulphur wells. Requirements of Process In considering such a possible process, it appeared that certain requirements must be met. Some of these are as follows: A. The hydraulic fluid selected must be sufficiently viscous that it can be injected into the well at pressure high enough to cause fracturing. B. The hydraulic fluid should carry in suspension a propping agent, such as sand, so that once a fracture is formed, it will be prevented from closing off and the fracture created will remain to serve as a flow channel for oil and gas. C. The fluid should be an oily one rather than a water-base fluid, because the latter would be harmful to many formations. D. After the fracture is made, it is essential that the fracturing fluid be thin enough to flow hack out of the well and not stay in place and plug the crack which it has formed. E. Sufficient pump capacity must be available to inject the fluid faster than it will leak away into the porous rock formation. F. In many instances, formation packers must be used to confine the fracture to the desired level, and to obtain the advantages of multiple fracturing. Development of Process As a necessary step in the development of this process, it was deemed advisable to determine if the Hydrafrac fluids were actually fracturing the formation or whether these special fluids were merely leaking away into the surrounding formation. To determine this, a shallow well, 15 feet deep, was drilled into a hard sandstone. Casing was set, the plug drilled, and the well deepened in the conventional manner. A fracturing fluid dyed a bright red was used to break down the formation. Sand mixed with distinctively colored solids was injected into the well with the fracturing fluid to prop open any fracture made in the formation. A simulated gel breaker solution dyed a bright blue was then pumped into the well to determine if the gel breaker would follow the first solution. The results are shown in Figure 1. It was noted that a fracture was formed about the well bore, that the propping agent was transported back into the break, and that the breaker solution did actually follow the fracturing gel out into the fracture. While it is realized that this shallow well test is probably not exactly equivalent to a deep test, the results were interpreted as being a definite indication of what happens down the hole during a Hydrafrac job. Of interest in this connection is an investigation reported by S. T. Yuster and J. C. Calhoun, Jr.&apos; This study, re~orted after the Hydrafrac work was under way, presents some excellent field data supporting the theory of fracturing a formation with hydraulic pressure. METHOD Steps of Hydrafrcu: Process Figure 2 shows a simplified cross-sectional view of a well treated by one version of the process. The first step, formation breakdown, is done with a viscous fluid, usually consisting of an oil such as crude oil or gasoline, to which has been added a bodying agent. Due to availability and price, war-surplus Napalm has been used in the majority of experiments to date. Napalm is the soap which was used in the war to make "jellied gasoline". The next step consists of breaking down the viscosity of the gel by injecting a gel-breaker solution and then after several hours, putting the well back on production. Figure 3 shows diagram-matically, a typical field hookup. The oil or gasoline is unloaded into the 10 bbl. tank shown on the left rear of the truck. This base fluid is picked up by the mixing pump and pumped through the jet mixer, where the granular soap is added. Next it goes into a small mixing tub, from which the high-pressure pump takes suction. The solution is then pumped into the well. The breaker solution is then taken from an extra tank and is displaced into the well immediately following the gel. When required, additional trucks may

