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By Otto H. Henry, J. J. Cordiano

Though powder metallurgy is one of the oldest of metallurgical processes, it is in its infancy as a branch of the modern field of metallurgy. As early as 3000 B.C., the ancients produced implements and weapons of iron by reducing iron ore in a charcoal fire and forging the resultant sponge while still hot into the desired shape. Melting and casting soon superseded the powder metallurgy practice, and it was not until the turn of the twentieth century that powder metallurgy was applied to the commercial manufacture of tungsten lamp filaments. From this beginning, the use of the powder metallurgy process spread" to the manufacture of porous oil-impregnated bearings, cemented carbide tools, contact points, diamond grinding wheels, clutch facings, starter brushes, resin-bonded radio cores, magnets, metallic filters, and other parts. More recently, and particularly during the present war, there has been a definite trend toward the manufacture of machine parts by this process in competition with the more conventional fabricating methods. Notwithstanding these many developments, scientific progress has been slow. While many articles on powder metallurgy have appeared in the press and various publications, there have been too few contributions to our technical societies, with the result that there is a dearth of the type of information necessary for the full development of this science. It is of primary importance that the results of research and development be freely disseminated if powder metallurgy is to realize its fullest potentialities. Purpose of Investigation Excluding the refractory metal field, all commercial powder metallurgical products made by a cold compressing and sintering operation contain voids. These voids can be substantially eliminated by subsequent severe working and heat-treatment, but ' such practice has not proved economical in most applications. By applying heat during the compressing operation, plastic deformation of the powder particles is substantially increased, and the resultant compact or briquette is practically free of voids. However, hot-pressing has many attendant problems, which at present preclude its use in the manufacture of precision parts. The more important of these are to devise: 1. A die steel capable of withstanding high pressures at elevated temperatures. 2. A high-temperature lubricant capable of preventing excessive die wear and welding of the compact to the die walls. 3. A method of retaining a neutral or reducing atmosphere in the compacting zone of the die assembly. 4. A means of ejecting the hot-pressed specimen into a neutral atmosphere until reasonably cold.

Jan 1, 1946

By J. G. Kura, P. D. Frost, L. W. Eastwood

THE preparation and general properties of mag-nesium-lithium base alloys have been described in earlier papers.l,2 Lithium forms solid solutions with pure magnesium, lowers its density, and improves its formability. The improved isotropy and better formability of these alloys are attributed to the ability of lithium to convert the magnesium lattice from hexagonal (alpha phase) to body-centered-cubic (beta phase) structure. This change in structure is, however, accompanied by some limitations which make it difficult, if not impossible, to combine all the desirable properties in one composition. The most important of these limitations is the tendency of the high-strength alloys to overage and lose strength at temperatures of the order of 150" to 200°F. A study was made of the effects of composition and heat treatment on the age-hardening character- istics of the alloys. Stability of properties was determined by hardness and tensile testing of the alloys at room temperature after various periods of exposure to elevated temperatures. Precipitation-hardening curves are shown for a number of magnesium-lithium-zinc alloys in fig. 1. All the alloys were solution treated at 700°F and aged at 200°F. The reason for using the drastic quench, toluene at —105°F, was to reduce the rapid precipitation of the hardening phase which takes place at room temperature. Previous experience has shown that a hardness of about 90 to 95 Rockwell E is indicative of yield strengths in the range of 35,000 to 40,000 psi. This is a desirable strength level for magnesium-lithium base alloys with specific gravities of the order of 1.65 or less. Although the hardness level is raised by large zinc contents, a corresponding decrease in the cold formability of these alloys occurs with increasing zinc content. Thus, alloys containing up to about 10 pct Zn and having hardnesses of the order of 70 to 75 Rockwell E may be bent over a very small radius; however, the 16 pct Zn alloy requires a bend radius of more than 8T. The hardness relationships illustrated in fig. 1 can be explained by the partial phase diagram shown in fig. 2. The zinc-free magnesium-lithium alloys are entirely body-centered cubic (100 pct beta phase) when the lithium content of the binary is 10.3 pct or higher. When zinc is added, the boundary between the beta and alpha-plus-beta fields at 700°F is shifted to lower lithium contents. In addition, the solubility of zinc at 700°F decreases with decreasing lithium content. It is shown by a study of micro-structures that the limit of solid solubility of zinc in the 6Mg/Li* matrix at 700°F is about 19 pct. It is believed from a study of the aging curves that this limit is about 2 to 3 pct at 200°F. Zinc additions up to about 2 pct increase the hardness and strength of the magnesium-lithium base solid solution. Larger additions of zinc effect further hardness increases, but precipitate during prolonged aging at 200°F. Alloys having 14 to 20 pct Zn precipitation harden extremely rapidly during quenching, even when quenched in toluene at —105° F. The high-zinc alloys overage at 200°F but are capable of maintaining reasonably high hardnesses for periods up to 1000 hr.

