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Meeting, Oct. -04, 1913.-The sum of $1,250 was directed to be sent to the International Engineering Congress, 1915, in accordance with the terns of the Institute's guarantee. It was voted to request the several Technical Committees to recommend names of their members as sub-chairmen and members of sub-committees to co-operate with the Bureau of Mines. The Finance Committee was empowered to send all members in arrears a notice that the provisions of the Constitution, by which they cease to hold the privileges of membership if their dues are not paid by Jan. 1, 1914, become operative on that date, unless the Directors vote to extend the time in each individual case. The report of the Nominating Committee, printed on page i, was accepted. It was voted that a notice to be prepared by the Committee on Increase of Membership and an application blank for membership be printed in the front of each Bulletin. The report of the Committee on Patent Law Legislation was adopted and the Committee discharged. The Budget of the Chairman and the Secretary-Treasurer of the Colorado Local Section for the balance of the present calendar year was accepted and an appropriation of $47.75 made to them. Upon the nomination of two members of the Committee on Honorary Members, backed by 13 members of the Institute who are not members of the Board of Directors, Dr. Frank Dawson Adams, of Canada, was unanimously elected an Honorary Member of the Institute. Upon the nomination of two members of the Committee on Honorary Members, backed by 11 members of the Institute who are not members of the Board of Directors, Mr. Ezequiel Ordoñez, of Mexico, was unanimously elected an Honorary Member of the Institute.

Jan 11, 1913

Prof. H. O. Hofman, Massachusetts Institute of Technology, Boston, Mass. (communication to the Secretary): When Mr. Stetefeldt quotes me as saying that " silver-assays are uniformly made by scorification," he has evidently not understood that I was referring solely to the practice of silver-lead smelting-works. Everybody knows that silver-mills do not employ the scorification-assay for regular work ; and it is equally certain that in very few, if any, silver-lead smelting-works will the crucible-assay be found in use for determining silver. The second part of the quotation, "as it is adapted to all kinds of ores and gives excellent results unless organic matter is present," although, of course, also intended in a restricted sense, might very well be extended to a general one. Mr. Furman, in his Manual of Practical Assaying,* says, on page 123: "We believe that the Colorado practice is preferable, as most ores will yield higher silver-results by scorification." The fact that the scorification-assay is the accepted one in Colorado is strong presumptive evidence for its accuracy, as exactness would nowhere else be more jealously demanded. Mr. Stetefeldt cites Albert Arents- as a supporter of his preference for the crucible-assay, although I had already done so in favor of scorification. Looking up again the reference, I find that I was justified in quoting him, as, while Mr. Arents advocates the crucibleassay for low-grade gold ores, not on account of the greater accuracy of its results, but because it is quicker and less expensive, he condemns it§ for the assay of silver-ores, and prefers the scorifier for rich goldores, and for coppery ores, and in general for ores containing both silver and gold. As I, like Mr. Stetefeldt, have kept no detailed

Jan 1, 1895

By Eric J. Jette, Frank Foote

The unusual physical, electrical and magnetic properties of the iron-nickel alloys has given rise to a voluminous literature. This work will be reviewed critically in "The Alloys of Iron and Nickel," a monograph of the Alloys of Iron Research Series, soon to be published. In what follows we shall therefore confine ourselves to those of the earlier investigations that involved the use of X-ray crystal-structure methods. The earliest X-ray work on the iron-nickel system was by Miss Andrewsl. Using the powder method of X-ray analysis purely as a means of identifying the phases present, she located a region between 20 and 30 weight per cent nickel in which body-centered and face-centered phases coexisted. No lattice constants nor details of heat-treatment were reported. Bain2 also reported some qualitative observations. McKeehan3 made a systematic investigation over the whole of the system, giving many of his alloys four and some five different heat-treatments. In alloys furnace-cooled from 900' to 950' C. he found two coexisting phases between 0.15 and 30 per cent nickel. The precision of the lattice-constant measurements was low in comparison with what can be obtained today. Even for alloys of the same heat-treatment, differences in the constants were often between two and ten parts per thousand. In regions where no change of lattice constant with heat-treatment should occur, differences of the same order of magnitude were found. Since the maximum change in the lattice constant of nickel with change of composition is only about 2 per cent of the constant for pure nickel, these variations in the constants for a given alloy cause the points to "scatter" badly about any curve that may be drawn to represent them and it is difficult to interpret such results. In spite of this, McKeehan shows that the lattice constant of nickel increased as the iron content increased. His results for the alpha-iron phase are less conclusive. Osawa4 also investigated the entire system. For alloys slowly cooled from 1150' C. and then filed into samples for X-ray analysis, he found

Jan 1, 1936

By Frank Foote, Eric J. Jette

The unusual physical, electrical and magnetic properties of the iron-nickel alloys has given rise to a voluminous literature. This work will be reviewed critically in "The Alloys of Iron and Nickel," a monograph of the Alloys of Iron Research Series, soon to be published. In what follows we shall therefore confine ourselves to those of the earlier investigations that involved the use of X-ray crystal-structure methods. The earliest X-ray work on the iron-nickel system was by Miss Andrewsl. Using the powder method of X-ray analysis purely as a means of identifying the phases present, she located a region between 20 and 30 weight per cent nickel in which body-centered and face-centered phases coexisted. No lattice constants nor details of heat-treatment were reported. Bain2 also reported some qualitative observations. McKeehan3 made a systematic investigation over the whole of the system, giving many of his alloys four and some five different heat-treatments. In alloys furnace-cooled from 900' to 950' C. he found two coexisting phases between 0.15 and 30 per cent nickel. The precision of the lattice-constant measurements was low in comparison with what can be obtained today. Even for alloys of the same heat-treatment, differences in the constants were often between two and ten parts per thousand. In regions where no change of lattice constant with heat-treatment should occur, differences of the same order of magnitude were found. Since the maximum change in the lattice constant of nickel with change of composition is only about 2 per cent of the constant for pure nickel, these variations in the constants for a given alloy cause the points to "scatter" badly about any curve that may be drawn to represent them and it is difficult to interpret such results. In spite of this, McKeehan shows that the lattice constant of nickel increased as the iron content increased. His results for the alpha-iron phase are less conclusive. Osawa4 also investigated the entire system. For alloys slowly cooled from 1150' C. and then filed into samples for X-ray analysis, he found