Jan 1, 1949

By K. R. Carson, J. Weertman

An attempt is made to ascertain the mechanism of tangle and cell formation and its dependence upon dislocation-interstitial carbon interactions. The strain-hardening behavior of single crystals of 3.25 pct Si-Fe was determined at 300° and 425°K and under conditions of both continuous and interrupted tensile strain. Significantly enhanced hardening was observed in crystals deformed at the elevated temperature, and it was further accentuated by interrupted straining. Transmission electron microscopy was used to study the resultant dislocation structures. Strain aging was found to aid tangle and cell formation at 425°K, but at both temperatures embryo tangles formed solely from primary glide dislocations, presumably by a process involving cross slip and "mushrooming". IN the course of plastic deformation all bcc metals and alloys develop a dislocation structure characterized by loose-knit groups of tangled dislocations. With increasing strain the tangles become more tightly knit and grow larger; finally a three-dimensional cellular substructure is formed:1 This process has been observed with the transmission electron microscope.&apos;-l7 However, most investigations were confined to the study of nearly pure polycrystalline metals at relatively low temperatures. At intermediate temperatures, 0.17 to 0.14 Tm where T, is the melting temperature in degrees absolute, the mobility of interstitial impurities such as carbon is high enough to permit migration to nearby glide dislocations but is still low enough so that a significant drag force is exerted.18,19 it is also in this temperature range that a hump occurs in the curve of work-hardening rate vs temperature for iron. Analogous plots for tantalum" and columbiumzo show a definite upward trend in the work-hardening rate. Keh and Weissman1 have pointed out that this behavior may be explained solely on the basis of changes in the dislocation configuration: at low temperatures the dislocations tend to be relatively straight and uniformly distributed, but at intermediate temperatures tightly knit tangles and cellular substructure appear. The interference of these tangles with glide dislocations causes the observed increase in the work-hardening rate. This explanation appears reasonable, yet one might ask what factors cause tangle formation to be so favorable at intermediate temperatures. It seens likely that the strong dislocation-interstitial interactions which are known to occur in this temperature range are at least partly responsible," with the magnitude of the effect being proportional to the interstitial concentration. The purpose of the present work is to study the relationship between tangle formation and strain hardening in a bcc metal in the temperature range 0.17 to 0.4 Tm. Particular emphasis was placed upon a study of the effects of interstitial-dislocation interactions. Single crystals of 3.25 pct Si-Fe containing about 200 ppm of C in solid solution were used in the investigation for the following reasons: 1) The mobility of interstitial carbon in 3.25 pct Si-Fe is negligible at 300°K but increases rapidly at slightly elevated temperature22. Hence, differences between the flow curves and dislocation structures of crystals deformed at 300°K, 0.17 T,, and crystals deformed, say, at 425°K, 0.24 Tm, should be appreciable because of the enhanced dislocation-carbon interactions at the elevated temperature. This effect was accentuated in some samples by interrupted straining, thereby introducing a certain amount of aging. 2) Near room temperature, slip in suitably oriented 3.25 pct Si-Fe single crystals is largely confined to the (110) planes.23&apos;24 Dislocation structures formed under conditions of single glide are the least complicated and their method of formation is the most easily discernable. 3) Dislocations in Si-Fe can be tightly locked with carbon atmospheres by a low-temperature aging treatment. The subsequent thinning of samples to foil thicbess causes little or no rearrangement in the dislocation structure.25 EXPERIMENTAL PROCEDURE Large single-crystal sheets of 3.25 pct Si-Fe were donated by Dr. C. G. Dunn of the General Electric Research Laboratory, Schenectady, N. Y. The orientations of the sheets were determined and slabs 1.0 by 0.25 by 0.05 in. were cut such that the desired tensile axis corresponded to the long dimension. The slabs were mechanically polished and subsequently decar-burized by heating at 1000°C for 3 days in a flowing wet-hydrogen atmosphere. A carbon content of about 200 ppm was introduced by heating at 805°C for 25 min in a flowing atmosphere of dry hydrogen containing heptane vapor. Shaped copper tools were then used to spark-machine at 0.125 by 0.50 in. gage length onto each slab. Vacuum annealing at 1225°C for 2 days followed by a quench into the cold end of the furnace to retain carbon in solid solution concluded the soecimen preparation. Continuous tensile flow curves for crystals of severa1 orientations Were obtained both at 300&apos; and 425°K. A strain rate of 6.67 x 10-4 Per set was used in these and all other tests. Crystals oriented for single glide, B and D in Fig. 1, were subjected to a 3.5 pct plastic elongation to insure uniform slip along the gage length; they were then immediately subjected to interrupted strain cycling as indicated in Fig. 2(a). Each cycle consisted of unloading to 1.5 kg per sq mm, holding

