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By R. A., D. L. Sponseller, Flinn

Using specially del'eloped titanium nitride crucibles and a pressurized syslem, it has been possible to determine the solzibilitv of liquid calcium in liquid iron and iron-base alloys. At 2925°F the solubility is 0.032 wt pet Ca in pure iron. The solubility is increased by aluminum, carbon, nickel, and silicon additions, and lowered by additions of gold. An inflection in the calcium-solubility curve occurs as carbon is added to iron. At approximately 0.87 Wt pet Ca the CaC, phase replaces liquid calcium, and the calcium concentration de- creases as more carbon is added to the iron. The maximum solubility, 0.36 wt pet Ca, was obtained in iron containing 10.5 wt pet Si. The data have important implications regarding the use of calcium in process metallurgy, as well as providing an interesting test of theories of metallic solutions. Reasonably good agreement is found with theories of Alcock and Richardson and of Wagner, and criteria are suggested which permit these theories to be applied more readily to systems of this type. AT the present time relatively little is known about the factors influencing solubility in liquid metals. Information of this type is important for such matters as the control of impurity levels in liquid metals, the use of magnesium in ductile-iron production, and the use of liquid-metal alloys as fuels and coolants in nuclear power plants. One important example of restricted solubility concerns the extent to which liquid calcium will dissolve in liquid iron. This is a matter of considerable interest in view of the strong potential of calcium for removing certain impurities in steel,. as well as the ability of calcium to desulfurize, inoculate, and produce spheroidal graphite in cast irons.' Since ferrous materials normally contain other elements in addition to iron, the interactions of third elements with the Fe-Ca system are of interest. In view of the foregoing, this investigation was conducted to determine the solubility of liquid calcium in liquid iron and the effects of various third elements upon the solubility. For reasons of theoretical and engineering importance, the elements investigated were aluminum, carbon, gold, nickel, and silicon. Numerous attempts were made in the early part of the present century to determine the solubility of calcium in both liquid iron and steel, employing a variety of open-melt and closed bomb-type systems.2-4 From the results of these tests Wever concluded that calcium is insoluble in liquid and solid iron.5 These investigations were unsatisfactory in that they failed to insure the presence of a liquid layer

Jan 1, 1964

By W. O. Philbrook, A. E. El-Mehairy

The reduction by hydrogen of individual particles of dense hematite implanted in beds of inert spheres is controlled by single-particle kinetics. No evidence of reagent starvation was found down to low flow rates established by pressure gradients as low as 0.01 in. H2O per- in. of depth in beds of spheres as small as 3/16 in. diam. The optimum size for most rapid reduction of beds of homogeneous ores results from the effect on reducing potential of the gas of competing factors of supply and consumption. A recent publication1 presented the results of a study of the rate of reduction of iron ore in a fixed bed by hydrogen introduced at constant pressure differential. Under these conditions the reagent flow rate varied directly with the bed permeability, which was a function of particle size and shape and bed voidage, and inversely with the temperature-dependent viscosity of the gas. The present note adds data from supplementary experiments designed to reveal whether or not any partial reagent starvation arising from a flow-dependent transport resistance in the gas phase might have been operative. Kinetic studies were made of the reduction of individual spheres of iron oxide inserted into beds of inert spheres, so that the reagent flow rate and aerodynamic conditions were again determined by bed characteristics and temperature. The experimental techniques and apparatus were similar to those previously described.' The synthetic iron ore spheres were wet-rolled by hand from powdered, reagent-grade* Fe2O3 and subsequently dried and then fired in air at 1250°C. The indurated pellets has almost no porosity as indicated by their specific gravity of 5.10. The beds were made of dense alumina spheres, closely sized to the same dimension as the iron oxide spheres, in the following diameters: 3/16, 1/4, 5/16, and 3/8 in. Each bed was hand-packed of particles of a single size to a controlled voidage of 0.32 and depth of 3 in. within a capsule having an internal diameter at least 10 times the particle diameter. A few weighed iron oxide spheres were individually planted in the central plane of the bed of inert spheres at points away from the wall. Reduction was carried out at atmospheric pressure by purified hydrogen at 670°, 800°, and 985°c. The reagent was supplied at precisely controlled pressure differentials of 0.01, 0.02, and 0.03 in. of water per in. of bed depth. This gave a range of flow rates similar to that used in the study of beds of ore and comparable with blast-furnace practice in terms of mols of reducing gas per hr per sq ft of cross-section. Viscous flow prevailed in all beds under the experimental conditions of this study. The reduced particles were checked for loss in weight and then sectioned for metallographic examination. Occasional particles were found to have contained minute internal cracks that interfered with the concentricity of the reduction interfaces, and data for such particles were rejected. An experimental rate constant for the reduction of the imbedded Fe2O3 spheres was calculated on the assumption that the rate was proportional to the metal-oxide interface area by an equation that has been found by McKewan2 to describe the reduction of single spheres