Jan 1, 1936

By W. Rostoker

IN the course of the development of the phase equilibrium diagram for the system Zr-Cr,' the structure of an as-cast allov having the composition ZrCr2 was analyzed and established to be isomorphous with MgZn2 (C14, hexagonal lattice, 12 atoms per unit cell). In a recent paper on the same system, Hayes, Roberson, and Davies' report for the ZrCr2 phase an isomorphy with MgCu2 (C15, cubic lattice, 24 atoms per unit cell). It appeared that this conflict might be resolved by assuming a high and low temperature modification for ZrCr2. That this was the case with the phase TiCr2 has recently been demonstrated by Levinger." Specimens of ZrCr2 annealed at 1200°, 1100°, 994", 900°, 834", 800°, and 700°C, respectively, and subsequently quenched were examined by X-ray diffraction analysis. It was successfully demonstrated that a transition from the MgZn, structure at lower temperatures to the MgCu, structure did occur at some temperature between 900" and 994°C. Table I lists the observed structures at the various annealing temperatures. In Table II, a summary of line spacings and intensities is given for each of the allotropic modifications. The first six lines of the MgCu2 structures have been located in the table to illustrate the close similarity between the patterns. Lattice parameters of the two modifications were calculated by a least squares solution of equations for interplanar spacings for a series of high angle lines. The results are as follows: MgZn2 type - c = 8.262 kX, A = 5.079 kX. MgCu2 type — a = 7.195 kX. It is interesting to note that TiCr2 behaves in reverse fashion yn that the MgCu, structure is the low temperature modification and the MgZn2 structure is the high temperature modification. References lR. F. Domagala, D. J. McPherson, and M. Hansen: This issue p. 279. 'E. T. Hayes, A. H. Roberson, M. H. Davies: Trans. AIME (1952) 194, p. 304; Journal of Metals (March 1952). 3B. W. Levinger: Trans. AIME (1953) 197, pp. 195-196; Journal of Metals (February 1953).

Jan 1, 1954

By W. O. Milligan, J. L. McAtee

THE constitution and structure of the hydrous forms of aluminum oxides and hydroxides have been studied in the laboratory of the Depart¬ment of Chemistry at Rice Institute for almost three decades. Progress reports have been made from time to time 13,17,18 summarizing and evaluating the existing state of knowledge concerning the complex inorganic system A12Oa-H2O. X-ray and electron diffraction analysis, together with dehydra¬tion isobars and isotherms, have been the most useful methods for increasing the understanding of the structure and interrelationships of the various forms of alumina and aluminum hydroxides. The purpose of this paper is to bring up to date the information now available, in the hope that a clearer understanding of the structures of these materials may prove useful in aiding mineralogists and geologists in studies of the genetic significance of the aluminum hydroxide minerals, and possibly of the closely related clay minerals. Early investigators found the system alumina-water to be confusing, since, prior to X-ray diffraction examination, it was not possible to clearly identify and characterize the various crystalline forms. One could not be certain as to whether or not different investigators were working with the same chemical individuals. In later studies, including some from the authors' laboratory, addi¬tional confusion resulted from difficulty in preparing pure samples of the various aluminum hydroxides and in obtaining relatively large crystals of dimensions above the colloidal range of particle size. Even at present, it is difficult to establish sets of interplanar spacings for the several forms of the aluminum hydroxides, as illustrated by the 29 different X-ray diffraction pat¬terns listed in a current publication. The nomenclature of the aluminum hydroxides is also extremely confus¬ing, inasmuch as two different systems are employed by large groups of in¬vestigators. Plans are being made to formulate a uniform system of nomen¬clature but in this report the designations employed will agree with previous papers from the same source.13,17,18 Four forms of crystalline aluminum hydroxides may be considered to be well defined and recognized, which, together with hydrous alumina "amor¬phous to X-rays," comprise an exceedingly complex inorganic system. Several

Jan 1, 1952

By Paul A. Farrar, Harold Margolin

The Ti-Al-V system has been delineated from 50 to 100 wt pct Ti and front 600 to 1400°C by X-ray and ntetallographic techniques. Isothermal sections were delineated at 600, 700, 800, 900, 1000, 1100, 1200, 1300, and 1400°C. X-ray and metallographic evidence indicated the presence of two phases and in addition to those reported by previous investigators of the ternary system'-3. T HE titanium-rich region of the Ti-Al-V system as originally proposed by Rausch et UZ, and Jordan and Duwez3 was based on the binary Ti-Al diagram as proposed by Bumps et uZ. As additional phases have been shown to exist5-' in the region previously thought to be all a, the titanium-rich region of the Ti-Al-V system is open to serious question. Therefore, in order to determine the effect of the indicated changes in the Binary Ti-Al system on the ternary Ti-Al-V system the present investigation was initiated. EXPERIMENTAL PROCEDURE The experimental procedures in this investigation are the standard techniques used in the study of titanium-alloy systems which have been described in detail previously.1° Consequently, only details pertinent to the present work are discussed. The alloys employed for the delineation of this system were prepared from titanium obtained from the Bureau of Mines (73 BHN) 99.99 pct Al and 99.7 pct V, by the consumable arc-melting technique. The titanium was premelted into buttons of 25 g because spattering during the first melt caused uncontrollable loss of alloying constituents. Typical analyses of the material used have been reported elsewhere Attempts to hot roll the alloys prior to heat treatment were made on the first series of alloys prepared, but as the area of extensive hot workability was fairly restricted, see Table I, this practice was discontinued. The times of isothermal annealing are given in Table 11. A preliminary heat treatment of 96 hr at 1000°C was used prior to heat treatment at lower temperatures. The standard techniques used for polishing specimens involved belt-grinding, grinding on emery paper, polishing electrolytically, and etching with Remington "A" etch. In the low-alloy region it was found that the oRo etch, developed by Ence and Margolin,o gave better contrast between phases. Where this procedure did not differentiate between phases clearly, the method of stain etching developed by Ence and was used. It has been previously reported15 that filing of titanium alloys is not desirable for producing X-ray powders, since the powder becomes contaminated by the file material. Therefore, for those samples not brittle enough to Crush, the procedure described below was used. The specimen was wrapped in molybdenum sheet and placed in a vacuum system and evacuated to 0.03 p. Palladium-pur if ied hydrogen was then admitted to the system until a partial pressure of 5o Cm of H was reached. The specimen was heated in the system to the temperature of original heat treatment and was slowly cooled over a period of 3 hr to 400°C while the partial pressure of hydrogen was maintained. The sample was removed from the system after it had completely cooled and was crushed to a powder of 230 to 270 mesh. The powder, wrapped in molybdenum sheet, was dehydrogenated at the temperature of original heat treatment until a partial pressure of 0.03 p was maintained in the system for at least 1/2 hr. The tube containing the powders was quenched in iced brine while still connected to the vacuum system. After dehydrogenation, the powder, except for the