Jan 1, 1951

By L. A. Wilson, N. H. Harrison, R. R. Clay, R. L. Reed. D. W. Reed

Experiments have been performed in a linear near-adiabatic system for the purpose of extending data on reverse and forward combustion from atmospheric pressure to 1,000 psig. Results obtained from reverse combustion appear to conform qualitatively with the existing description of the process when reaction kinetics are suitably modified to account for the increase in pressure, i.e., increasing tbe pressure decreases the peak temperature and increases the combustion zone velocity. Forward combustion appears to be a fuel dominated process wherein peak temperature and combustion zone velocity are not very sensitive to changes in pressure. The moderate effects of pressure that do exist at low flux virtually disappear at high flux providing all oxygen is consumed. With this provision. increasing the pressure decreases the frontal velocity and increases the peak temperature. Results me shown graphicaIIy which demonstrate the effects of presswe on peak temperature, rate of advance, oil recovery, air/oil ratio, carbon oxides produced and temperature distributions. INTRODUCTION Numerous field tests of oil recovery using the technique of underground combustion are now in progress. Operating pressures used are always substantially in excess of atmospheric pressure. Nevertheless, the literature contains no laboratory data pertaining to the effects of pressure except for those of Martin, Alexander and Dew.1 Unfortunately, these data appear to reflect heat losses which may have obscured some of the effects of increased pressure. The underground combustion processes are exceedingly complex, and general concepts relating to them have necessarily been described in relatively simple terms. Particularly with regard to forward combustion, the interaction between multiphase fluid flow, heat transport and various rate mechanisms is so involved that to date a rigorous treatment is not available. In this paper a linear near-adiabatic system is described which was found capable of operating at pressures up to 1,000 psig and temperatures of at least 1,100 F. Using this equipment, experiments on both forward and reverse combustion were accomplished at elevated pressures and the data presented as a function of air flux or temperature. It will be assumed that the reader is familiar with the papers of Wilson, Wygal, Reed, Gergins and Henderson on forward combustion and that of Reed, Reed and Tracht3 on reverse combustion, so that it is not necessary to repeat the details of the two processes. EQUIPMENT AND PROCEDURE It was decided to study the effects of pressure over the interval 0-1,000 psig using a near-adiabatic system. Since satisfactory operation of such a system requires very thin tubing walls, it proved necessary to insert the entire combustion tube and heater assembly into a high pressure jacket in such a way that the internal tube pressure could be counterbalanced by pressurizing the annulus. This meant that the numerous heater and thermocouple wires had to pass through gas-tight seals that required considerable effort to maintain effective. An unexpected difficulty arose in connection with the nature of the annulus pressuring gas. It turned out that the composition of this gas critically affected the functioning of the adiabatic control system. Operation of the equipment at elevated pressures was not particularly difficult. The problems that did arise were a direct consequence of the large numbers of connections and seals involved. EQUIPMENT The equipment consisted of the combustion tube which fitted within the pressure jacket. This jacket was in turn mounted on a wheeled carriage which facilitated movement and provided for rotation of the