Jan 1, 1962

By N. E. Rogen, N. J. Grant

WHILE direct measurements of the growth of precipitate particles during aging is of fundamental value, few such measurements have been made. Direct measurements by means of optical or electron-microscopy and X-ray techniques are preferred, however, many of the aging studies have been based on indirect methods such as electrical resistivity and hardness. Because of the minute size of most precipitate particles (less than 1000A) the light microscope is of limited use while electron microscopy is subject to slowness, etching problems and consequent resolution problems. It is fortunate that alloys of the Nimonic type, based on Ni-Cr-Ti-Al, lend themselves to accurate and relatively easy particle size measurements. With proper balance of titanium and aluminum, the only aging precipitate is the gamma prime (r') Ni3,(Al, Ti)2 phase and this phase is the basis of the high-temperature strength of these allos.3-6 The Ni3(Al, Ti) phase is a face-centered-cubic, ordered structure with nickel atoms occupying the cube faces. Titanium atoms can replace three out of every five aluminum atoms and when substituting do so preferentially.2 Electron microscopy has shown that during aging of most of the commercial alloys of this type, precipitate particles are unusually uniform in size and distribution, and that the volume of (r') phase is large (20 pct).4,7 The aim of this investigation was to measure the growth of (y') phase during aging. In so doing, it was hoped that a clearer understanding of the aging process would be attained. X-ray line broadening was used as the measure of precipitate particle size. This technique was selected because it can measure and average the diameter of thousands of particles in one operation. The variations in hardness and matrix lattice parameter with aging were also studied and related to the particle size. EXPERIMENTAL PROCEDURE An alloy of the following composition was studied: Cr Ti A1 C Ni Wt pct 20.71 2.98 1.43 0.04 bal. At. pct 22.06 3.47 2.95 0.18 bal. The alloy, a 15- lb vacuum melt, was forged to 1/2-in. diam at a temperature of 1900" to 2200°F; was solution heat treated for 4 hr at 2000°F and water quenched; and was then aged in various ways. The ASTM grain size was 4 to 5. No (7') phase could be detected by X-ray analysis after solution treatment and electrolytic extraction. Aging was performed on 2-in. long specimens at 1400°, 1500°, and 1600°F for increasing times. One-half inch sections were removed after each time increment and were then electropolished in a solution of H3P04 saturated with chromium trioxide at a potential of 30 v and rectified with a tantalum electrode. Rockwell hardness measurements were taken using one side of the polished specimen. Matrix lattice parameter determinations were made on the other side using filtered chromium radiation references with the position of the (220) line of a silicon standard. To enable the precipitate particles of the (y') phase to be measured using X-ray line broadening techniques, it is first necessary to separate and concentrate this phase by electrolytic extraction. Extraction is necessary because the difference between matrix and precipitate lattice parameters is only approximately 0.5 pct and intensities of.the (y') phase lines are very weak relative to those of the matrix. The extraction techniques employed have been described before and found to produce a reasonably quantitative separation.398 A water solution of 15 pct H3Po4 is used at a current density of 0.5 amp per sq in. at 6 v. The precipitate particles are separated from the liquor by centrifuging and decanting and are then washed, dried and repowdered. A plot of the X-ray intensity vs diffraction angle for the (111) line of the precipitate particles was used as a measure of particle size. The intensity curve approximated the shape of Gaussian distribution function and its breadth was measured at the half height. The (220) line of a silicon standard was used to correct the measured line breadth for instrumental and other broadening errors. The Scherrer formula was used to calculate particle

Jan 1, 1961

By William E. Schoeneck

This paper presents the problem of oil-well abandonment as a group of studies involving the compilation of physical well data, the use of special curves, maps, and interpretative Procedures, in order that operations can be analyzed and means for reducing costs can be effected. Methods for the calculation of the economic limit of production and resultant oil reserves are suggested in order that profitable production may be continued and premature abandonment prevented. INTRODUCTION Purpose Extensive studies have been made and much has been written on the procedures for prospecting, drilling, completion, production and repair of oil wells, but the writer has long felt the need for a study of the procedure that should be followed when considering the abandonment of a well. The production from numerous well bores of a fluid material (a circumstance peculiar to the oil industry) that is continually decreasing in quantity leads to an increasing ratio of operating cost to production. It is for this reason that oil fields are not abandoned as a whole and detailed consideration of each well is required before it can be determined whether more is being expended than will be returned On any well or lease in question. It is the purpose of this paper, therefore, to compile, correlate, and present all matters worthy of consideration in the problem of oil-well abandonment; to suggest interpretative procedures based on such compilations, to the end that reliable estimates of reserves and life may be obtained; to show, as a result of such interpretative procedures, the possibilities for corrective measures conducive to economical production, thereby extending both profitable reserves and length of life. Scope and Approach Compiling data and outlining a study having the complexity of the problem at hand are naturally subject to the personal experiences of one who undertakes the study; however, the chosen approach and grouping of the subject material may be helpful in the consideration of abandonment problems. Consideration has been given to wells that make gas and water incident with the production of oil; but consideration has not been given to either gas wells or condensate-producing wells, for wells of the latter type have sufficient problems to warrant separate investigation. The major subdivisions of this paper-— physical considerations and economic considerations—do not imply that either of these phases can be considered independently, but rather that the two are mutually dependent and are the component parts of an engineering study.

Jan 1, 1946

By William E. Schoeneck

This paper presents the problem of oil-well abandonment as a group of studies involving the compilation of physical well data, the use of special curves, maps, and interpretative Procedures, in order that operations can be analyzed and means for reducing costs can be effected. Methods for the calculation of the economic limit of production and resultant oil reserves are suggested in order that profitable production may be continued and premature abandonment prevented. INTRODUCTION Purpose Extensive studies have been made and much has been written on the procedures for prospecting, drilling, completion, production and repair of oil wells, but the writer has long felt the need for a study of the procedure that should be followed when considering the abandonment of a well. The production from numerous well bores of a fluid material (a circumstance peculiar to the oil industry) that is continually decreasing in quantity leads to an increasing ratio of operating cost to production. It is for this reason that oil fields are not abandoned as a whole and detailed consideration of each well is required before it can be determined whether more is being expended than will be returned On any well or lease in question. It is the purpose of this paper, therefore, to compile, correlate, and present all matters worthy of consideration in the problem of oil-well abandonment; to suggest interpretative procedures based on such compilations, to the end that reliable estimates of reserves and life may be obtained; to show, as a result of such interpretative procedures, the possibilities for corrective measures conducive to economical production, thereby extending both profitable reserves and length of life. Scope and Approach Compiling data and outlining a study having the complexity of the problem at hand are naturally subject to the personal experiences of one who undertakes the study; however, the chosen approach and grouping of the subject material may be helpful in the consideration of abandonment problems. Consideration has been given to wells that make gas and water incident with the production of oil; but consideration has not been given to either gas wells or condensate-producing wells, for wells of the latter type have sufficient problems to warrant separate investigation. The major subdivisions of this paper-— physical considerations and economic considerations—do not imply that either of these phases can be considered independently, but rather that the two are mutually dependent and are the component parts of an engineering study.