Jan 1, 1962

By R. J. Quigg, G. S. Doble

Commercial stress -relieved TD Nickel bar was shown to retain room- and elevated-temperature tensile strength after exposure up to 2501°F. Cold swaging increased both room -temperature and 2000°F tensile strength. After annealing at 2500°F the strengthening due to swaging was retained at 2000°F hilt eliminated at room temperature. Annealing produced changes in hardness and X-ray half peak width indicating the presence of recovery processes as 1071° as 1000°F but no recrystallization of swaged material was noted at any temperature. In contrast to swaging, rolling induced a recrystal-lized structure after annealing. The tensile strength of this recrystallized structure was comparable to the cold-worked condition. High-temperature tensile properties of as -received bar were highly anisotropic with the transverse tensile strength being one fifth the longitudinal value. The aniso-/ropy is affected by working direction and may he partially reversed by changing the direction of metal flow. The divergence in tensile strength, beginning above 550°F or- approximate one third the absolute melting point, is strain-rate dependent. T D Nickel is a commercial dispersion-hardened alloy containing 2 vol pct thoria. The dispersion, consisting of spherical particles 0.030 to 0.050 in diameter with an interparticle spacing of less than 1 is reported to maintain stable properties up to 2400°F.1 This stability of second phase results in maintenance of elevated-temperature strength at higher temperatures and longer times than normal nickel-base superalloys.2 The purpose of this paper is to describe the effect of various mechanical working operations on the strength and microstructural stability of TD Nickel bar. MATERIAL AND PROCEDURES All material used in this study was commercial TD Nickel bar. This material is produced by a chemical process which results in a nickel powder containing a dispersion of thoria particles. The powder is then pressed, sintered, extruded, and subsequently worked to bar stock. Three starting materials from three separate lots were used: as-extruded bar. 1-in.-diam stress-relieved bar, and 1/2-in.-diam stress-relieved bar. Since TD Nickel bar stock is cold-worked without a recrystalliza-tion anneal, the accumulated deformation or degree of cold work in these materials increases as the bar diameter decreases. Some of the 1/2-in.-diam bar was swaged to 1/4 in. diameter at room temperature in order to produce an as-worked condition for comparison with the stress-relieved stock. Tensile testing was performed on an Instron Tensile Tester at a constant crosshead speed of 0.020 in. per min. The 0.2 pct offset yield strength was measured from the load-crosshead movement plot. Specimen gage dimensions were 0.080 in. in diameter by 0.40 in. in length, producing a strain rate of approximately 0.050 min-1. Specimens were tested in air and heated within a resistance-wound furnace controlled to ±5°F. A 15-min soak at temperature was employed before testing. Samples were heat-treated in air and specimens machined after exposure with sufficient material removed to eliminate any surface contamination. X-ray line breadth was determined from a diffractometer scan of a transverse face of a bar using copper K, radiation. Metallographic preparation utilized standard mechanical polishing with Carapella's etch. Specimens for electron microscopy were electropolished in a 1:7 sulfuric/methaol solution and chromium-shadowed collodion replicas prepared. RESULTS AND DISCUSSION I) Effect of Elevated-Temperature Exposure on the properties of TD Nickel. The effect of various elevated-temperature exposures on the room-temperature tensile strength of TD Nickel is shown in Table I. In the unexposed condition the tensile strength, reduction in area, and hardness all increase with increasing accumulated deformation while the elongation decreases. After exposure at 2500°F the strength of all three materials decreases to about 65,000 psi and the elongations increase slightly. The apparent increase in strength of the 1-in. bar after a 2000°F treatment is probably experimental scatter. These results indicate that the room-temperature strengthening due to additional deformation is annealed out upon elevated-temperature exposure. In contrast to the room-temperature data, the 2000°F tensile strengths increase in order of increasing deformation even after exposure. Although some loss of strength occurs after exposure, much of the effect of working is still maintained at 2000°F. The room-temperature hardness after various

Jan 1, 1965

By H. l. Burghoff, J. S. Porter

This paper presents the results of an investigation of the effect of cold-working and annealing treatments upon the occurrence of preferred orientation in annealed brass wire. The subject has received less consideration than has the same phenomenon in annealed brass sheet or strip, and perhaps very properly so in view of the obvious and undesired results obtained in the forming or drawing of strip having preferred orientation, which results are in contrast with the lack of any spectacular visual evidence in wire. The factors of cold-working and annealing that control preferredness in strip are naturally expected to function similarly in wire. Indeed, one might expect the condition to be commoner in annealed wire, because the severity of the cold-working between anneals in commercial Practice is usually much greater for wire than for strip. For example, a wire that is to be finished in the annealed condition on a diameter of 0.040 in. is commonly subjected to a final reduction of 90 per cent between the last two anneals, the large reduction being accomplished in the successive drafts of a multiple-die machine. Wire for rivets, for instance, on 0.125-in. diameter, although given a slight reduction of about Io per cent after the final anneal, may have been given a prior reduction of 75 to 80 per cent. Barrettl states the fiber axis of annealed 70-30 brass wire to be [111], with some indication of [IOO] as a secondary fiber axis. Croft and Sachs2 have reported briefly on some differences in brass wire with random and with preferred orientations. They showed statistical plots of the twin-band angles with respect to the wire axis or direction of drawing as observed on an axial plane. They also pointed out that the resistance of the wire to corrosion-cracking when externally stressed and exposed to a mercurous nitrate solution decreased as the degree of the preferred orientation increased. Material and PRocedure All the wire for the investigation was processed from one portion as cut for extrusion from a cast billet of the following analysis: 70.13 per cent copper; 0.01 lead; 0.01 iron; 0.02, nickel; 29.83 zinc (by difference). The billet section, 8 in, in diameter, was extruded hot to 3/4-in. diameter, after which it was processed by alternate cold-drawing and annealing treatments as indicated in Fig. I. The earliest anneals in process were at about 1100°F. and the next to the last reductions by drawing were 58 per cent. The diameter of the finally annealed wire was 0.132 in. Semifinal anneals were at 800°F., 950°F. and 1100°F. and reductions of 47.5, 74, 83.5 and 89.5 per cent were employed in drawing to 0.132 in. The final anneals were at 87s°F., 1050°F. and 1250°F. and were