Jan 1, 1969

By Luc Delaey, Horace Pops

The structure and morphology of thermoelastic and burst type martensitic phases that form upon cooling in Cu-Zn-Si p phase alloys have been studied by transmission electron microscopy. The martensitic phases are composed of a lamellar mixture of two close-packed structures with different stacking sequence, namely ABCBCACAB (orthorhombic) and ABC (fcc). Striations within thermoelastic martensite are most likely produced during interaction with impinging burst-type martensite and not as a consequence of secondary shears. In a study of the martensitic transformation in ternary Cu-Zn based 0 phase alloys1 the dependence of the martensitic transformation temperature, M,, with composition shows variations for elements within a constant valence subgroup and between different subgroups. Such variations are not reflected in a change in habit plane, which is approximately the same for each ternary alloy, namely in the vicinity of (2, 11, 12 Ip. The fact that the habit plane remained constant, despite large differences in M, temperature and electron concentration, suggested2 that the crystal structures of the martensitic phases could be nearly the same. Crystal structures of ternary Cu-Zn based martensites have been determined recently for alloys containing the three-valent elements gallium3, 4 and aluminm. The present studies have been made to examine the structures and morphology of the martensitic phase in ternary Cu-Zn based alloys containing a four-valent element, silicon. I) PROCEDURE Two alloys were prepared by melting and casting weighed quantities of the component high-purity metals in sealed quartz tubes under half an atmosphere of argon. They were subsequently remelted by levitation under a protective atmosphere of argon. After allowing for losses of zinc as determined by the difference in weight before and after casting, the compositions in atomic percent of both alloys were established to be Cu-33.5 Zn-1.8 Si and Cu-27 Zn-5.0 Si. These alloys were homogenized in the P-phase field for 2 days at 800" C. Bulk samples consisted of a martensite phase at room temperature, the M, temperature being approximately 30&apos; and 200" for the 1.8 and the 5 pct Si alloys, respectively. Thin disks were cut from the ingots using a spark machine, and they were heated for 5 min at 800&apos; and quenched into water in order to obtain martensite. These slices were thinned chemically at room temperature in a solution consisting of 40 parts HN03, 50 part H3PO4, and 10 parts HC1 and thinned further electrolytically by the Window technique, using a voltage of 15 to 25 v and a mixture of 1 part HN03 and 2 parts methanol, which was kept at a temperature near -30° c. Foils were examined by transmission electron microscopy using a Philips EM 200 electron microscope. 11) RESULTS AND DISCUSSION 1) Structure and Morphology. Fig. 1 shows the martensitic phase in the alloy containing 1.8 at. pct Si. This phase is composed of contiguous platelets, each containing striations. The direction of the striations changes at the boundary between individual platelets. These internal markings resemble the striations that are usually identified as stacking faults, as for example in Cu-A1 martensites6-a or the lamellar mixture of two close-packed phases in Cu-Zn-Ga marten-sites.3p &apos;9 lo In the present alloys, selected-area diffraction experiments have been obtained in order to determine the nature of the striations. Figs. 2(a), (61, and (c) are electron diffraction patterns of an area inside a single martensite plate. Fig. 2(a) contains diffraction spots which correspond to two close-packed structures with different stacking sequences, namely ABCBCACAB (orthorhombic) and ABC (fcc). Spots belonging only to the fcc structure are indicated by arrows. By tilting the foil either the orthorhombic structure, Fig. 2(b), or the cubic structure shown in Fig. 2(c) may be obtained. When the foil is oriented so that only the diffraction spots of the orthorhornbic structure are present, bright-field illumination shows small lamellae, as seen in Fig. 3. In this figure the lamellae that belong to the fcc structure are bright bands inside the dark extinction contours of the orthorhombic structure. The boundaries of the lamellae are parallel to the basal planes of the orthorhombic structure and to the {Ill} planes of the cubic structure, the close-packed directions of both structures being parallel. The 5 pct Si alloy shows similar features as those described for the 1.8 at. pct Si alloy.