Jan 1, 1946

By H. M. Howe

It has seemed to the writer that one important, and indeed sufficient reason, for our slow progress in learning the relation between the chemical composition and the physical properties of cast-iron, has been that the problem has not been attacked properly. It would be well to select the most probable working hypothesis which we can find, and proceed to test that hypothesis by comparison with observed facts, and by making new observations specially designed for such a test. Our first step, then, is to select the most probable working hypothesis ; and to attempt this selection, to state the hypothesis and its immediate corollaries, and to take some first steps toward testing it, is the object of the present paper. Its chief purpose is to bring the hypothesis to the attention of those who are more familiar with the evidence than the writer can pretend to be, and in a better position both to present new evidence and to discuss it. The hypothesis here selected is, that composition governs properties in the case of cast-iron, in the same general way and for the same reasons as in the case of steel, mutatis mutandis. This hypothesis, which of course makes no claim to originality, certainly seems reasonable and probable; its exposition and discussion are made easy by our existing knowledge of the constitution of normal or " carbon " steel; it therefore seems worthy of consideration.

Jan 1, 1902

By R. T. Mishler

I wish to express my keen appreciation of the article on the above subject by Coe and C1evenger.l It has been doubly interesting to me, for the reason that the experience recorded and the principles evolved practically parallel the results of similar investigations made by myself and others at The Lucky Tiger Mine, El Tigre, Sonora, Mex. An outline of the work at El Tigre may aid in confirming the principles expressed by Coe and Clevenger. El Tigre has the unenviable distinction of possessing a slime with a much lower settling rate than any recorded in the article discussed. Under most favorable conditions the settling rate is about one-third that reported for the Liberty Bell mill, and one-tenth that reported for the Nipissing, Golden Cycle, and Presidio mills. This slow settling characteristic of Tigre ore has necessitated careful investigation of settling phenomena throughout the various evolutions of the plant. Previous Settling Investigation at Tigre During construction work at the mill, the metallurgical engineer in charge, D. L. H. Forbes, ran a series of experiments on settling. His tests proved that deep settling tanks were not ordinarily necessary. The use of tanks 2 or 3 ft. in depth was suggested.2 Later experiments demonstrated that the following principles of settling applied to Tigre pulp.3 1. In settling dilute pulp, settling rates are independent of pulp depth. 2. In settling thick pulp, settling rates are approximately proportional to pulp depth.4

Jan 1, 1918

By J. D. Edwards

When Charles Martin Hall invented the electrolytic process for the production of aluminum, one basic requirement was a supply of pure alumina. Now, more than 50 years later, the same requirement still holds, and there are no technical straws in the wind to indicate that this situation is likely to change. Long ago, Aluminum Company of America took a number of steps to see that this country should not face shortages of alumina and aluminum in time of emergency. As one step to this end, the Company developed and used a supply of bauxite in South America in order to conserve dwindling Arkansas reserves. Another, and more a program than a step, was to investigate every type of process that might bear the possibility of utilizing the low-grade ores of aluminum that are more plentiful than bauxite. It is a long story, but the investigation included electric-furnace processes, acid extraction processes and alkaline extraction processes, with or without preliminary furnace and sinter treatments. Some of the processes developed were operated in commercial production. This work has been continuous since the first World War. The turn of the wheel came sooner than was expected when, in 1942, bauxite shipmerits through the caribbean became uncertain and hazardous through the operation of submarines. The tremendous requirements of aluminum for the war effort were consuming high-grade bauxite at an alarming rate and a national search for substitutes began. High-grade bauxites, for technical and economic reasons, have been defined as those containing about 7 per cent or less of silica. While bauxite of this grade was limited in amount in the United States, there was in sight a substantially greater volume of low-grade, high-silica bauxite not amenable to economic treatment by the Bayer process, but richer in alumina than the clays or other available low-grade ores. It was at this point, and after several years of intensive research on this particular phase of the problem, that Aluminum Research Laboratories brought to completion the invention of one of its research staff, which made practical the utilization of large reserves of low-grade bauxite in America. Bayer Process The Bayer process has been almost universally used for the production of alumina from bauxite. This process, in outline, comprises the digestion of hely ground bauxite in a solution of caustic soda (NaOH) under pressure and at an elevated temperature. Alumina in the bauxite goes into solution as sodium alumi-"ate and the impurities—oxides of iron, titanium and silicon—remain undissolved. The undissolved residue, known as "red mud,'' from its color, is separated and run to waste. AluKlinum hydrate (A12O3.3H2O) is precipitated from the solution of sodium aluminate, and the liquor containing the caustic soda and some alumina is returned to the Process for digesting more bauxite. The aluminum hydrate, after washing, is calcined at a high temperature to produce

