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By C. D. Hall, F. E. Dollarhide

Fluid Ioss agent.s for crude oil and for water have been studied in dynamic tests. A treatment using a spearhead with a fluid loss agent followed by plain fluid appears feas ible in crude oil, but not in water. An equation for spearhead depletion shows that spurt loss relative to fracture width must be low, if the portion of spearhead fluid in the treatment is to be small. The presence of colloidal matter in crude oils aids the fluid Ioss agent. Unlike in kerosene, where flow limited the agent deposition, in crude oils the filter cake continually formed and leak-off declined. The volume-time relation varied somewhat for different crudes, but was best described by a square root of time function. Spurt loss was inversely proportional to agent concentration. After the fluid loss agent initiated the filter cake, the crude oil colloids built on it effectively. A 2-minute or a 5-minute spearhead with double the normal agent concentration gave the same fluid Ioss curve as the same concentration did for a 30-minute test. The agents tested in water gave fluid Ioss plots on which, for the first few minutes, volume was proportional to the square root of time, but later became proportional to time. For fracture area calculation the customary square root of time function is a satisfactory approximation. Leak-off rates and spurt losses were higher in water systems than in oils. The spurt Ioss tended to be inversely proportional to concentration. In spearhead tests, the filter cakes were not eroded by water flow. However, the rather high spurt loss values make spearhead treatments impractical for water-based fluids. Introduction The effects of dynamic testing conditions on the performance of fluid loss agents in kerosene have been studied previously.' We have extended the work to include crude-oil- and water-based fracturing fluids. An understanding has been gained of the mechanisms of formation and functioning of the filter cakes of fluid loss agents. The practical aspects of evaluating performance of agents in relation to fracture area calculations also are considered. The feasibility of using the fluid loss agent in a spearhead stage of the treatment is examined further for both types of fluids. Experimental Procedure The dynamic fluid loss tests were performed in an apparatus similar to the high-pressure apparatus described in a previous publication.' A fracturing fluid was circulated over a rock surface located in a closed pressurized loop. The fluid flowed axially over the cylindrical surface of a core 2 in. in diameter X 3.5 in. long, mounted (with the flat ends sealed off) in a pipe, with 0.117 in. annular clearance. The filtrate was collected in a central hole in the core and led through valves to graduated cylinders. Provision was made for changing quickly the circulating fluid during the test (spearhead runs) without interrupting the filtration pressure. The only modifications were to add heating tapes and water jackets for the tests with crude oils, all conducted at ISOF, and to change all parts exposed to the test fluid to stainless steel for the tests with water-based fluids. The latter tests were made at room temperature, 80F. Three crude oils were tested. A mixed crude, obtained from a local refinery, contained a considerable amount of light ends. For safety reasons, it was stripped to 250F vapor temperature before use in the fluid loss tests. The other two oils were used as obtained from lease tanks. One was a greenish-brown, 37" API paraffinic crude, and the other was a black, 32" API asphaltic crude. The fluid loss agent for oil, here designated for brevity as Agent A, was Adomite@ Mark II*, a granular solid commercial agent, the same as previously tested in kerosene.' Three different compositions of fluid loss agents were tested in Tulsa tap water. Agent B was adomit& Aqua*, a solid commercial fluid loss agent, comprising clays and hydrophilic gums principally derived from starch. Agent C was a mixture of three parts of Agent B with two parts of silica flour. Agent D was Dowel1 J137, a mixture of guar gum and silica flour. The test cores were cut from contiguous blocks of Berea or Bandera sandstones. For the oil tests, the cores were oven dried, evacuated, saturated with kerosene, and the kerosene permeability was measured. The cores used with the water-based fluids were pretreated by saturating with 3 percent calcium &loride solution to minimize pemeability damage by the fresh water due to clay migration. The

Jan 1, 1969

By R. L. Rickett, S. H. Kalin, J. T. Mackenzie

Aluminum killed low carbon steel, § which is now used extensively for severe deep drawing or other difficult forming operations, is unusual in that its grain structure, after cold reduction and box annealing in accordance with conventional continuous sheet or strip mill practice, often is elongated, although at times it is equiaxed. Since this unusual structure has been found superior for many, but not all, severe forming operations, recrystallization of the steel, both at constant temperature and on continuous heating, was investigated and compared with that of rimmed steel in the hope that something might be learned about the mechanism of, and the factors controlling, the formation of such elongated grains. In this structure, the grains are elongated both in the lengthwise direction of the strip and transverse to this direction, even though nearly all of the extension in both hot and cold rolling is in the lengthwise direction. The grains are thus roughly pancake-shaped, being longer and wider than they are thick, as observed also by Burns and McCabe,1 and as illustrated by the typical structures shown in Fig 1. Fig la, representing a conventional longitudinal section, shows the length and thickness of the grains, whereas Fig Ib shows their length and width as seen by examining a section parallel to the sheet surface. Both illustrate the very irregular grain boundaries usually associated with the elongated grain shape. A finer equiaxed grain structure in this same grade is shown in Fig Ic. Either the elongated or the equiaxed structure may be present in the annealed product, and in rare instances the two types may coexist in a single specimen, as shown in Fig 1 d. Isothermal Recrystalliza-tion of Rimmed and Alamimum Killed Steel An aluminum killed steel known to have an elongated grain structure after conventional processing (Steel B, Table l), was selected for the initial recrystallization studies; for comparison, a rimmed steel, A in Table 1, was used. Samples of each in the form of hot rolled strip 0.075 and 0.095 in. thick, respectively, were cold rolled on a small laboratory mill in steps of about 0.010 in. per pass to obtain total reductions of 40 and 60 pct. Small pieces of the cold reduced strip were heated in lead at selected constant temperatures for one of several periods of time, then cooled in air. Rate of heating in the lead was, of course, very fast. Hardness of the cooled specimen was measured and a longitudinal section examined metallographically. Isothermal recrystallization curves for these two steels at 1050°F, based on hardness of the air cooled specimens, are shown in Fig 2 in which the amount of recrystallization corresponding to each plotted point is indicated. The marked difference in the behavior of these two types of steel is evident. After a corresponding amount of cold reduction, the rimmed steel recrys-tallizes in a much shorter time than the killed steel and the shape of its recrystallization curve, (plotted on a logarithmic time scale), is very different. The curve for rimmed steel indicates that recrystallization is analogous to isothermal transformation of aus-i.enite in that it proceeds at a progressively faster rate up to some 50 pct recrystallization, then at an increasingly slower rate. For the aluminum killed steel, however, the start of