Jan 1, 1944

By H. l. Burghoff, J. S. Porter

This paper presents the results of an investigation of the effect of cold-working and annealing treatments upon the occurrence of preferred orientation in annealed brass wire. The subject has received less consideration than has the same phenomenon in annealed brass sheet or strip, and perhaps very properly so in view of the obvious and undesired results obtained in the forming or drawing of strip having preferred orientation, which results are in contrast with the lack of any spectacular visual evidence in wire. The factors of cold-working and annealing that control preferredness in strip are naturally expected to function similarly in wire. Indeed, one might expect the condition to be commoner in annealed wire, because the severity of the cold-working between anneals in commercial Practice is usually much greater for wire than for strip. For example, a wire that is to be finished in the annealed condition on a diameter of 0.040 in. is commonly subjected to a final reduction of 90 per cent between the last two anneals, the large reduction being accomplished in the successive drafts of a multiple-die machine. Wire for rivets, for instance, on 0.125-in. diameter, although given a slight reduction of about Io per cent after the final anneal, may have been given a prior reduction of 75 to 80 per cent. Barrettl states the fiber axis of annealed 70-30 brass wire to be [111], with some indication of [IOO] as a secondary fiber axis. Croft and Sachs2 have reported briefly on some differences in brass wire with random and with preferred orientations. They showed statistical plots of the twin-band angles with respect to the wire axis or direction of drawing as observed on an axial plane. They also pointed out that the resistance of the wire to corrosion-cracking when externally stressed and exposed to a mercurous nitrate solution decreased as the degree of the preferred orientation increased. Material and PRocedure All the wire for the investigation was processed from one portion as cut for extrusion from a cast billet of the following analysis: 70.13 per cent copper; 0.01 lead; 0.01 iron; 0.02, nickel; 29.83 zinc (by difference). The billet section, 8 in, in diameter, was extruded hot to 3/4-in. diameter, after which it was processed by alternate cold-drawing and annealing treatments as indicated in Fig. I. The earliest anneals in process were at about 1100°F. and the next to the last reductions by drawing were 58 per cent. The diameter of the finally annealed wire was 0.132 in. Semifinal anneals were at 800°F., 950°F. and 1100°F. and reductions of 47.5, 74, 83.5 and 89.5 per cent were employed in drawing to 0.132 in. The final anneals were at 87s°F., 1050°F. and 1250°F. and were

Jan 1, 1944

By P. Duwez, C. B. Jordan

The phenomenon of the change of volume of pressed powder compacts upon sintering is well known in the field of powder metallurgy. Depending upon the metal or metals involved and the pressure used in forming, a compact may, in the course of time of sintering at a given temperature, expand mono-tonically, contract monotonically, or first show a volume change of one sign followed by a change of the opposite sign. It is clearly desirable to have accurate knowledge of the magnitude and sign of the change in dimensions to be expected in any given case, both from the point of view of direct usefulness in the fabrication of parts by powder metallurgy, and from the longer range viewpoint of elucidating the fundamental mechanism of metallic sintering. The present study was therefore undertaken as a first step in acquiring systematic and reasonably quantitative knowledge of the change in density of metal powder compacts during sintering. For practical reasons, copper was selected as the material to be studied first, and its densification followed as a function of temperature and time of sintering in hydrogen and in vacuum. Experimental Procedure The copper powder used was that designated by the manufacturer (Metals Disintegrating Co., Elizabeth, N. J.) as MD-151. This powder was sifted through Tyler standard screens to separate the fraction having particle size range between 200 mesh and 325 mesh, and this fraction was used in all the subsequent work. Compacts weighing about 10 g were then pressed in a 1 in. diam round die, using a pressure of 20,000 psi throughout. Sintering was carried out in commercially built electric furnaces in which the resistance windings are so disposed as to produce a nearly uniform temperature along the axis of the furnace for a length of about 18 in. centrally located. In order to be able to sinter in a controlled atmosphere, a 2 in. stainless steel tubing was inserted in the furnace. Each end of the tube was cooled by a water jacket about 7 in. long, and closed with a rubber stopper. The hydrogen used for one series of specimens was purified as described in Ref. 1. For the other set, a pressure of about 0.5 mm Hg was maintained during sintering by a Welch Duo-Seal Pump. The specimens were heated on square trays made of stainless steel. In placing specimens in the trays, a thin even layer of powdered aluminum oxide was first sprinkled on the bottom of the tray. A copper guard disk about half the thickness of the specimen was then placed in the tray and covered with a second layer of alumina. The actual specimen was then set on the guard disk, and a final coat of alumina sprinkled over the specimen. This technique was evolved for sintering the specimens in such a way as to reduce the influence of unknown extraneous factors to a minimum. If the specimen is placed directly on the tray and sintered, it is found that the resulting shape is that of a frustum of a cone, rather than a section of a right circular cylinder, since friction with the tray prevents the bottom of the specimen from contracting at the same rate as the top. In the arrangement used in these experiments, the guard disk provided a support which shrank at the same rate as the specimen, and the alumina powder reduced to a minimum friction between guard disk and tray, and between specimen and guard disk. The procedure followed in sintering consisted of bringing the furnace to the required temperature, and then inserting the specimen into the central heated portion of the furnace tube in one of the two atmospheres used. At the end of the heating period, the specimen was cooled by bringing it into a portion of the furnace surrounded by a water jacket. These manipulations were carried out without opening the furnace, by means of rods which were attached to the trays and operated through a sliding seal in the rubber stopper. The progress of densification of the copper compacts was studied at 1300, 1400, 1500, 1600, 1700, and 1800°F. At each of these temperatures, a specimen was allowed to sinter for each of the following time intervals: M, 1, 2, 4, 8, 16, 32, and 64 hr. The thickness and diameter of each specimen were measured with micrometers before and after sintering, and each was weighed on an analytical balance after sintering. Results The techniques described in the preceding section were found to give satisfactory results. The specimens were not detectibly warped after sintering, and were usually of uniform diameter (that is, truly round) to within 0.001 in., a very few showing a variation in diameter of ±0.002 in. All specimens were found to have the same diameter