Jan 1, 1949

By D. H. Baldwin, R. E. Reed-Hill

DURING the course of experiments involving oxygen equilibrations with a high-purity Pd-5 at. pct Rh alloy, the appearance of a subscale was noted. Most of the heat treatments in a pure oxygen atmosphere were performed at 900°C. The presence of the subscale was noted when the oxygen partial pressure was in excess of approximately 95 mm, up to 1 atm, the highest pressure used. According to available thermodynamic information' on the free energy of formation of Rh2O3 (the only reliably reported solid oxide of rhodium), this oxide should not be stable under these conditions, nor, of course, any oxide of palladium. Extraction of the subscale from the matrix was affected by treatment with aqua regia, and the resulting X-ray diffraction powder pattern is shown in Table I. This pattern is not that of Rh2O3, nor that of any known rhodium or palladium oxide. It can be indexed on a hexagonal lattice with a. = 5.22Å and co = 6.0Å. In addition to this unknown material, there was a weak Rh2O3 pattern. An X-ray fluorescence analysis of the powder gave 3214 palladium counts per sec and 5381 rhodium counts per sec, thus indicating the likelihood of a double oxide of palladium and rhodium. In view of the fact that the above result was obtained on a single sample, it is perhaps best not to insist upon the above ratio of about 0.6, but possibly to tentatively assume 0.5 or 1/1. The small amount of Rh2O3 in the X-ray pattern might have occurred on cooling, and it seems possible that the double oxide, below some temperature level, is not as stable as Rh2O3. To examine this point, some of the extracted double oxide was heated on a sheet of pure palladium in air at 900°C, and allowed to furnace-cool over a period of several hours. The X-ray diffraction pattern of the powder showed approximately the same intensity of Rh2O3 and the "hexagonal" oxide as before, but, in addition, a rather faint pattern of another crystalline species made its appearance. This finding again suggests partial transformation of the major (double) oxide to other oxides on cooling from 900°C. Application of the phase rule shows that only one equilibrium oxide (subscale) could have been present at temperature. Vacuum-fusion, oxygen analysis of the extracted subscale showed 7.7 ± 0.7 pct O. Combining this information with that of the X-ray fluorescence analysis suggests the formula PdRhO. This compound should have an oxygen content of 7.07 pct, which is within the range of error of the oxygen analysis. However, until a more careful stoichiometric study is made, it is suggested that the formula be written

Jan 1, 1965

By A. U. Seybolt

In part 111' of this series it was shown that during the selective oxidation of a 3 1/4 pct Si-Fe alloy in damp hydrogen, only silica, (observed at room temperature) as low cristobalite or low tridy-mite or both, was formed as an oxidation product. In some in- „ stances where the film was fairly thin (probably well under 100A) there was some suggestion of an amorphous form of SiO2. The present investigation of oxidation rate showed that the selective oxidation of silicon-iron can be rather complicated, and apparently impossible to rationalize in an unequivocal manner. In some temperature regions, notably near 800" and 1000°C, the data seem to obey the familiar parabolic rate law. However, at intermediate temperatures complications were noted, some of which are possibly due to the order-disorder reaction in the silicon-iron solid solution. IN an earlier report' it was shown that during the oxidation of 3 1/4 pct Si-Fe alloys in H2O-H2 atmospheres only silica films were formed in the temperature range from 400° to 1000°C in hydrogen nearly saturated with water at room temperatures, or at dew points as low as -45°C. In the work to be reported here, some observations are made on the rate of oxide film formation. As in the earlier investigation, electron diffraction patterns generally showed either low tridymite or low cristobalite or both, except for some very thin films. These sometimes showed diffuse rings, presumably due to a very small crystallite size, or in a few cases, diffuse bands probably caused by an amorphous film. EXPERIMENTAL PROCEDURE Vacuum-melted silicon iron made of high-purity materials was rolled into strips 0.014 in. thick, and cut into samples 1/2 in. wide by 1 in. long. Chemical analysis showed 3.2 pct Si and 0.002 pct C. All samples were surface abraded with 600-grit paper, were solvent cleaned, and then placed in an paper,apparatus containing a "Gulbransen type"2 micro-balance. Here the gain in weight of the samples of about 5 sq cm area could be followed as a function of time during the oxidation caused by the water in atmospheres of various controlled water-hydrogen ratios. The water-hydrogen ratios can most easily be described as varying from a dew point of 0°C (PH2O-p^2 = 6.2 x 10-3 , to K (P j -40°C (PH2O/PH^= 1.3 X 10-* Most of the experiments were conducted at the 0°C dew-point atmosphere because drier atmospheres caused so little gain in weight that the accuracy of measurement was poor. Because of this, only the data obtained at PH2O,/P,,,= 6.2 x X3 will be reported. The temperature range extended from 800" to 1000°C; and most of the oxidation runs lasted for about 24 hr. The reproducibility of any reading was about ± 1 ?, but the sensitivity of the balance was about 0.2 ?. The atmosphere, flowing at 200 cm per-min, was preheated to the furnace temperature before contacting the specimen. While the gas flow caused a measurable lift on the sample, it was ordinarily sufficiently constant so that it was not an appreciable source of error. X-ray and electron diffraction checks of the samples before and after oxidation showed no evidence of preferred orientation, either on the metal samples or on the silica films formed. EXPERIMENTAL RESULTS The data obtained are summarized in Table I, and some are given in detail in Figs. 1 to 4. In the fourth column of Table I, kp refers to the parabolic rate constant in the expression (?/cm2)2 = kpt + c [1] where ? = micrograms gain in weight kp = parabolic rate constant in units r2 /cm4 t = time in minutes c = constant It will be noted that in many cases no value for kp is given; this is because in these instances the data did not obey the parabolic rate law. The silica film thicknesses given in the last columns are values calculated from the weight gain, an average tridy-mite-crystobalite density, and by assuming a perfectly plane surface. Fig. 1 shows the data plotted in the form of Eq. [I], hence a linear plot indicates parabolic behavior. It has been frequently observed in the literature that