Jan 1, 1969

By M. Metzger, J. C. Bilello

Microyielding in 99.999 pct Cu occuwed in two distinct parabolic microstages and was substantially indeoendent of grain size at the relatiz~ely large grain sizes stzcdied. The strain recouered on unloading was a significant fraction of the forward strain and was initially higher in a copper-coated single crystal than in poly crystals. Results were interpreted in terms of cooperative yielding and short-range dislocation motion activated otter a range of stresses, and a formalism was given for the first microstage. It was suggested that models involving long-range dislocation motion are more appropriate for impure or alloyed fcc metals. THERE are still many unanswered questions concerning the degree and origin of the grain size dependence of plastic properties. In the microstrain region, a theory of the stress-strain curve proposed by Brown and Lukens,&apos; based on an exhaustion hardening model in which the grain boundaries limit the amount of slip per source, accounted for the variation with grain size of microyielding in iron, zinc, and copper.&apos; This theory assumes N dislocation sources per unit volume whose activation stress varies only with grain orientation. Dislocations pile-up against grain boundaries until the back stress deactivates the source, which leads to a relationship between the axial stress and the strain in the microstrain region given by: where G is the shear modulus, D the grain diameter, a the flow stress, and a, is the stress required to activate a source in the most favorably oriented grain.3 If this or other grain-boundary pile-up models are correct, then the reverse strain on unloading would be much larger for a polycrystalline specimen than for a single crystal. Also, the microplasticity would become insensitive to grain size if this could be made larger than the mean dislocation glide path for a single crystal in the microregion. These questions are examined in the present work on polycrys-talline copper and a single crystal coated to provide a synthetic polycrystal. EXPERIMENTAL PROCEDURE Tensile specimens 3 mm sq were prepared from 99.999 pct Cu after a sequence of rolling and vacuum annealing treatments similar to those recommended by Cook and Richards4-6 to minimize preferred orientation. Grain size variation from 0.05 to 0.38 mm was obtained by a final anneal at temperatures from 310" to 700°C. Dislocation etching7 revealed pits on those few grains within 3 deg of (111). For all grain sizes dislocation densities could be estimated as -107 cm per cu cm with no prominent subboundaries. The single crystals, of the same cross section, were grown by the Bridgman technique with axes 8 deg from [Oll] and one face 2 deg from (111). An anneal at 1050°C produced dislocation densities of 2 x 106 cm per cu cm and subboundaries -1 mm apart in these single crystals. A Pb-Sn-Ag creep resistant solder was used to mount the specimens, with a 19 mm effective gage length, into aligned sleeve grips fitted to receive the strain gages. All specimens were chemically polished and rinsed8 to remove surface films just prior to testing. The synthetic polycrystal was made by electroplating a single crystal with 1 µ of polycrystalline copper from a cyanide bath. Mechanical testing was carried out on an Instron machine using two matched LVDT tranducers to measure specimen displacement, the temperature and the measuring circuit being sufficiently stable to yield a strain sensitivity of 5 x 107. At the crosshead speeds employed, plastic strain rates were, above strains of 10¯4, about 10¯5 per sec for polycrystalline specimens and 10-4 per sec for the single crystals. Plastic strain rates were an order of magnitude lower at strains near l0- &apos;. A few checks at strain rates tenfold higher were made for reassurance that the initial yielding of polycrystalline copper was not strongly strain-rate dependent. Test procedures followed the general framework outlined by Roberts and Brown.9,10 An alignment preload of 8 g per sq mm for polycrystals, and 2 to 4 g per sq mm for single crystals, was used for all tests. These gave no detectable permanent strain within the sensitivity of the present experiments; although at these stress levels, small permanent strains are detectable in copper with methods of higher sensitivity.11 12 stress and strain data are reported in terms of axial components. RESULTS General. The initial yielding is shown in the stress vs strain data of Fig. 1. For polycrystals, cycle lc, the loading line bent over gradually without a well-defined proportional limit, and almost all of the plastic prestrain appeared as permanent strain at the end of the cycle. The unloading curve was accurately linear over most of its length with a distinct break indicating the onset of a significant nonelastic reverse strain at the stress o u, indicated by the arrows. The yielding in subsequent cycles, Id and le, had the same general character. The single crystal behavior, shown to a different scale at the right of Fig. 1, was different in that initially the nonlinear reverse strain was unexpectedly much greater than for polycrystals. It should be noted that these soft crystals had a small elastic

Jan 1, 1970

By William E. Ford, Edward Salisbury Dana

THIS Appendix contains a series of tables, more or leas complete, of minerals arranged according to chemical composition or to certain prominent crystallograhic or physical characters. These, it is believed, will be of service not only to the student, but ago to the skilled mineralogist. The type used in the printing of the mineral names indicates their relative importance. Table I is a complete list of the species named in this book arranged fist according to the prominent basic elements which they contain and secondly according to their acid radicals. Table II is of Minerals arranged according to their System of Crystallization The other tablets make no claim to completeness, being limited often to common ah important species. For an exhaustive system of Determinative Tables based particularly upon blowpipe and chemical characters, the student is referred to the work of Professors Brush and Pen- field, mentioned on p. 330.