Jan 1, 1950

By A. L. Field

This general subject has been so thoroughly discussed by Dr. Herty and his associates, especially with regard to the degree of oxidation of the metal at the time that the silicon pig or spiegel is added, that I am not going to spend much time on that today. I should like to propound a question, which is based on my own observations made some years ago while with a large alloy-steel company which had two open-hearth furnace plants. It is true that one of these plants was not engaged particularly in making alloy steels, but there were certain relations between slag and metal composition which appeared to me to be entirely different in the two plants. I have an explanation for it that is more or less incomplete, but possibly Dr. Herty or Mr. Reinartz or some of the others may be able to complete it. Suppose we take our three layers; the metal on the bottom, on top of that the slag, and on top of the slag, the gas. We cannot overlook the gaseous phase. Regardless of the effect of the iron oxide in the slag on the rate of carbon elimination—and that, of course, is rather important in alloy practice since it is not desirable to have the carbon dropping too rapidly at the time the deoxidizing is had in the furnace—it will probably be admitted that it depends on the iron oxide in the metal for a given carbon oxide. I have seen cases where with approximately identical metal and slag compositions one furnace would work twice as rapidly as another in removing carbon. Of course, there is some explanation of this in what others have already said, that the question of the exact lime and silica content of the slag determines the activity and viscosity of the slag; but I am convinced, without having reviewed the actual records since I was asked to make this talk, because they were not available at the time, that the slags in these two furnaces were not materially different. Putting it another way, one furnace would have

Jan 1, 1935

By A. L. Field

This general subject has been so thoroughly discussed by Dr. Herty and his associates, especially with regard to the degree of oxidation of the metal at the time that the silicon pig or spiegel is added, that I am not going to spend much time on that today. I should like to propound a question, which is based on my own observations made some years ago while with a large alloy-steel company which had two open-hearth furnace plants. It is true that one of these plants was not engaged particularly in making alloy steels, but there were certain relations between slag and metal composition which appeared to me to be entirely different in the two plants. I have an explanation for it that is more or less incomplete, but possibly Dr. Herty or Mr. Reinartz or some of the others may be able to complete it. Suppose we take our three layers; the metal on the bottom, on top of that the slag, and on top of the slag, the gas. We cannot overlook the gaseous phase. Regardless of the effect of the iron oxide in the slag on the rate of carbon elimination—and that, of course, is rather important in alloy practice since it is not desirable to have the carbon dropping too rapidly at the time the deoxidizing is had in the furnace—it will probably be admitted that it depends on the iron oxide in the metal for a given carbon oxide. I have seen cases where with approximately identical metal and slag compositions one furnace would work twice as rapidly as another in removing carbon. Of course, there is some explanation of this in what others have already said, that the question of the exact lime and silica content of the slag determines the activity and viscosity of the slag; but I am convinced, without having reviewed the actual records since I was asked to make this talk, because they were not available at the time, that the slags in these two furnaces were not materially different. Putting it another way, one furnace would have

Jan 1, 1935

By William H. Baer, George M. Carlton, Blake M. Loring

IT is a well known fact that age-hardening alloys remain in a supersaturated, or partially supersaturated, condition only for limited periods of time at temperatures below the solvus. In order to develop optimum properties by subjecting the quenched alloy to precipitation or age-hardening treatment at a specified temperature, it is necessary that the cooling rate be sufficiently high to maintain the required degree of supersaturation of the solid solution. In practical applications the size and shape of the specimens obviously have considerable influence on the rate of cooling and there is need for more information on the effects of various rates of cooling. Cooling rates of quenched aluminum alloys generally have been established by the type of quenching medium, the temperature of the medium and the dimensions of the specimen.1,2,3 Except for the work of Roth3 little quantitative information is available on the measurement of cooling rates of aluminum alloys and the significance of the influence of various cooling rates upon the mechanical properties. The purpose of the present investigation was to study the use of the Jominy test for aluminum alloys (Table I). EXPERIMENTAL PROCEDURE The material for this investigation consisted of extruded rods 1 ¼ to 1 ½ in. in diam. The chemical compositions were as follows: [ ] The modified L-type Jominy specimen with dimensions shown in Fig I was selected as the most convenient means for obtaining a wide range of cooling rates. The standard Jominy specimen was not satisfactory because its cooling rate was not sufficiently high. The four flat surfaces machined at right angles along the length of the L-type specimen to a depth of 0-015 in. facilitated the hardness measurements. The specimens were machined from the extruded stock with no intermediate forging. New specimens were used for each aging experiment. The specimens were given solution treatments of 2 hr duration at recommended temperatures in a Hoskins furnace (Table 2). The temperature of the furnace was maintained constant to ±3°C. No protective atmosphere was necessary because the thin film of oxide that formed on the surface of the specimens had no effect on the hardness measurements.