Jan 1, 1960

By A. L. Ph. B. Holley

(Read at the Philadelphia Meeting, February, 1878.) THIS paper is an abstract and a discussion of results obtained by the United States Test Board in experiments upon 14 brands of wrought iron, most of which are well known and of high repute.* The iron was all intended for chain-cables; it was tested in the form of bars, usually of nine sizes, from 1 inch to 2 inches round, and also in the forms of single links and short chains. Not less-than 2000 tensile tests were made, each showing elastic limit, elongation, and reduction of area. This work was done with conspicuous intelligence and fidelity, at the Washington Navy Yard, by Commander L. A. Beardslee. Some important practical results and principles which he has developed, and others which he has confirmed, will be referred to. The chemical part of this work consists of 42 complete analyses (including slag), by Mr. Blair, chemist to the Board. EFFECTS OF COMPOSITION ON STRENGTH. Variations in the physical qualities of iron may he due to different composition, or to different treatment in manufacture, or to both these complex causes. In order to determine the specific causes of variation, one class of altering conditions should be made to vary largely, while the other classes should be kept uniform. Then another class should be varied, and so on, until the value of each is ascertained. As all the irons under consideration were intended to have that purity and refinement which was deemed indispensable in chain-cables, their chemical analyses are perhaps more important in proving that physical variations result chiefly from treatment, than in pointing out the specific effects of certain ingredients. While the subject of treatment-especially the increase of strength by greater reduction in rolling-may be the more important one, it can be best appreciated after we have familiarized ourselves with the gen¬eral chemical and physical characters of the irons. The typical facts are given in the following tables. * As the present object of the Board is not to compare the products of different makers, but to discover the physical effects of various composition and treatment, the irons are designated by letters rather than by their trade names.

Jan 1, 1878

By William Klement

KNELLER' has recently reported that extensive metastable solid solutions may be obtained in Cu-Fe alloys by simultaneous vapor deposition. This note reports that solid solutions, apparently single -phase, can be obtained for Cu-Fe alloys containing 0 to 20 and 85 to 100 at. pct Fe by rapid quenching from the melt; the inability to extend the solid solubilities further is related to the liquid miscibility gap, Fig. 1, as for Cu-Co alloys.2'3 Accurate lattice spacings of the copper-rich fcc and iron-rich bcc solid solutions have been obtained. Homogeneous alloys were prepared by casting4'5 and sintering2 from elements of 99.9+ pct purity. The quenching techniques were as before,' except the iron-rich alloys were liberally covered with argon while at elevated temperatures. Flakes about 1 sq mm in area were obtained and investigated with the Debye-Scherrer technique, as previously described.2,4 All X-ray work was done at 25° 2°C using filtered copper and cobalt K radiation. Relative visual intensities of the diffraction lines for the phases in the quenched alloys are shown in Table I. The lattice spacings of the fcc structure for alloys containing up to 80 at. pct Fe are plotted in Fig. 2. The variation of these lattice parameters with composition is in good agreement with the re- of cementite spots usually present (all hkl reflections are allowed) and the ease of confusing them with ferrite or martensite reflections. Copies of the report can be obtained by writing to the Materials Research Department, Rocketdyne. 6633 Canoga Avenue, Canoga Park, Calif., 91304. A copy is also available at the Engineering Societies Library, 2nd floor, 345 East 47th Street, New York, N.Y., 10017. Photocopies, either full-size or microfilm, may be purchased from the Engineering Societies Library. sults6 of Andersen and Kingsbury, Fig. 2, although there is some disagreement in absolute value. This discrepancy may be due to the different temperatures at which the X-ray measurements were carried out and perhaps to the different extrapolation procedures. Also, Andersen and Kingsbury6 state that their lattice spacings were computed relative to the wavelengths given by Siegbahn in 1933; this reference has not been found and it is assumed that the well-known 1931 wavelengths were used, the lattice spacings then being in kx units which are converted into angstroms by the factor 1.00202. There is no support for the contention that solution of iron decreases the lattice parameter of copper, as con-

Jan 1, 1965

By J. R. Low, M. Gensamer

During the course of an investigation into the drawability of automobile-body sheet steel, it became apparent that certain advantages would be possessed by a deep-drawing steel with a very low yield strength, but almost normal tensile strength, provided a reduction in yield strength could be accomplished without sacrifice of ductility and fine grain size. It would also be desirable to have this steel free from strain-aging; that is, free from the tendency for the yield point to return after it had been eliminated by straining. It was known that, wet hydrogen treatment acted to eliminate aging, but as carried out by other investigators, at relatively high temperatures, this treatment resulted in grain coarsening. It has been established by some of the experiments reported in this paper that all of these objectives can be accomplished by treatment in wet hydrogen at a low temperature, in the neighborhood of 72o°C. The time of treatment is relatively short (about 3 hr, to completion with 20-gauge sheet) if the water content of the hydrogen atmosphere is made fairly high, say aimost 30 per cent by volume. At this temperature. the grain size remains fine in the time required. After this treatment sheet reduced the usual amount by cold-rolling has a grain size of about A.S.T.M. No. 7. The yield point is completely eliminated, and the yield strength is reduced to a very low value, in the neighborhood of 15,000 lb. per sq. in. The stress-strain curve departs gradually from the straight-line elastic part after the fashion of nonferrous deep-drawing alloys. This elimination of the yield point is accompanied by a verv low indentation hardness; for example, 32 Rockwell B or even lower. There is no aging as measured by increase in the yield strength upon aging at room temperature or for 3 hr. at 200°C., after stretching about 10 per cent in tension. Tensile strength is only slightly less than the box-annealed sheet, seldom dropping much below 40,-ooo lb. per sq. in. Elongation is practically unchanged, or increased slightly. The term yield point, as here used, refers to the phenomenon of heterogeneous deformation occurring at a substantiallv constant load, observed principally in annealed low-carbon steels. If such a steel is loaded in tension, the load increases steadily with elastic strain, suddenly falls, fluctuates slightly about some constant value for a time and then begins to rise again as deformation proceeds. The maximum initial load before the sudden drop is generally called the "upper yield point"; the value of the load where deformation proceeds at a