Jan 1, 1950

By Bailey Willis

IN 1882, Peckham put forward a provisional hypothesis to account .or the distillation of petroleum.1 He did not formally state the hypothesis, but in a discussion of facts drawn from many fields he made it clear that he regarded petroleum, and especially the petroleum of the Pennsylvania fields, as a "fractional distillate produced under high pressure and consequently at a comparatively high temperature.?2 He quotes James Hall on the geology of the Appalachians and says:3 It is not necessary here to discuss the nature or origin of metamorphic action. It is sufficient for our purpose to know that from the upper Silurian to the close of the Carboniferous periods the currents of the primeval ocean were transporting sediments, sorting them into gravel, sand, and clay, forming gravel bars and great sand beds beneath the riffles and clay banks in still water, burying vast accumulations of sea weeds and sea animals far beneath the surface. The alteration, due to the combined action of heat, steam, and pressure, of the formations of the Appalachian system from Point Gaspe in Canada to Lookout mountain in Tennessee, involving the Carboniferous and earlier strata, distorting and folding them, and converting the coal into anthracite and the clays into schists along their eastern border, could not have ceased to act westward along an arbitrary line, but must have gradually died out farther and farther from the surface (source?). The great beds of shale and limestone containing fucoids, animal remains, and even indigenous petroleum must have been invaded by this heat action to a greater or less degree, and that "chronic evaporation" of Prof. Lesley must have been the inevitable consequence. From an investigation of the relations between coal and petroleum, White has" more recently concluded as follows: (1) Petroleum is a product generated in the course of the geodynamic alteration of deposits of organic debris of certain types buried in the sedimentary strata. (2) The quantity and characters of the oils generated are determined by: (a) the composition of the organic deposit at the beginning of its dynamo-chemical alteration; (b) by the stage in the progress of the dynamo-chemical alteration of the organic substances; (c) by the elimination, under certain conditions, of the heavier and more' viscous hydrocarbons through filtration incident to migration.

Jan 1, 1920

By M. M. Rao, P. G. Winchell

The growth rates of bainitic plates were measured at 400°C in Fe-Ni-C alloys containing 0.10 atom-fract~on nickel and 0.0012 to 0.0075 atonz-fraction carbon. The growth rates are adequately represented by where xc is nearly the atom fraction carbon of the bulk austenite and PXCy is nearly the carbon atom fractlon in the ferrlte of radiids p In equilibrium with austetzite. The form of the equation is that predicted by a model in which carbon diffusion in austernite controls the gvowth, but the numerical constatnt is two orders of magnitude below that suggested by the model. THE growth of bainitic plates in steel is often assumed to be controlled by the diffusion of carbon away from the advancing plate tip. This hypothesis predicts that the growth rate will increase as the carbon content of the austenite, xCz, is reduced toward the carbon content of the saturated ferrite comprising the plate tip, PxCY The growth rate should vary approximately as (xCg- pxCy)-1. Experimental observation of the growth behavior at low carbon levels should provide a significant test of this model. An alloying element in addition to carbon is required so that low-carbon austenite can be experimentally observed while undergoing bainitic transformation. Nickel was selected. The presence of nickel complicates the interpretation of the data in two ways: First, diffusion of nickel during the transformation would make analysis very difficult. Nickel is assumed immobile during the transformation. Second, nickel affects the solubility of carbon in ferrite and austenite in equilibrium. This effect has been evaluated.' At the completion of our experimental work Goode-now et al.2 published data in essential agreement with the observations to be reported here. Since their discussion is abbreviated and their data are scanty in the region of interest, we believe the present work is of significance. I) THE MODEL OF BAINITIC PLATE GROWTH The rate of lengthening of a plate is assumed to be controlled by the diffusion of carbon from the advancing ferrite-austenite interface into the surrounding austenite. The precipitation of carbides is assumed to be a secondary process. For ease of analysis the carbon-atom ratio,* pxCy, of austenite in equilibrium with ferrite which is convex with minimum curvature radius p, and the carbon-atom ratio, PxCY, of that ferrite in equilibrium with austenite are assumed independent of location on the ferrite-austenite interface. Since these carbon contents vary with the radius of curvature of the ferrite, p, their assumed positional independence must be held as an approximation. The consequences of these assumptions have been developed approximately by zener3 and Hillert,4 and the resulting equation for a platelet has been applied to bainite by Speich and cohen5 and Kaufman, Radcliffe, and Cohen.8 The Zener-Hillert equation* for plates is: The analysis of Hillert is supported by that of Hor-vay and cahn7 which involves no mathematical approximations but does include the assumption that the a/y interface coincides with an isoconcentration line. The solutions of Horvay and Cahn for elliptic paraboloids are replotted in Fig. 1. The shape of the paraboloid is expressed in terms of the ratio of the principal radii of curvature at its tip, A =p1/p2, which is also the ratio of the minor to the major axis of the elliptic cross section. The Zener-Hillert equation for plates is also plotted. The agreement is within a factor of two for (pxyaCr - xyC )/(xyC - PxCaY) between 0.5 and 100. This is the range of interest here and in most other work on bainite. The original form of the Zener-Hillert equation was the form given above with the right-hand side replaced by (pxCya -xCy)/(PxCya). This replacement is not appropriate here. 11) THE EXPERIMENTAL PROCEDURE Alloys were prepared and three kinds of experiments carried out. Continuous-cooling-transformation experiments were carried out on wires by measuring temperature and resistance during continuous cooling. Isothermal-transformation experiments were carried out on wires by measuring electrical resistance as a