Jan 1, 1922

By Waldemar Lindgren

CONTENTS. [ ] I. INTRODUCTION. THE precious metals, gold and silver, are the basis of the monetary systems of the world. It is, therefore, natural and inevitable that widespread interest should be manifested in their production and in the various classes of deposits in which they are contained. At times a great scarcity of the precious metals has prevailed; at other times the production has seemed so abnormally large that fears have been entertained regarding their ultimate retention as standards of value. Since most nations have adopted the gold standard, and the remaining ones appear likely to do the same in the near future, the question of available supply of gold for the present and future very naturally arises. This necessarily involves a consideration of the characteristics of the gold-deposits. After the absorption of the gold treasures of the New World by the conquistadores, the gold-placers of Brazil and Russia

Jan 1, 1913

By Ellis Clark

Within the last ten years the progressive party of China, headed by Li Hung Chang, the Viceroy of Chi-Li, has been making great efforts to develop the mining resources of that country, and particularly those that are within reasonable distances of the sea-board. Attention was first paid to the coal-deposits, especially those at KaiPing, which have been placed on a profitable basis with an output of 1500 tons per day, under the energetic management of Mr. Claude Kinder, M.I.C.E., and the successful financiering of Tong King Sing. These coal-mines were described in a report by Kwong Yung Kwang, edited as a paper for the Institute (Duns., xvi., 95.) The attention of the leaders of the progressive party has for the past five years been turned also toward the development of the precious and related metals—gold, silver, copper and lead. De-

Jan 1, 1891

By Leon Dominian

I. INTRODUCTION APART from local needs in the country&apos;s development, the interest attached to Turkish fuels grows chiefly out of the importance of the railway industry in Asiatic Turkey. Geographical conditions make of the tracks in this region the most essential link in a chain of world-girdling lines. By its position Asia Minor can be likened to a bridge in the through routes destined to connect European factories with Asiatic and African markets. An uninterrupted right-of-way from points in central Europe to populous Indian cities must necessarily pass through the valleys A Anatolia. Crossing thence the Taurus Mountains its natural passage is indicated as the Mesopotamian lowland and the shores of the Indian Ocean. Similarly land connection between Europe and Africa can be obtained only by passage through Asia Minor, Syria and Palestine. The occurrence of fuel within an area of such significance from the

Jan 6, 1916

By S. J. McCarroll

THE Three Kids mine, some six miles east of Henderson, Nev., is in a typical southwest desert area, with high dry summer heat and cool to cold winter seasons. The manganese deposit was located during World War I.1 During this period 15,000 to 20,000 tons of ore assaying up to 41 pct manganese were shipped. Interest in the deposit was not revived until the middle thirties, when experiments on the ore were initiated. Test work indicated possible recovery of only 70 pct by flotation, but in 1941 additional work was done at the Boulder City pilot plant of the U. S. Bureau of Mines and also by M. A. Hanna Co. As a result, the Manganese Ore Co. was formed and a plant utilizing the SO, process was constructed. Numerous operation difficulties ensued, and the plant was closed when the manganese situation in the country eased.

Jan 3, 1954

By C. S. Roberts

THE advent of a sensitive X-ray method of analysis recently has allowed the determination of retained austenite in amounts as low as 0.3 pct.&apos; As a result this phase has been found in quenched low carbon steels where its presence has not been generally suspected. In the course of a study of the tempering process,&apos; retained austenite determinations were made by the X-ray method on a series of high purity Fe-C alloys and plain carbon steels. The chemical analyses of these materials and details of the hardening procedure are given in Table I. Results were obtained after quenching to 72°F (22°C) and — 321 °F (—196°C). Austenitizing temperatures were between 100" and 150°F above A, or Acm. All proeutec-toid cementite or ferrite was in solution. The combination of the results with those of Averbach, Castleman, and Cohen,&apos; and earlier results of Esser