Jan 1, 1944

By J. R. Low, M. Gensamer

During the course of an investigation into the drawability of automobile-body sheet steel, it became apparent that certain advantages would be possessed by a deep-drawing steel with a very low yield strength, but almost normal tensile strength, provided a reduction in yield strength could be accomplished without sacrifice of ductility and fine grain size. It would also be desirable to have this steel free from strain-aging; that is, free from the tendency for the yield point to return after it had been eliminated by straining. It was known that, wet hydrogen treatment acted to eliminate aging, but as carried out by other investigators, at relatively high temperatures, this treatment resulted in grain coarsening. It has been established by some of the experiments reported in this paper that all of these objectives can be accomplished by treatment in wet hydrogen at a low temperature, in the neighborhood of 72o°C. The time of treatment is relatively short (about 3 hr, to completion with 20-gauge sheet) if the water content of the hydrogen atmosphere is made fairly high, say aimost 30 per cent by volume. At this temperature. the grain size remains fine in the time required. After this treatment sheet reduced the usual amount by cold-rolling has a grain size of about A.S.T.M. No. 7. The yield point is completely eliminated, and the yield strength is reduced to a very low value, in the neighborhood of 15,000 lb. per sq. in. The stress-strain curve departs gradually from the straight-line elastic part after the fashion of nonferrous deep-drawing alloys. This elimination of the yield point is accompanied by a verv low indentation hardness; for example, 32 Rockwell B or even lower. There is no aging as measured by increase in the yield strength upon aging at room temperature or for 3 hr. at 200°C., after stretching about 10 per cent in tension. Tensile strength is only slightly less than the box-annealed sheet, seldom dropping much below 40,-ooo lb. per sq. in. Elongation is practically unchanged, or increased slightly. The term yield point, as here used, refers to the phenomenon of heterogeneous deformation occurring at a substantiallv constant load, observed principally in annealed low-carbon steels. If such a steel is loaded in tension, the load increases steadily with elastic strain, suddenly falls, fluctuates slightly about some constant value for a time and then begins to rise again as deformation proceeds. The maximum initial load before the sudden drop is generally called the "upper yield point"; the value of the load where deformation proceeds at a

Jan 1, 1944

By Aloys IL. Wollrab

The conditions that govern the selection of a suitable type of detachable bit for the small, isolated mine, for rock work and tunnel contracting and for the large mine are quite dissimilar, therefore intelligent recommendation of a particular make of detachable bit must involve consideration of many factors. Small, isolated mines may find advantageous a detachable bit that a larger mine cannot afford to use, because of more efficient conventional steel sharpening and steel-distribution practice, but a small mine may not be able to adopt the practice of large mines because of necessary capital expenditures for equipment for detachable-bit sharpening and . shanking. The perfect detachable bit, suitable for all conditions, has not yet been developed. Conventional Drill Bit in Use That drilling speed increases as the bit gauge decreases is well known, but since small-hole drilling is the exception rather than the rule the rate of such increase is probably not so generally recognized. Tests carried out by Holman Brothers Limited1 with 7/8-in. steel show that when bit sizes are reduced from I½ in., I3/8 in., and I3/16 in-; to I3/8 in., I1/4 in.., and I1/8 in., respectively, the volume of the hole is I 5 per cent less and the drilling speed 49 per cent higher. Recent tests by the United States Bureau of Mines2,3 in hard, uniform basalt showed that a reduction in average gauge from 2.077 to I,826 in., a difference of o.25I in., gave an increased drilling speed of 65 per cent. The limits to which a drill hole may be extended depend upon the loss in gauge. Since the conventional bit with 5° and 14° clearances did not possess sufficient reaming edge to permit the smaller gauge changes that were required for small-hole drilling, experiments were made in bit construction with a view to correcting this deficiency. This resulted in the adoption of the full reaming cross bit (having full Carr charac1erist.i~~) by some mines4 In order to drill holes having a minimum taper from the collar to the bottom of the hole, full reaming center-hole cross bits with 90° cutting angles, 5° and 14° wing tapers, forged on 7/8-in. quarter-octagon drill rods, are used in the conventional drill-steel practice at Hollinger. In the steel shop close attention is given to the condition of the dies and dollies, which, combined with a rigid inspection of the finished bit, ensures as nearly a perfect bit as call be forged economically. Shop practices and costs have been discussed in earlier paper.5,6 The method by which the radii for the special dies used for forging bits of different gauge diameter are obtained so that the points and reaming edges cut circles of the same diameter has been discussed by Hibbert. Requiremnts for Detachable. Bit for Hollinger Under these it it was appar- ent that it would be difficult to introduce a detachable bit that could successfully compete with the conventional bit already in