Jan 1, 1968

By B. M. Loring, I. R. Krame, F. M. Walters

NO observations on the mechanical properties of man-manganese alloys have been published since pure manganese became readily available, either distilled manganese or electrolytic manganese. The purpose of this investigation was to determine whether iron-manganese alloys are essentially brittle, as reported by Hadfield,' or whether the lack of ductility observed was due to impurities in the alloys that he studied. Experimental Methods The alloys were melted in a roo-lb. high-frequency induction furnace with a magnesia crucible, using ingot iron and electrolytic manganese. The heats were split, the first giving six 18-lb, ingots and the second three. Each successive heat was higher in manganese and about 0.3 per cent silicon was added as ferrosilicon. The alloys forged without difficulty and were given a 9' per Published by permission of the Navy Department. Manuscript received at the office of the Institute June 28. 1941. Issued as T.P. 1369 in Metals Technology. September 1941. * Division of Physical Metallfirgy Naval Roscarch Laboratory. Anacostia Station Washington. D. C. 1 References are at the end of the paper. 4 cent reduction to ¾-in. rounds. The chemical analysis of the alloys is given in Table I. The forged rods were homogenized for 224 hr. at r150°C. (2100°F.) and air-cooled. The alloys were tested in two conditions of heat-treatment: (I) as normalized from 870°C. (1600°F.) and (2) normalized from 870°C. and tempered for I hr. at 540°C. (Iooo°F.) and air-cooled. The tensils specimens were 0.505 in. in diameter with a 2-in. gauge length, and the impact specimens were v-notch Charpy. The proportional limit and yield strength were taken from the stress-strain diagrams drawn by a Peters recorder. The data obtained from the tensile test and the hardness measurements are given in Table 2. Specimens that were normalized are designated by N; those that were normalized and tempered by T. Alloy G was tempered after forging (D).

Jan 1, 1942

By B. M. Loring, I. R. Krame, F. M. Walters

NO observations on the mechanical properties of man-manganese alloys have been published since pure manganese became readily available, either distilled manganese or electrolytic manganese. The purpose of this investigation was to determine whether iron-manganese alloys are essentially brittle, as reported by Hadfield,' or whether the lack of ductility observed was due to impurities in the alloys that he studied. Experimental Methods The alloys were melted in a roo-lb. high-frequency induction furnace with a magnesia crucible, using ingot iron and electrolytic manganese. The heats were split, the first giving six 18-lb, ingots and the second three. Each successive heat was higher in manganese and about 0.3 per cent silicon was added as ferrosilicon. The alloys forged without difficulty and were given a 9' per Published by permission of the Navy Department. Manuscript received at the office of the Institute June 28. 1941. Issued as T.P. 1369 in Metals Technology. September 1941. * Division of Physical Metallfirgy Naval Roscarch Laboratory. Anacostia Station Washington. D. C. 1 References are at the end of the paper. 4 cent reduction to ¾-in. rounds. The chemical analysis of the alloys is given in Table I. The forged rods were homogenized for 224 hr. at r150°C. (2100°F.) and air-cooled. The alloys were tested in two conditions of heat-treatment: (I) as normalized from 870°C. (1600°F.) and (2) normalized from 870°C. and tempered for I hr. at 540°C. (Iooo°F.) and air-cooled. The tensils specimens were 0.505 in. in diameter with a 2-in. gauge length, and the impact specimens were v-notch Charpy. The proportional limit and yield strength were taken from the stress-strain diagrams drawn by a Peters recorder. The data obtained from the tensile test and the hardness measurements are given in Table 2. Specimens that were normalized are designated by N; those that were normalized and tempered by T. Alloy G was tempered after forging (D).