By Hsun Hu

Direct observations were made on the recrystalli-zntion of a cold-rolled (110) [001] crystal of 3 pct Si-Fe by annealing thin sections of the specimen inside the electron microscope during examination. Subgrain formation, presumably by polygonization, occurs rapidly, followed by a slow increase in the subgrain size before recrystallization can be detected. No migration of the subgrain boundaries was observed, and the formation of recrystallization nuclei by coalescence of subgrains is suggested. Re-c~ystallization characteristics of various texture components were individually examined. AS reported in a previous paper: orientations of the various deformation texture components in a 70 pct cold-rolled (110) [0011 crystal of 3 pct Si-Fe were completely confirmed by transmission electron diffraction patterns taken at various areas of the specimen. These orientations can be summarized as follows: Over most areas of the deformed crystal (111) planes are parallel to the surface. These areas correspond to either $- the two main defor: mation textures, the (111) [112] or the (111) [112].2-5 Within a few areas, (100) planes parallel to the surface are frequently found. These areas represent the minor deformation texture component, the (100) [Oll] type, which is derived from rotated Neumann bands.2'4'5 Only in very rare instances are (110) planes found parallel to the surface. This orientation corresponds to the very weak texture component of the (110) [001] type. In a pole figure, this (110) [0011 orientation is located within the orientation spread between the two main (111) [1121 type textures. Usually the electron diffraction patterns taken at various areas of the specimen are very simple ones, i.e., for any one area the pattern consists only of sharply defined spots of a single orientation. In some areas, however, more or less continuous rings of weaker intensities are superimposed on a simple pattern, indicating the presence of a wide range of additional orientations. In order to understand in detail the recrystallization of this cold-worked crystal, the recrywtallization characteristics of each of the various deformation texture components must be examined. This can best be done by using a high-temperature stage and transmission electron microscopy techniques, whereby small areas corresponding to the various texture components can be selected individually for examination. The present paper presents results obtained by this method. MATERIAL AND METHOD Specimens were prepared from a previously studied1 single crystal of a commercial grade 3 pct Si-Fe alloy with an initial orientation (110) [00l], cold-rolled 70 pct from 0.014 in. to 0.004 in. in thickness. Thin foils were prepared by electrolytic polishing as described in the earlier paper.' Specimens of this thin foil were then mounted in a high temperature stage similar to the one designed by Whelan.6 A direct current was used as the heating source. The temperature of the heating grid was calibrated by means of a Pt vs Pt-10 pct Rh thermocouple in a vacuum chamber (0.01 to 0.02µHg). Maximum variation within the temperature range of 250o to 000°C was about ± 25°C. After the desired areas were selected for examination, the specimen was heated to a low temperature for some time while the selected area was constantly watched. When no further change in structure and orientation could be observed, a higher temperature was applied. Photomicrographs and diffraction patterns were taken from time to time during examination, with the heater temporarily turned off* while the photographs were

Jan 1, 1962

By N. J. Grant, C. Stein

A more complete determination of the chromium-rich portion of the Cr-Ni phase diagram was made, based in part on resistivity measurements. The existence of a eutectoid reaction at 1215°C,made,based in addition to the previously reported eutectic reaction at 1343°C, was confirmed. Metallographic studies, lineal analysis, and diffusion-couple evidence were utilized to support Metallographicand extend the findings of the resistivity measurements. Delineation of the a chromium solvus line shows that the maximum solubility of nickel in a chromium decreases rapidly from 25 wt pct Ni at the eutectoid temperature to 16 wt pct. Ni at 950°C. IN recent years alloys of high chromium and nickel content have become of more interest as better performance of metals at higher temperatures is sought. It has become increasingly important, therefore, that the Cr-Ni binary diagram, which is composed of two of the elements commonly found in many high temperature alloys, be known more accurately. In particular, the chromium-rich portion of this diagram has for a long time remained incompletely determined and has been reported in the literature with a great deal of conflicting evidence. In general, electrolytic chromium of nominal purity was used by most of the earlier workers, who, except for Jenkins et al., made no further attempt to purify the metal. In the present redetermination of the chromium-rich portion of the Cr-Ni phase diagram, every effort was made to use the purest component metals available and to retain this purity throughout the preparation of the alloys and their subsequent handling. Early work by Voss, Bain," and Phebus and Blake4 indicated that the Ni-Cr binary diagram was a simple eutectic system with rather extensive terminal solid solutions. Later, Nishigori and Hamasumi," Tasaki, Weaver and Jellinghaus,' Matsunaga, and Jette, Nordstrom, Queneau, and Foote attempted to determine the limits of the phase fields. Except for Jette and coworkers, the other investigators agreed that the temperature of the eutectic reaction occurred between 1320" and 1340°C and at a composition of 50 or 51 pct Cr. There was, however, considerable disagreement as to the melting point of the chromium-rich alloys and the limits of the solid-solution fields. As a result of the studies of Jenkins et al., the liquidus and solidus curves up to 80 and 90 pct Cr, respectively, were outlined. In addition, the solid-solution phase fields at higher temperatures had been investigated and showed only two phases. The boundary of the chromium-rich a phase was not determined precisely according to these authors, but indications were that it tended to confirm the earlier work of Nishigori and Hamasumi. A more recent investigation by Taylor and Floyd,'" using X-ray methods, essentially corroborated the diagrams proposed by Jenkins et al., and by Wise and Eash (see Fig. 1). Again, no indication of a third phase in the chromium-rich portion of the diagram appeared. The earlier observations, however, are not substantiated by the modifications to the Ni-Cr binary diagram proposed by Bloom and Grant." In the investigation carried out by Bloom and Grant, X-ray methods showed that an eutectoid reaction existed at approximately 1180°C, in addition to the eutectic reaction at 1343°C (see Fig. 1). Their determination of the melting point of pure chromium was 1930°C (later revised to 1903"C)." Experimental Procedure and Results The chromium used for this study was electrolytic chromium, made available by the United States