Jan 1, 1948

By J. W. Lacey, F. H. Brinkman, J. E. Faris

This paper presents an analysis of the high-pressure, gas-driven LPG-slug process, based on fluid flow tests in areal models. Two types of tests were made. One series was made in low-pressure models which permitted observation of fluid movement. Three completely misci-ble analog fluids were used. A second series of tests was made in high-pressure models using methane, propane and a light refined oil saturated with methane at room temperature and 1,550 psig. Under the test conditions of room temperature and a pressure level of 1,550 psig, the phase diagram for the fluids used is similar to those for many of the field systems where the process is considered for use. A method for using these laboratory data to calculate field performance of the process is outlined. As a result of this work, it is concluded that small banks of LPG (5 per cent HV or less) are not effective in increasing oil recovery in horizontal reservoirs. Znstead, where small banks are used, the driving gas quickly penetrates the LPG bank because of fingering and channeling; and from this point on, the process behaves essentially as an immiscible gas-injection project. The validity of this conclusion was substantiated by: (1) laboratory studies of the effect of rate, model size and mobility ratio on miscible displacement in areal models; and (2) calculation of field recovery, which compared closely with actual field recovery. INTRODUCTION Field applications and pilot tests of the gas-driven, LPG-bank, oil-recovery process are on the increase. Most of these tests are employing small banks (2% to 5 per cent hydrocarbon volume) of LPG, which is miscible with both the driving gas and the oil in place, in an effort to attain an effective yet economical miscible displacement of oil by gas. The expectation of miscible displacement with small banks is based on the concepts that: (1) lengths of solvent-oil mixed zones, measured during miscible displacements in long slim cores, are representative of those that will occur in the field; and (2) areal sweep efficiencies5 measured in electrolytic model studies are applicable to miscible displacement in reservoirs. Our experimental evidence indicates that the mixed-zone lengths and sweep efficiencies mentioned are not applicable to miscible displacement in reservoirs. In this paper we present an evaluation of the gas-driven, LPG-bank oil-recovery process based on fluid flow experiments in areal models. These results are used to predict the performance of a field pilot test of this process, and the results are compared with the actual test results. THE EFFECTIVENESS OF LPG BANKS The effectiveness of LPG banks of various sizes in accomplishing miscible displacement of oil by gas was determined by displacement tests in a model representing one-quarter of a confined five-spot pattern. The model, 12 X 12 X 1/4 in. in size, was packed uniformly with glass beads. It was operated at a pressure of 1,550 psig and at room temperature; the fluids used were methane, propane and refined oil saturated with methane at 1,550 psig. The saturated oil had a viscosity of 1.2 cp at room temperature. The results of these tests are shown in Fig. 1, where recovery is plotted as a function of the volume of fluid injected for: (1) an immiscible-gas drive with an oil-to-gas viscosity ratio of 85; (2) three sizes of LPG banks; and (3) two completely miscible displacements with mobility ratios of 85:1 and 10:1. (The miscible displacement data plotted are the averages of several tests.) The results show that a 2½ per cent bank of LPG does not increase oil recovery over that obtained by immiscible-gas drive. The 7 and 17 per cent banks are, respectively, about 30 and 50 per cent effective (with reference to the M = 85 miscible-displacement curve) in increasing oil recovery at the point where 2½ hydrocarbon volumes (HV) of fluid have been injected. The percentage effectiveness of the banks at a given volume of fluid injected is defined as Recovery by Bank — Recovery by Gas Drive Recovery by Miscible Recovery by Flooding Gas Drive We conclude from these results that banks of LPG smaller than about 5 per cent HV in an individual stratum will cause from little to no increase in oil recovery. This finding was substantiated by work in low-pressure models, which permitted visual observation of fluid movements. In these tests, three completely miscible fluids having the same viscosity ratios as those used in

By AIME AIME

CADWALLADER EVANS JR. has long been a leading figure in the anthracite mining industry and one of Pennsylvania's prominent citizens. He is, in fact, a native son, having been horn in Pittsburgh on Sept. 17, 1880. At Lehigh, from which he graduated in 1901 with the degree of Mechanical Engineer, Tom Girdler was a classmate, and both were active in football affairs. Going hack to Pittsburgh, he got his first job as trouble shooter for the Oliver Iron & Steel Co. A year later he entered the coal industry, getting a job with the Blaine Coal Co. as inspector of construction and later was superintendent of the Blaine mine at Elizabeth. Pa.

Jan 1, 1943

By O. Hoover, M. Herman, V. V. Damiano

The Jetter and borie' teclznique of determining textures using a spherical specimen has been applied to tlze study of compression-rolled beryllium sheet. Snzall spheres the order of 1 mm in diam cut from the beryllium sheet were autotnatically rotated about tz41o axes using the G.E. single-crystal goniometer. Quantitative pole figures were obtained without tke need to apply absorption corrections. Compression-rolled beryllium exhibited peak intensities ,for (0002) planes of positions tilted 10 deg to the rolling plane and a near random distribution of (1010) planes about the nornal to the rolling plane. TECHNIQUES for determining textures of rolled sheet material are amply described in the literature. The techniques are found to be variations of two basic methods. One due to Decker, Asp, and arker, referred to as the transmission method, utilizes a thin-sheet specimen in which the X-ray beam enters the specimen from one side and the intensity of the beam which emerges from the opposite side is measured. The second method due to chulz,3 referred to as the reflection method, utilizes a thick specimen and the intensity of the beam emerging from the same side is measured. The two rotations of the specimen in the beam are designated a and 8. In order to completely determine the texture of sheet material, it is generally necessary to use a combination of the two methods. The calculations involved in correcting the raw X-ray data for absorption effects and the combining of the data obtained by the two methods are very laborious and time consuming. To avoid the intensity corrections which arise as a result of the changing diffraction volume and path length within the sample other methods have been proposed. The Norton method utilizes a cylindrically shaped specimen cut from the sheet material. Since the rods have rotational symmetry, the absorption correction is constant for rotations about the sheet texture. Jetter and Borie' employed a spherical specimen to analyze the fiber texture of extruded aluminum rods. The spheres were rotated rapidly about the fiber axis to include a large number of grains in the X-ray beam and changes in intensity with respect to tilts of the fiber axis were measured. The absorption correction was constant for all angles and was neglected. The Jetter and Borie' technique finds excellent ap- plication to very fine-grained low-absorbing metals in which the entire sphere volume can contribute to the diffraction volume. In the case of low-absorbing metals, however, serious limitations on specimen thickness occur as demonstrated by Braggs due to de-focussing effects. Peak shifts may occur which negate the assumption that integrated intensities are proportional to peak intensities. These limitations in sphere size to the order of 0.5 to 1 mm for beryllium require that the grain size be sufficiently small to include a large enough statistical sample. The present paper describes the application of spherical specimens less than 1 mm in diam to the quantitative determination of pole figures for compression-rolled beryllium sheet having a grain size the order of 10 p. EXPERIMENTAL 1) Specimen Preparation. Two techniques for spark-machining beryllium spheres were tried. One involved the use of a hollow cylinder as a cutting tool. The tool was fed into the rotating cylindrical specimen as shown in Fig. l(a). The hollow cylinder was carefully aligned such that the axis of the cylinder and the axis of the specimen lay in the same plane and were 90 deg to each other. As the hollow cylinder was fed into the rotating cylindrical specimen, a spherical shape was formed as shown in Fig. 1. Alignment was very critical. Slight misalignment resulted in the formation of a barrel-shaped specimen instead of a sphere. A second technique involved the use of a cutting wheel shaped as shown in Fig. 2 with a groove of the desired radius. A section of the sheet specimen was first turned into a cylinder on the left part of the cutting wheel. It was then shifted to the right and a spherical specimen was turned as shown in Fig. 2. The axis of the cylinder lay in the plane of the sheet. Flats corresponding to the rolling plane of the sheet were used to grip the specimen during the machining operation and these served to identify the rolling plane of the sphere. 2) Rotation of Spec=. The spherical specimen is shown mounted on the G.E. single-crystal goniometer in Fig. 3. The knob A of the goniometer shown in Fig. 3 rotates the specimen about the pedestal axis. These angles have been designated as @ angles. The knob B rotates the specimen about an axis perpendicular to the pedestal axis. These angles have been designated as p angles. A device was made to automatically drive the single-crystal goniometer by means of two flexible shafts connected to the A and B knobs as shown in Fig. 3. The motor system was designed to rotate the knob A, thus rotating the specimen through angles of $I while the B knob remained stationary. After one complete