Jan 1, 1942

By Franklin G. Pardee

IN 1920 the Minnesota Tax Commission estimated a reserve of 1,341,674,538 long tons of iron ore in Minnesota, the Michigan State Tax Commission report showed 199,092,855 long tons in reserve in that state, and the Wisconsin Geological Survey set the Wisconsin reserves at 21,500,000 long tons. The total reserve that year for the Lake Superior District amounted to 1,562,267,393 long tons. Ten years later the reserves of iron ore in these same districts were Minnesota 1,235,227,510, Michigan 168,349,823, and Wisconsin 23,000,000, or a total of 1,426,577,333 long tons. The decrease in ore reserves in this ten-year period was 135,690,060 long tons, but the shipments were 520,746,975 long tons. In other words, the ten-year depletion in reserves was only 8.68 per cent. If similar conditions carry into the future this calculation would indicate a life for the ore reserves of the Lake Superior region of over 100 years.

Jan 1, 1933

By A. J. Teplitz, J. K. Rodgers, E. M. Pohoriles

This note is presented in order to call attention to a newly developed laboratory apparatus that appears to have interesting possibilities for the study of lost circulation of the pressure-parting type, for a more realistic evaluation of sealing materials for this type of loss, and for investigation of other aspects of hydraulic fracturing. A study of lost circulation, conducted jointly by operating divisions of the Gulf Oil Corp. and the Gulf Research & Development Co., has been in progress for the past few years. Earlier phases of the study dealt with mechanical factors contributing to loss of returns in laminar type sediments.' One aspect of this type of loss which has been widely discussed in the literature and elsewhere concerns the geometry of the fractures into which such losses occur. This subject is not merely a philosophical one, but has an important bearing on procedures for combating lost circulation difficulties and on other well operations. The further course of the collaborative studies previously mentioned has produced some information on this subject which, though limited in amount, is believed to be significant. In several typical cases of lost circulation in laminated shale and sand formations, the wells have been surveyed with instruments2,3 capable of detecting the points of loss with considerable accuracy. These wells were located in the Gulf Coast of Texas and Louisiana, in the Texas Panhandle, and in the Rocky Mountain area. In each of these instances the loss was shown to be occurring at some distance removed from the bottom of the hole and sharply confined to a very narrow interval, less than 1 ft in thickness. It is rather difficult to imagine that fractures of a vertical nature' would be of the limited extent indicated by the surveys in these wells. Furthermore, the high rates of loss at relatively low pressure differentials observed in some of these instances together with the narrow intervals involved would appear to require the radial flow pattern which would be associated with a more or less horizontal fracture plane. In view of the foregoing observations and records of successful squeeze cementing operations, in attempting to construct a laboratory apparatus For simulating pressure induced lost circulation, it was decided that the design should be based on a horizontal type of fracture. It was realized that5,6 Vhe production of horizontal fractures in a formation with non-penetrating fluid requires some mechanism for transmitting vertical components of the hydraulic forces to the plane of parting. This was accomplished, as will be evident in the description of the apparatus that follows, by providing recesses in the wall of the borehole which are believed to be representative of wellbore configuration found in Gulf Coast wells. The possible influence of such borehole irregularities on both pressure fracturing and the treatment of lost circulation appears to have been neglected in many studies of these subjects. It is believed that the present apparatus, incorporating features that take into account some of the factors mentioned, will provide means of gaining a further understanding of pressure induced fracturing and possibly for more realistically evaluating the numerous sealing agents, particularly the non-time-setting materials employed in treating the pressure-parting type of loss. DESCRIPTION OF APPARATUS The test cell used in the laboratory investigations is shown in Fig. 1. A schematic diagram of the entire system is shown in Fig. 2.

Jan 1, 1956

By A. Raman

The Nb-Co system was nuestigated in the range 10 to SO at. pct Co with X-rays. A pt phase with the W6Fe.r-type structure occurs in the system between 46 and 52 at, pct Co. Its unit-cell dimensions are nearly identical to those of the p Phases found in the Nb-Fe and Nb-Ni systems. Two Laves phases, one having the MgZnz-type structure and the other the MgCuz-type structure, already t-eported in the literature, are found to exist in the system. The ,l.IgZnz-type phase occurs between 62 and 64 at. pct Co. A MgNi2-type Laves phase, reported in the literature, is no! obtained. A binalry phase is found to exist belozv I000C around 82 at. pct Co. THE cobalt-rich side of the system Nb-Co has been repeatedly investigated by previous inestiators" and the following intermediate phases are known to occur: NbCo, which crystallizes in the MgCu2-type structure and Nbc03,' reported originally by Wall-bam, which has the MgNiz-type structre. Jordan and uwez' as well as lliott' were unable to find the MgNiz-type phase. Two phases, designated as x and y, were reported by Saito and eck.' The phase x was inferred to have a narrow composition range near 77 at. pct Co. No published work is known to the author which reports the investigations in the niobium-rich portions of the system. This paper presents the results of an investigation in the Nb-Co system between 10 and 80 at. pct Co. EXPERIMENTAL PROCEDURE Two or three grams of the alloys under investigation were prepared using niobium (99.9 pct +) and cobalt (98.8 pct + with 0.14 pct Fe and and 0.03 pct C) in a tungsten-electrode arc furnace under commercial argon atmosphere. They were then wrapped in molybdenum sheets and annealed for a period between 5 days and 1 week at 1300°C in high vacuum (10-" orr) or in evacuated quartz amules for 2 weeks at 1000°C. Powders of -325 mesh size were prepared for X-ray work by crushing and grinding the specimens. Subsequent reannealing of the powders was not undertaken since most of the alloys were brittle and broke easily. X-ray powder patterns of the as-cast and annealed samples were prepared in a Siemens cylindrical camera (57.3 mm radius) with Cr-K, radiation. A Siemens diffrac to meter was used to get the X-ray patterns of some new phases. Metal log raphic examination of the alloys supplemented the X-ray findings. RESULTS The results of the X-ray and microstructural analysis Of the alloys are in in Table I. The lattice parameters of the phases are listed in Table 11 for quick reference. A set of micro photographs in Fig. l(n) to (j) show the microstructures of some alloys. A probable equilibrium diagram is drawn in Fig. 2