Jan 1, 1943

By Aloys IL. Wollrab

The conditions that govern the selection of a suitable type of detachable bit for the small, isolated mine, for rock work and tunnel contracting and for the large mine are quite dissimilar, therefore intelligent recommendation of a particular make of detachable bit must involve consideration of many factors. Small, isolated mines may find advantageous a detachable bit that a larger mine cannot afford to use, because of more efficient conventional steel sharpening and steel-distribution practice, but a small mine may not be able to adopt the practice of large mines because of necessary capital expenditures for equipment for detachable-bit sharpening and . shanking. The perfect detachable bit, suitable for all conditions, has not yet been developed. Conventional Drill Bit in Use That drilling speed increases as the bit gauge decreases is well known, but since small-hole drilling is the exception rather than the rule the rate of such increase is probably not so generally recognized. Tests carried out by Holman Brothers Limited1 with 7/8-in. steel show that when bit sizes are reduced from I½ in., I3/8 in., and I3/16 in-; to I3/8 in., I1/4 in.., and I1/8 in., respectively, the volume of the hole is I 5 per cent less and the drilling speed 49 per cent higher. Recent tests by the United States Bureau of Mines2,3 in hard, uniform basalt showed that a reduction in average gauge from 2.077 to I,826 in., a difference of o.25I in., gave an increased drilling speed of 65 per cent. The limits to which a drill hole may be extended depend upon the loss in gauge. Since the conventional bit with 5° and 14° clearances did not possess sufficient reaming edge to permit the smaller gauge changes that were required for small-hole drilling, experiments were made in bit construction with a view to correcting this deficiency. This resulted in the adoption of the full reaming cross bit (having full Carr charac1erist.i~~) by some mines4 In order to drill holes having a minimum taper from the collar to the bottom of the hole, full reaming center-hole cross bits with 90° cutting angles, 5° and 14° wing tapers, forged on 7/8-in. quarter-octagon drill rods, are used in the conventional drill-steel practice at Hollinger. In the steel shop close attention is given to the condition of the dies and dollies, which, combined with a rigid inspection of the finished bit, ensures as nearly a perfect bit as call be forged economically. Shop practices and costs have been discussed in earlier paper.5,6 The method by which the radii for the special dies used for forging bits of different gauge diameter are obtained so that the points and reaming edges cut circles of the same diameter has been discussed by Hibbert. Requiremnts for Detachable. Bit for Hollinger Under these it it was appar- ent that it would be difficult to introduce a detachable bit that could successfully compete with the conventional bit already in

Jan 1, 1943

By Carl R. Davis, J. L. Willey, S. E. T. Ewing

The first tube-mill on the Rand was put into operation in May. 1904, at the Glen Deep Mine. From that time onwards, tube-mills were added to various plants, although little was known regarding the capacity of a given tube-mill when working on banket ore. Within a few years, however, the so-called standard size (length of shell, 22 ft. 0 in.; diameter, 5 ft. 6 in.) was generally used until the last year or two. Practically the only exceptions were about 30 tube-mills having a length of 16 ft. and a diameter of 6 ft., and a few open-end mills of the roller-supported type. Most of the information obtained during the last 15 years has been obtained with mills of the standard dimensions. The adoption of the tube-mill as an accessory to the stamp mill was rapid; and where 3 tube-mills were working on the Rand at the end of 1904, 244 were in use seven years later.' By 1910, good practice provided 1 tube-mill for 20 stamps of 2000-lb. falling weight. The horsepower of the motors driving the tube-mills had increased from 80 to 100 and then to 125 at this date. Broadly speaking, current practice at that date aimed at a ha1 product of which 60 per cent. was suitable for sand treatment and 40 per cent. for slime. The sand grading was +60 mesh, 6 per cent.; +90 mesh, 25 per cent.; — 90 mesh, 69 per cent.; and the slime grading +200 mesh, 2 per cent.; —200 mesh, 98 per cent. It was recognized comparatively early that the tonnage of — 90-mesh product produced by a tube-mill per 24 hr. was a convenient measure of

Jan 1, 1925

By R. S. Wagner, H. Brown

Criteria for nucleation with the aid of twin planes during crystal growth from the melt are discussed. It is shown experimentally that bismuth crystals can grow from a subercooled melt in a twinned bismdtic form. A mechanism of growth based on the presence of at least me twin plane is proposed. It is well known that faceted growth can be observed in crystals grown from the vapor phase, dilute solutions, or from the melt. Faceted growth, in which the crystal is bounded by its slowest growing faces, will occur if the growth rate is strongly orientation dependent. The addition of atom layers on a facet plane can only occur by two-dimensional surface nucleation or with the aid of an imperfection. Nucleation with the aid of dislocations was proposed by rank' and observed to be of particular importance in crystal growth from the vapor phase. Nucleation with the aid of two-dimensional imperfections, notably twin planes, was suggested by stranski2,3 and Frank.4 A twin plane, terminating at the growth interface, can form a reentrant step at which nucleation can occur at a much smaller super-saturation (or supercooling) than required for two-dimensional surface nucleation. Nucleation by a twin plane usually results in a fast growth rate along a crystallographic direction parallel to the twin plane. Such a nucleation mechanism, based on the presence of a twin plane, has been used by Dawson5 to explain the growth and morphology of sheet-like crystals of paraffin n-hectane. In recent years more evidence was found that nucleation by twin planes occurs frequently in crystal growth from the vapor phase and from dilute solutions, for example, in cadmium,' barium titanate,7 silver,8 silicon9 and gallium arsenide.10 In crystal growth from a supercooled melt, however, nucleation by twin planes has so far only been observed in materials with the diamond or zinc blende structure. Bennett and Longini11 were the first to recognize the important role a single twin plane plays in the growth of germanium dendrites. Subsequently, it was found that a prerequisite for continued propagation of germanium dendrites is the presence of two parallel twin planes which form a self-perpetuating system of nucleation sites.12 Sili- con and some III-V compounds such as InSb also grow dendritically by twin plane nucleation. It appears that the following criteria must be satisfied in order that nucleation with the aid of twin planes can occur: A) The growth form of the material must be faceted." B) The formation of twin boundaries, by a fault in layer sequence during growth, by plastic deformation, or by an accidental meeting of properly oriented crystals, must be possible. C) Twinning must form a reentrant step where the twin boundary terminates at the faceted growth interface. D) These three conditions are necessary, but in certain cases not sufficient for continued crystal growth with the aid of a twin plane. Depending on interface morphology, a combination of more twin planes is sometimes required to form a self-perpetuating system of nucleation sites. This investigation was carried out with the idea in mind that nucleation with the aid of twin planes is a more general phenomenon and should occur in those materials, grown from a supercooled melt, which satisfy the criteria outlined above. It has been found that crystals of high-purity bismuth grown from a supercooled melt can grow by the aid of a twin plane. In the first two sections the faceted growth form and the twinning elements of bismuth are discussed. In the last section prismatic crystals of bismuth, which appear to grow with the aid of a deformation twin are discussed.