Jan 1, 1967

By L. C. Brown, S. K. Behera

The diffusion rate in Ag-Sb couples is sensitive to con~pressive load with the width of Ag3Sb, the only phase present in the diffusion zone, increasing with stress up to 800 psi and remaining constant above this. Kirkendall marker experiments show silver to diffuse much faster than antimony in Ag3Sb and incipient porosity may therefore develop at the Ag/Ag3Sb interfnce restricting the transfer of atoms from the silver into the diflusion zone. Application of compressive stress reduces the tendency for porosity to develop and so increases the growth rate. In a recent paper Brown et al.1 observed a significant increase in the thickness of Cu2Te in Cu-Te diffusion couples on application of a compressive stress as low as 20 psi. Similar stress effects have also been observed in the Fe-A1,2 Al-u,3 arid cu-sb4,5 systems. It has been suggested that the increase in growth rates of intermetallic phases in these systems is due to a decrease in the amount of Kirkendall porosity with applied stress. In the present paper, results are presented of the effect of compressive stress on diffusion in Ag-Sb, together with a detailed examination of the Kirkendall effect. The Ag-Sb phase diagram6 shows that antimony has a moderate degree of solid solubility in silver, 5.7 at. pct at 350°C, but that there is essentially no solubility of silver in antimony. There are two intermediate phases— (hcp7) from 8.8 to 15.7 at. pct Sb and Ag3Sb (orthorhombic8) from 21.8 to 25.9 at. pct Sb. EXPERIMENTAL Diffusion couples were prepared from fine silver of 99.95 pct purity and from antimony of 99.7 pct purity. Both the silver and antimony were produced in the form of discs 1/2 in. in diam by approximately $ in. thick, with surfaces ground flat to 3/0 emery paper. Diffusion anneals were carried out in the apparatus previously described.1 A compressive load was applied to the diffusion couple through a lever arm system, with a reproducibility estimated to be ±10 psi. All runs were carried out in a protective hydrogen atmosphere. Following the diffusion anneal specimens were sectioned and polished and the width of the diffusion zone was measured metallographically. Composition profiles were measured using an electrostatically focused electron probe with a spot size of 10 , counting on Sb L radiation. Corrections for matrix absorptiori and fluorescent enhancement9 were not required. S. K. BEHERA, formerly Graducate Student, Department of Metallurgy, University of British Columbia, is now Postdoctoral Fellow, Whiteshell Nuclear Laboratories, Atomic Energy of Canada Ltd., Pinawa, Manitoba. L. C. BROWN, Junior Member AIME, is Associate Professor, Department of Metallurgy, University of British Columbia, Vancouver, B.C., Canada. Manuscript submitted June 14, 1968. IMD RESULTS Fig. 1 shows an electron probe traverse of a typical diffusion zone. In all couples examined only one intermediate phase was observed and the composition of this phase, 23 wt pct Sb, was in good agreement with the composition of Ag3Sb, 23 to 28 wt pct Sb. The presence of this phase was confirmed by X-ray diffraction of filings taken from the diffusion zone. The probe traverses showed no detectable solid solubility in either the silver or the antimony although the phase diagram indicates that some antimony, up to 6.5 wt pct pct Sb, should be in solid solution in the silver. However the width of this portion of the diffusion zone would be expected to be very small in view of the low diffusion coefficient in the silver, 4 x 10-l6 sq cm per sec at 350°C, 10 compared with that in the Ag,Sb, estimated as 3 x 10-8 sq cm per sec in the present work, and this region would therefore not be expected to be seen in the probe traverse. Application of stress resulted in a significant increase in the width of the diffusion zone, Fig. 2. At 350°C, the thickness of Ag3Sb increased from 250 at 0 psi to 400 p at the limiting stress of 800 psi, indicating an apparent 150 pct increase in the diffusion coefficient. Similar behavior was also observed at 400°C, indicating that the stress effect is not characteristic of just one temperature. The growth of Ag3Sb at 350°C and at various stresses is shown in Fig. 3. In every case the growth rate was parabolic indicating diffusion control. The kinetic curves all passed through the origin showing that delayed nucleation of Ag3Sb was not responsible for the stress effect and that it was a real growth effect. A series of tests were carried out in which diffusion was allowed to take place at a lower stress following an initial high stress diffusion anneal. Speci-