Jan 1, 1967

By Robert Mehl

RELATIVELY few data have been collected on the rates of diffusion in ternary solid solution systems. In general it does not seem worth while to gather extensive data for such systems until the factors that determine the rates of diffusion in binary systems are better understood. But the rates of diffusion in a ternary system of limited solid solubility, in which the terminal solid solution is in equilibrium with an intermediate phase and may thus be represented as a quasibinary system, represents a case of special interest. In this case, where by reason of the association of the two solute metals in an intermediate phase a special attraction of the two solute atoms may be safely assumed, some interaction of these atoms during simultaneous diffusion in the solvent lattice might be expected. It has frequently been proposed that molecular solid solutions exist in quasibinary and in other ternary (and binary) solid solutions. There is no direct evidence for such solid solutions; arguments based upon the supposed anomaly in certain physical properties1 are hardly important; unexpected density relationships have proved deceptive ;2 suggestions of molecular solid solutions have been made on the basis of solution laws in their application to certain systems, but without result;3 attempts to find lattice parameters in the solid solution Al-MgZn2, which cannot be calculated from the separate effects of magnesium and zinc and might therefore be taken as evidence for a molecular aggregation, have given negative results.4 Fundamentally, methods for the determination of the state of molecu¬lar aggregation in solution depend upon the kinetic behavior of the par-ticles constituting the system. If it could be shown that the two solutes in a quasibinary ternary system diffuse in molecular proportions, despite a radical difference in the separate rates of diffusion of each solute when diffusing alone in the solvent lattice, some basis for the concept of molecu-lar solid solution would be afforded. Freche5 examined the rates of independent and simultaneous diffusion of magnesium and silicon in

Jan 1, 1939

By W. Mont Ferry

It is impossible to speak in exact terms of the effect that selective flotation has had, is having, and may have on the State of Utah. Its results enter into the economic structure of the state in so many ways and its ramifications are so widespread, that every line of industry is affectcd. Some effects can be definitely determined; others can be reasonably approximated; but the effect as a whole can not be set out in exact figures. Utah is essentially a mining state; mining is its basic industry and always will be. Agriculture, equally a basic industry, and of course, equally vital, can be practiced on only 6 per cent. of the 85,000 square miles of its area. It follows, therefore, that the economic future of this state depends upon a development of its natural resources. About 6 or 7 years ago, the mining industry in Utah was at a low ebb. This condition was caused partly by postwar conditions and other temporary causes, but prevailed also, which was most important, because the direet-smelting ores of the state were being rapidly exhausted and the cost of treatment of complex ores was almost prohibitive. Furthermore, the wet concentration of low-grade ores was unsatisfactory and did not result in producing a good smelting product. On visualizing this situation, one of the large smelting companies in the valley had the courage, ability and faith to develop and expand the principles involved in selective flotation of complex ores. This example has been followrd by other smelting and reduction companirs and the result has changed the entire aspect of the mining industry in Utah. The utilization of the zinc in the low-grade, lead-zinc-silvrr ores was the principal prob1t.m to be solvcd. The average yearly production from the State of Utah for the 10 years beginning 1914 and ending 1923, was something less than 10,000 tons of zinc corlcentrates. This period includes the world war, when abnormal priccs stimulated production. In 1924, selective flotation began to be practiced on a considerable scale, replacing concentration by gravity and bulk flotation which had been used generally until this time. Production and Value of Zinc Concentrates The production of zinc concentrates during 1924 was approximately 24,000 tons, or twice the average yearly production of the previous 10