Jan 1, 1962

By J. F. Held

In a study of the influence of cold rolling on mechani cal properties of steel, it was found that the specific rolling procedure influenced crystallographic orientation. Properties developed by several rolling modes were determined and related to crystallographic orientation. Sanzples were cold-rolled various amounts on a laboratory mill. When palm oil was used as a lubricant, the crystallographic orientation was homogeneous throughout the thickness of the samples. Other samples were rolled without lubrication. Variations in intensity of the recrystallization texture components persisted throughout more than 50 pct of the volume of these samples. When the average plastic strain ratio, which is dependent upon crystallogvaphic orientation, was plotted as a function of percent reduction, a maximum was found at 40 pct in the samples which contained the observed texture variation. No maximum was found for the samples with the homogeneous texture distribution. Other mechanical properties, such as tensile strength and yield strength, were not influenced by the variation in crystallopaphic orientation. MECHANICAL properties of steel sheets depend, in general, upon the structural properties of the steel. For example, the Petch equation describes the relationship between yield strength and grain size. Other properties, such as hardness, vary with chemical composition. The plastic strain ratio, or R value, has been found to be dependent upon crystallographic orientation . In the course of investigating the effect of cold rolling on mechanical properties, it was found that a previously reported relationship between percent cold reduction and R value was not always observed. Published data had shown that the optimum cold reduction for best R values is 70 pct for aluminum killed steel.' However, by altering the rolling conditions, the optimum reduction can be shifted to much lower values, or it can be moved to very high values. This paper describes the rolling conditions that lead to shifting of the optimum cold reduction. The effect of rolling conditions on the various structure parameters and the resulting mechanical properties are evaluated. EXPERIMENTAL PROCEDURE Samples of three low-carbon aluminum killed steels were cold-rolled various amounts on a 9-in.-diam 2-high laboratory mill. Hot-mill thermal practice and steel chemistries are listed in Table I. Steel A was rolled with palm oil lubrication and heavy reductions on each pass; i.e., a total reduction of 75 pct was ac- complished with a maximum of five passes. Steel B was rolled without lubrication, and light reductions were given on each pass. After approximately 75 pct reduction, it was necessary to use a small amount of light oil to achieve any additional reduction in thickness. Following cold reduction, the samples were box-annealed at 1300°F for 10 hr. The heating rate between 800" and 1300°F was 50°F per hr, and the cooling rate following the soak period was 50°F per hr. Tensile specimens were machined from the annealed material and these were used to measure yield strength, tensile strength, and the plastic strain ratio (R value). Recrystallization textures were determined by an inverse pole figure technique.*'3 Integrated intensities of the (110), (002), (112), and (222) reflections were recorded for those planes lying parallel to the sheet surface. Examinations were made on both surfaces of each sample, and also at various levels beneath each surface to approximately 0.010 in. depth by etching techniques. RESULTS R Values. The R values obtained in steels A and B are shown as a function of percent cold reduction in Fig. 1. No optimum cold reduction was observed in steel A, rolled with palm oil lubrication. It is likely, however, that an optimum reduction would have occurred had higher reductions than 88 pct been employed. The optimum reduction in steel B occurred at 40 pct. The behavior in both of these steels is quite

Jan 1, 1968

By E. P. Abrahamson II

The effect of transition element binary solid-solution additions upon the recrystallization temperature of vanadium has been investigated. Cr, Fe, Co, Ni, Mo, Ru, Rh, Os, and IY lower the recrystallization temperature, while Ti, Mn, Zr, Cb, Pd, Hf, Ta, W, Re, and Pt raise it. The majority of elements have their greatest effect in less than 0.15 at. pet. Both the rate of change of recrystallization temperature with atomic percent solute and the limit of initial linearity are found to Correlate with the free atom grozdnd state outer electron configuration of the sollte element. THE work of Abrahamson and Grant1 and Abraham-son and Blakeney2 has shown that the solute's elec- tron configuration appears to be a prime determinant of both brittle-to-ductile transition and recrystallization temperature in dilute binary alloys. It has also been shown by Abrahamson3 that the limit of linearity, i.e., the limit of initial linear change of recrystallization temperature with atomic percent solute, is also a function of the electron configuration of the solute in iron base alloys. Because of the systematic nature of the solute electron configuration correlation, it is to be expected that some systematic variation might be observed upon changing the solvent. Thus, this study of recrystallization in vanadium base alloys is the first of a series aimed at defining the role played by the electron configuration of solute in determining the recrystallization characteristics of dilute transitional alloys. PROCEDURE All alloys were made using 99.8 pct V containing 0.011 C, 0.024 N, 0.08 0, 0.006 H, 0.035 Ta, and

Jan 1, 1962