Jan 1, 1969

By W. Mitchell, B. H. Bergstorm, C. L. Sollenberger

A unique compression testing machine was constructed to load individual 1/8 to I-in. spheres of glass, etc., at rates from 100 to 100,000 lb per min. During loading the applied load was continuously plotted us the deformation of the sphere-platen system. The load-deformation curve conforms to the theory of elasticity. The spheres were surrounded by steel retaining rings or by gelatin (to prevent secondary fracture). The product size modulus was determined from screen analyses. The data shows: 1) Energy input per unit mass is inversely proportional to the product size modulus (or directly proportional to the surface area per unit mass). 2) Increased loading rates slightly increase the energy input per unit mass required for fracture without affecting the preceding relationship. Theory and experiments show that much of the input strain energy is transformed into kinetic energy of fragments at fracture, this being a reason efficiencies based on "surface energies" are exceedingly small. This large kinetic energy component is usually dissipated as heat but may be partially reclaimed because impact of fragments against the surface of steel retaining rings causes additional comminution. There are currently several theories of crushing, all of which can be derived from the general energy equation of Gillilandl as was pointed out by Mitchellet al in 1954'and more recently by Rose and Sullivan. If the exponent of the equation dE-x-"dx is assigned values of 2,1, or 3/2, one obtains by intergration between suitable limits, the equations of Rittinger, kick,' and Bond,' respectively. Other investigators prefer to let the exponent be a variable parameter. To help resolve the controversy, the Allis-Chal-mers Research Laboratories set up a series of carefully controlled experiments in which the level of energy input required to induce the comminution of a single particle by slow compression loading was very accurately measured. The energy input requirement, in conjunction with the size analysis of the fragments produced at fracture, yielded an accurate energy-product size relationship for the conditions studied. APPARATUS The experimental apparatus was designed to apply a compressive load on opposite sides of an "ideal particle." Spherical shapes were chosen, because point contact loading is typical of the mechanics of conventional crushers. The bulk of the experimental data was obtained with glass spheres because glass is a fairly homogeneous, brittle material for which the properties follow definite statistical distributions. The spheres ranged from 1/8 to 1-in. diam. The compressive load was applied to the specimen at a uniform rate by a loading mechanism (Fig. 1) which acted through a system of levers. The uniform rates, ranging from 100 to 100,000 lb per min, were obtained by metering water into a bucket suspended at the end of the secondary level. Point contact was made with the sphere through tungsten-carbide platens. This latter material is extremely hard and has a high modulus of elasticity, thereby having a minimum of distortion when loaded. The actual load on the sphere was measured independently of the lever system by a load cell, Fig. 2, which was designed so that the voltage output of the load cell would be proportional to load. The deformation of the specimen was indirectly measured by a pair of transformers which were attached to opposite edges of the upper platen. The cores of the transformers, which were attached to the lower platen, moved relative to the transformer so that the voltage output was proportional to the deformation of the sphere-platen system. The load was plotted against the deformation on an X-Y recorder. The area under the curve, as shown on Fig. 3, was proportional to the energy input of the

Jan 1, 1961

By N. K. Chen, R. Maddin

THE textures of straight-rolled and of cross-rolled molybdenum were first determined with the aid of pole figures by Custers and Riemersma.' These authors have shown that for straight-rolling, the main texture was (100) [0111 with a considerable spread about the rolling direction. After cross-rolling a second texture was obtained in which there was a [111] axis perpendicular to the rolling plane, possessing a rotary symmetry. Recently Semchy-shen and Timmons2 in their study of preferred orientation of arc-cast molybdenum sheet obtained similar pole figures. In these two investigations, polycrystalline materials were used. In the main, the textures of molybdenum in these cases are qualitatively consistent with rolling textures of other body-centered cubic metals, such as iron and Fe-Si alloys." In the present investigation, single crystals of molybdenum were deformed by rolling with respect to specific crystallographic planes and directions. Since the deformation textures of polycrystalline aggregates have been related intimately to the behavior of individual grains,4 a study of possible correlations of final textures with respect to the initial orientations of the single crystals might conceivably lead to a better understanding of the textures. Annealing treatments were carried out after deformation in order to study the recrystallization characteristics as well as the recrystallization texture. Rolling of Single Crystals Single crystals of molybdenum (about 1/8 in. in diarn x 1-in. long), grown by the method previously described,5 were cold-rolled without intermediate anneals. Except for specimens MR-1 and MR-2, which were rolled at random in the preliminary test in order to find a proper rate of reduction, all other specimens were carefully documented as to their respective orientation before deformation by means of X-ray Laue back-reflection methods. A stereo-graphic projection was constructed from which it was possible to determine a particular plane and direction to be considered for rolling. Parallel flat surfaces were then polished metallographically with respect to a reference scratch on the specimen which was mounted in sealing wax. These flat surfaces contained the plane chosen for rolling. After etching, a Laue back-reflection photogram was again made of one of the flat surfaces to determine the exact plane of rolling. The initial orientations of all the specimens (specified by two elements for each crystal, direction of rolling and the pole of the rolling plane) are summarized in Fig. 1. The specimens were mounted in plasticene between two hardened Si-Fe plates. The sandwich was then rolled down, keeping the direction constant in the case of straight-rolling. In cross-rolling (MR-10, MR-11, and MR-12) the sandwich was rotated 90" after each pass so that every first and third pass contained the same rolling direction. Specimens MR-14, MR-15, and MR-16 were compression-rolled following the manner of Barrett." In these cases the direction of the sandwich through the rolls was changed by 3" to 5" for each pass until the specimens were rolled to the desired reduction in thickness. It was found that if extreme care was exercised in rolling, i. e., the amount of deformation per pass was extremely small, the specimens could be rolled to a large reduction in thickness. The rate of reduction used, with a single exception of MR-1. was generally 0.001 in. per 10 passes. Thus, it took about 800 passes to reduce a specimen to a final reduction in thickness of 87 to 98 pct. The results of rolling are shown in Table I. Cold-Rolling Textures The final orientations were determined by the conventional Laue transmission method," using molybdenum radiation, with or without a zirconium filter. Pole figures were plotted from (1101 and (200) reflections in which three degrees of intensity— heavy, medium, and light—were determined visually. Three main types of textures have been observed from the deformed single crystals. These are: 1—a

Jan 1, 1954