Jan 1, 1928

By Ming-Kao Yen

A considerable amount of work has been reported in the literature in regard to the texture and earing behavior of copper strip. The rolling texture of copper has been confirmed as (110) [112] and (112) [111], which yields ears of a drawn cup at the position 45" from the rolling direction.1-3 The recrystallization texture has been established as the cubic or (100) [001] texture, where the earing positions are at 0" and 90" to the rolling direction.4-8 It has also been reported that in the development of cubically aligned grains of copper strips, the percentage of this cubic texture increased with an increase of final reduction and final annealing temperature.8,9 A comprehensive study on H.C. copper (British commercial copper of high-conductivity quality = Cu 99.95 pct, O2 0.03 pct, Ag 0.003 pct, Fe 0.005 pct and Pb < 0.001 pct) was made by Cook and Richards.6 They concluded that the recrystallization textures could be described as one or more of the following textures: (1) a single texture (100) 10011, (2) a twin texture (110) [112] and (3) a random orientation, depending upon the previous history of the specimen concerned. The effect of various alloying additions in copper was reported by Dahl and Pawlek.10 They found that certain alloying additions, such as 5 pct Zn, 1 pct Sn, 4 pct Al, 0.5 pct Be, 0.5 pct Cd, or 0.05 pct P suppressed the formation of cubic texture. Brick, Martin and Angierll reported that the cold rolled textures due to various additions fitted a rather simple pattern. However, the recrystallization textures were subject to very considerable variations. In the discussion of this paper, Baldwin stated that deoxidized copper containing 0.02 pct P gave a complicated recrystallization texture at lower temperature. When this copper was annealed at high temperature, a single texture appeared which was described as (110) [ill] but. according to a pri- vate communication from Baldwin, this orientation reported was in error and should have been reported as (110)[112]. He also reported that the earing positions of drawn cups were at 60" to the rolling direction.12 Recently, Howald, in his discussion on the paper by Hibbard and Yen,13 reported that the rolling texture of phosphorus deoxidized copper, containing from 0.006 to 0.020 pct phosphorus, was of the pure copper type. When these coppers were annealed at lower temperatures, they exhibited a random orientation, and when they were annealed at higher temperatures they had a mixed (111)[110] and (100)[001] texture, depending on the severity of the final reduction and annealing temperature. However, the specific influence of phosphorus and other impurities on the recrystallization textures and the deep drawing properties of copper strip has not been thoroughly reported. Therefore, an attempt has been made in the present work to determine the rolling and recrystallization textures and also the earing behavior of five types of commercial copper and thereby to evaluate the effect of phosphorus and some other significant impurities on the development of texture for cold reductions of about 87 to 89 pct. Materials Used The five types of copper employed in the present investigation were two phosphorus deoxidized coppers of different phosphorus content (0.007 and 0.013 pct P), an oxygen-free copper (OFHC), an electrolytic tough-pitch copper, and a fire-refined tough-pitch copper. These materials were subjected to a thorough spectroscopic and chemical analysis. The designations and the chemical compositions were as shown in Table 1. The coppers, FA1, FA2 and FA3. were hot-forged from 3-in. billets into a ½ X 6-in. plate and cold rolled to the ready-to-finish gauge indicated below. FA4 and FA5 were hot rolled and scalped to ready-to-finish gauge. The grain size of all the materials in the ready-to-finish condition was about 0.030 to 0.045 mm. Table 2 shows the last stage of the production schedule for each copper strip used. Experimental Procedure ANNEALING, GRAIN SIZE AND HARDNESS DETERMINATIONS Specimens of each type of copper were finally annealed in air for periods of one hour at temperatures ranging from 300 to 1600°F and were subsequently cooled in air. The average grain diameter of the annealed specimen was estimated by comparing with a standard grain size chart. Hardness was determined on the Rockwell 15 T scale. CUPPING TESTS Cups were made in a blanking and drawing set, in which blanks of 2-in. diam were drawn to a cup of 1.25-in. diam with an average depth of about 0.75 in. The clearance between the punch and die was about 0.032 in. The ears of the cup were measured with a special fixture which read the height of ears to one-thousandth of an inch on every ten-degree interval along the circumference of the cup. POLE FIGURES The usual transmission diffraction method with unfiltered copper radiation was employed to determine the pole-figures of the specimens cold-rolled or annealed at 900°F. All the pole-figures were derived from the positions of intensity maxima on 111 diffraction rings of the X ray photo-grams taken at 10 rotation of a

Jan 1, 1950

By Paul A. Beck

While the recrystallization properties of most of the practically important metals are known in considerable detail, those of lead are still relatively little known in spite of some valuable contributions in recent years. This condition probably is due to the difficulties involved in applying the usual methods of investigation. The microscopic method of discriminating between the elongated deformed grains of the familiar lenticular shape and the equiaxed recrys-tallized grains is not successful with fully refined lead: lenticular grains cannot be seen under the microscope with any amount of deformation whatever. The probable cause of this phenomenon was recognized long ago. With large deformation the time of recrystallization at room temperaturc is shorter than the period of preparation of the specimen for microscopic examination; with small deformation the deformed grains arc not noticeably elongated in the first place. However, with small cleformation the migration of the grain boundaries can be observed. The only systematic investigations yet published on the recrystallization of lead, those by R. S. Russell, 1-3 make use of the conditions just described. Russell considered recrystallization completed when no further migration of boundaries could be observed. A serious objection to this method arises from the fact that there is no evidence to support the view that grain-boundary migration results only from recrystallization. If such migration does result from other sources after recrystallization is completed—after the deformed grains have been replaced by new unde-formed grains—the "time of recrystallization" as determined by Russell may be too long. Furthermore, the method is subject to the above.-mentioned limitation because of the unavoidable period of preparation of the sample. According to Russell, even with the fastest technique 5 min. clapsed before the deformed samples were ready for examination, and consequently no reearystallization time shorter than 5 min. could be measured. The lack of success in detecting the recrystallization of lead by the usual hardness or tensile tests is again caused by the time necessary for