Jan 1, 1954

NEW, MEMBERS The following list comprises the names of those persons who became members during the period July 10, 1916; to July 31, 1916: BOYD, ROBERT RUSSELL Supt:,-Arizona -Commercial Min Co., Globe, .Ariz. BRADLEY, HENRY FRANKLIN, Chem, American Smelt & Ref. Co. Murray,:Utah: BROWN, THOMAS ELLIS, JR..:&apos;. L .:.::..55 Hill, St;; Morristown, N. J. CARY, WEBSTER P., Expert Operator,-General Engineering. Co:, Salt Lake City, Utah. CLARK, ALONZO WEBSTER 3223_ Scottwood Ave., Toledo, Ohio. CORP, CLIFFORD Old Dominion Copper Min. & Smelt. 60., Globe, Ariz. CROMBIE, W. RANSOM, Min. Engr Detroit Copper Min. Co., Morenci, Ariz. DELANEY, EUGENE A., Chief Engr., Berwind-White. Coal Mining -Co., Windber, Pa ELBELT, WILLIAM HENRY, Dept. Foreman., Chino Copper Co., Hurley, N. Mex. FOSTER, L. JULIO, Mgr., Minas i Fundicion ; ?La Junta," San Bernardo, Chile, South America. GASKILL, JAMES PHILLIPS, Genl. Mgr.,.Ajo Cons. Copper Co., Ajo, Ariz., via Gila, Ariz. .

Jan 9, 1916

By H. E. Sadler, Prof. Silliman

The research here recorded was undertaken early in the present year, and has been prosecuted steadily for about eight months. While the work has been under my constant supervision and advice, the labor has all been performed by Mr. Sadler, to whom is chiefly due the development of the successive steps which have led to the final result. The process is better than I dared to hope, and we are able to place at the command of chemists and engineers interested in the matter an apparatus of continuous and uninterrupted action, and methods of analysis by which the daily averages of the two variable and inconstant factors of illuminating gas, ammonia and sulphur, may be determined with all needful accuracy, even by those little skilled in chemical manipulation, and with very little loss of time. This research has been carried out in the laboratory of the New Haven Gaslight Company.

By Edwin A. Sperry

In 1892 I tested an ore, which was peculiarly difficult to treat, on several concentrators then in general use, including t,he Frue-vanner, the Luhrig table and the Cornish buddle. Owing to the character of the ore it had to be crushed- to a very fine state of division, and the results obtained were far from satisfactory; a large proportion of the values was lost in the slimes, which indicated the necessity of a very careful sizing before dressing. Even after reworking some of the slime-tailings, the results, in my opinion, were not as good aa those which might be obtained on a table designed more especially for the handling of slime. Although the subject of slime-concentration has occupied the attention of many engineers who have threshed the field quite thoroughly, the results obtained in my work led to a careful

Jan 1, 1904

By James E. Lawver

A SURVEY of Minerals Beneficiation Div. membership indicated genuine interest in automatic process control, but revealed that the average mill is operating with a minimum of self-regulating devices. Apparently, the mill operators are content to continue without controls until the practicality of self-regulating devices is more generally accepted, or, in the opinion of the writer, until automatic controls become a necessity to meet economic demands of product quality and cost. Both to stimulate interest in control, and to solicit publication of technical know-how by members and equipment manufacturers, this paper presents a cross section of control problems in two general categories: (a) Control problems that can usually be solved by reference to the literature, i.e. controls that have proven successful in the mineral or chemical industries; (b) Problems that are troublesome and frequently unsolved due to unavoidable adverse conditions in the mill circuit to be controlled.

Jan 10, 1953

By B. W. Veal, B. S. Chandrasekhar

THE Laue method of orienting single crystals requires the use of tables of angles between crystal-lographic planes, and between zone axes. Such tables have been published for cubic crystals, and some rhombohedra12 and hexagonal3 crystals. A table of angles between planes in ß-tin has also been published;4 these angles refer to only low-index planes, and are not particularly helpful in the actual indexing of spots on a Laue photograph. Furthermore, it is often useful to know the angles between zones which share a common low-index plane. We have calculated such tables of angles for ß-tin and indium, both between planes in principal zones, and between zones passing through principal planes. The results are given in Tables I and 11. The standard formulas were used, with c/a = 0.54554 for 0-tin, and 1.07586 for indium.

Jan 1, 1962