Jan 1, 1940

By Paul A. Beck

While the recrystallization properties of most of the practically important metals are known in considerable detail, those of lead are still relatively little known in spite of some valuable contributions in recent years. This condition probably is due to the difficulties involved in applying the usual methods of investigation. The microscopic method of discriminating between the elongated deformed grains of the familiar lenticular shape and the equiaxed recrys-tallized grains is not successful with fully refined lead: lenticular grains cannot be seen under the microscope with any amount of deformation whatever. The probable cause of this phenomenon was recognized long ago. With large deformation the time of recrystallization at room temperaturc is shorter than the period of preparation of the specimen for microscopic examination; with small deformation the deformed grains arc not noticeably elongated in the first place. However, with small cleformation the migration of the grain boundaries can be observed. The only systematic investigations yet published on the recrystallization of lead, those by R. S. Russell, 1-3 make use of the conditions just described. Russell considered recrystallization completed when no further migration of boundaries could be observed. A serious objection to this method arises from the fact that there is no evidence to support the view that grain-boundary migration results only from recrystallization. If such migration does result from other sources after recrystallization is completed—after the deformed grains have been replaced by new unde-formed grains—the "time of recrystallization" as determined by Russell may be too long. Furthermore, the method is subject to the above.-mentioned limitation because of the unavoidable period of preparation of the sample. According to Russell, even with the fastest technique 5 min. clapsed before the deformed samples were ready for examination, and consequently no reearystallization time shorter than 5 min. could be measured. The lack of success in detecting the recrystallization of lead by the usual hardness or tensile tests is again caused by the time necessary for

Jan 1, 1940

By Henry Louis

IN the discussion on the paper on subsidence by R. V. Norris and H. W. Montz (Teohnical Publication No. 153), H. N. Eavenson has been good enough to quote some of my views regarding the phenomena of subsidence; he has, of course, only mentioned these briefly, and as he has not represented them quite correctly, it is evident that I have failed to make them clear. Seeing that he, and apparently some of the others who took part in the discussion, appear to hold views different from my own, I think it advisable to put my opinions down as definitely and as clearly as possible, because it appears to me at least possible that some of the differences above referred to may be differences of language and definition rather than of fact. The statements I propose to submit refer to the simplest cases, namely where an area in a practically horizontal bed has been entirely worked out. My experience has been confined to beds of bituminous coal and of ironstone, but D I do not at the moment see why there should be any difference in principle between the working of a bed of anthracite and one of bituminous coal, provided that the other conditions are the same. I wish to emphasize that I am considering the conditions of complete working out of the mineral bed with the roof allowed to come down and form goaf in accordance with the general British practice; 1 am excluding, therefore, methods of hydraulic, pneumatic, and hand stowage where extraneous material is brought in to hold up the roof. I am also excluding the case of bord and pillar working where pillars of small size are deliberately left in, apparently with the idea that these will subsequently crush and let the roof down gradually. Such a method of mining has long been discontinued in this country, indeed in Europe generally, and I venture to predict that the time will come when such a recklessly wasteful method will no longer be tolerated even in the United States. Further, I am referring entirely td static conditions after the mineral bed has been worked out and the ground has come to rest; the phenomena that occur during the course of extraction are much more complicated, and these I am not discussing here. Under these conditions, I have

Jan 1, 1929

By John R. Lotz

DEVELOPMENTS in Iran currently arousing interest in a considerable portion of the world, particularly on the part. of that country&apos;s immediate neighbor on the North and in our own country, an inseparably related to and largely dependent upon the government&apos;s attempts to strengthen its economy and improve the standard of living of its people. These efforts are encompassed by provisions of the Seven-Year Development Plan recently enacted and not, in the process of implementation. It is a fine example of what one financially sound but extremely backward and poorly equipped country has undertaken to do on its own account and with its own resources. This Seven-Year Plnil was formally authoriztld by an act of the Iranian Parliament in February 1948. Its stated objects are to carry out such plans for the development of the country and its economy as ail1 raise the standard of livinc: and standard of education of the people, and re- duce the cost of living. A seven-yrar program for carrying out the work within the limits of appropriations was assigned under the law. The total amount to be expended during the seven- year period was fixed at the equivalent of $670 millioil at current rates of exchange.

Jan 1, 1950

By Reichmuth, Donald R.

Most brittle solids are relatively weak in tension and this weakness can be very significant in determining their performance in structures and excavations. Consequently, accurate knowledge of the tensile strength of brittle materials has long been recognized as important. In the past, measurements of the tensile strength of materials such as concrete, ceramics, and particularly rock have been hindered by problems encountered in fabricating test specimens and in accurately loading them. These difficulties have resulted in a scarcity of published tensile strength data. This can be readily seen in tabulations such as Wuerker&apos;s "Annotated Tables of Strength and Elastic Properties of Rocks.

Jan 1, 1968

By J. T. Berling, J. B. Conway

MANY studies have been devoted to the correlation of low-cycle fatigue behavior. Several of these have also been concerned with the identification of an effective approach to the prediction of low-cycle fatigue behavior from short-term tensile data. Perhaps the first such approach was that reported by coffin1 in the form: where is the plastic strain range, Nf is the number of cycles to failure, and c is a constant characteristic of a material. In this analysis by Coffin it was reasoned that in a short-term tensile test the value of Nf could be considered as equal to a , in which case the value of c is interpreted as the tensile ductility, f, measured in such a test. If, therefore, the Coffin equation is assumed to be applicable to a given material, it is a simple matter to predict the low-cycle fatigue behavior. Once the tensile ductility is known, this point is located at Nf = 1/4 on a log-log plot of vs Nf and a line is drawn through this point with a slope of to yield a prediction for the fatigue life. Actually, while this equation is quite useful it is not generally applicable, for experiment has shown that the value of —$ does not reflect the relationship between and Nf for all materials or even for a given material over all temperature ranges. An equation similar to the Coffin equation was prepared almost simultaneously by Manson.2 This expression had the form: In this case the exponent on Nf was not assigned any particular numerical value in accord with the various values of this exponent which had been observed for different materials and at different test conditions. Because of this characteristic it will be recognized that little use can be made of this expression in predicting low-cycle fatigue results. A fairly effective expression for use in predicting fatigue behavior was proposed by Manson3 based on a study of numerous sets of experimental results. This relation (Method of Universal Slopes) makes use of modulus of elasticity, ultimate strength, and tensile ductility, and assumes an exponent on Nf equal to 0.6 in representing the plastic strain range contribution to total strain range. While this equation of Man-Son does not yield completely accurate results it must be recognized as being the best means available at

Jan 1, 1970

By Robert E. Green, Wolfgang Sachse

Simullaneous ultrasonic attenuation measurements of both quasishear waves propagating in single cryslals of aluminum indicate that, in the undeformed annealed state, the dislocation density is generally not uniform on all slip systems. Change oof attenuation measurements made during plastic defortnation of crystals , which possessed specific orientations ideal for studying the orientation dependence of dislocation damping, indicate that, for low strain levels, dislocation motion occurs on additional slip systems besides the primary one, even for crystals oriented for plastic deformation by single slip. THE sensitivity of internal friction measurements permits such measurements to be used successfully in studying the deformation characteristics of metal crystals. On the basis of experimental observations, T. A. Read1 was the first to associate internal friction losses with various dislocation mechanisms. Since that time further work2-&apos; has been performed and a dislocation damping theory has been formulated by Granato and Lucke.6 In the amplitude independent region, this theory predicts the attenuation a to be dependent on an orientation factor O, a dislocation density A, and an average loop length L. if is a constant, independent of crystallographic orientation. For a given crystallographic orientation, changes in dislocation density and loop length give rise to the observed attenuation changes accompanying plastic deformation. The Granato-Liicke theory suggests the investigation of the orientation dependence of attenuation measurements in hopes of obtaining information to separate dislocation motion losses from other losses.7 An experimental study of the orientation dependence of attenuation in undeformed annealed single crystals should yield an insight into the uniformity of dislocation distribution throughout the entire specimen. A similar study on crystals plastically deformed in a prescribed fashion should give information about the alterations in the dislocation distribution on the slip systems activated during plastic deformation. The possible modes of elastic waves which can be propagated in aluminum,8 copper,9 zinc,10 and other hexagonal metals" have been calculated. Associated with each mode of wave propagation are dislocation damping orientation factors, which are based on the resolution of the stress field of that particular elastic wave onto the various operative slip systems in the material. These orientation factors have also been calculated as a function of crystallographic orientation in the papers cited above. Einspruch12 obtained agreement between predicted and observed attenuation values of longitudinal and shear waves in (100) and (110) directions of two undeformed aluminum crystal cubes. He ascribed the slight deviations between predicted and observed values to a nonuniform dislocation distribution, or to other loss mechanisms. In shear deformation of zinc crystals, Alers2 found that the attenuation of shear waves having their particle displacements in the slip plane was very sensitive to the deformation, while the longitudinal wave attenuation was affected only when the wave propagation direction was not normal to the slip plane. Using aluminum single crystals oriented for single slip, Hikata3 et al. found that during tensile deformation the change of attenuation of the shear wave (actually quasishear) having particle displacements nearly perpendicular to the primary slip direction exhibited the easy-glide phenomena, while longitudinal waves did not. Similar results were reported by Swanson and Green5 during compressive deformation of aluminum crystals. These results are in qualitative agreement with the calculated orientation factors for specimens of this orientation. In well-annealed, undeformed aluminum crystals, the damping is expected to be due to dislocations vibrating on all twelve slip systems. The orientation factors associated with this initial damping will be designated by O2 and O3, where a, represents the average orientation factor for the slow shear (or quasishear) wave and O3 represents the average orientation factor for the fast shear (or quasishear) wave. The calculation of these values for aluminum crystals by Hinton and Green8 shows that they vary very little as a function of crystallographic orientation—at most, by a factor of 2.47. If the dislocation density and loop length are uniform, then in the initial undeformed state, Here the subscript zero refers to the initial value of the attenuation. Also for aluminum, the calculations8 show that the orientation factors for primary slip only, associated with each shear wave, exhibit a sharp minimum for particular crystallographic orientations. A composite plot of the two shear wave orientation factors for primary slip only is shown in Fig. 1. Since these orientation factors are associated with dislocation motion occurring on the primary slip system only, the proper condition to check these factors might be attained by slightly deforming a single crystal oriented for primary slip. For dislocation motion on the primary slip system only,

Jan 1, 1969

By Richard Miller

The investigations of large-grained specimens carried out by Polanyi and Schmid,1 Sykes,2 Goucher,3 Yamaguchi,4 Gough, Cox, and Sopwith,5 Carpenter and Elam,6 Aston,7 and others have shown qualitatively that grain boundaries restrain the deformation of adjacent crystals. But whether or not the influence of the grain boundary is confined to the glide planes intersected by the boundary has not been demonstrated in any of these investigations, nor has there been carried out any quanti-tative analysis, of the influence of a boundary on the deformation of a crystal. Indeed, the specimens employed in the previous work con-

Jan 1, 1934