Jan 1, 1956

By S. C. Riemer, I. Iwasaki, J. N. Orlich

The effects of percent solids, mill loading, and grinding time on product size distribution and ball wear were studied in a laboratory ball mill for a taconite ore. Mild steel balls and HCLA steel balls were used to examine the role that ball hardness play in grinding. Net production of - 44-µm (- 325-mesh) material reached maximum at 70% solids, whereas the ball wear decreased as pulp density increased. HCLA steel balls ground the taconite ore finer than mild steel balls under otherwise identical conditions. Examination of ball surfaces with a scanning electron microscope suggested that corrosive wear was mini- mal under nitrogen flushing conditions, and that grinding with mild steel balls involved nipping rather than attrition, whereas grinding with harder HCLA balls involved both nipping and attrition. Pulp viscosity controlled the thickness of pulp layer on balls, thereby affecting grinding efficiency and ball wear.

Jan 1, 1986

By Nick A. Hasenack, Heinz Kister, Rolf B. Vogel, Kees H. van Toor

A full survey of the laboratory and blast furnace tests carried out on two types of acid pellets is given. From the lab tests it appears that type B has a better low temperature disintegration index and a lower reducibility index than type A. The chemical composition and swelling indexes do not differ for both types. From the blast furnace test periods, carried out with a charge of 45% of pellets and 45% of sinter, it follows that both types of pellets lead to the same pig-iron production, blast furnace permeability, and blast furnace dust production. It also can be concluded that type B pellets cause a significantly higher coke consumption.

Jan 1, 1977

By D. Turnbull, R. E. Cech

Small particles, 10-20 microns diameter, of a 28.6 atom pct nickel, balance iron alloy, have been supercooled 186 C with respect to bulk alloy M, temperature. Particles exhibit a marked mechanical shock sensitivity while being held in a supercooled state. The tendency for shock to induce martensitic transformation appears to be a maximum at —140 to —160°. Slow cooling of particles in mechanical contact with one another results in extensive martensite formation. This is prob-ably the same effect as the catalytic effect observed in polycrystals where martensite formation in one grain induces transformation in other grains. AS a result of extensive research over the past decade on the martensitic transformation, a much better though not complete understanding of the transformation has resulted. Recent reviews by Bilby and Christian' and Kaufman and Cohen2 have

Jan 1, 1959

By J. H. Wilhelm, Y. Naide

Continuous thickeners can be sized from previous experience, continuous pilot-scale test results, or batch settling tests. It is relatively simple to size full-scale thickeners when previous experience or pilot-scale operating data are available. But batch testing is often the only realistic method for sizing thickeners due to time restrictions, budget limitations, and availability of sample material. Many authors have, therefore, suggested means of running batch tests and analyzing the resulting data. Fundamental thickening theory began with the work of Coe and Clevenger (1916). In order to determine the size of the thickener settling area, they proposed that a series of batch settling tests be run at various initial concentrations. The solids handling capacity at each concentration can then be determined and the lowest capacity (maximum area requirements) used to size the thickener. Kynch (1952) developed a mathematical analysis in which the relationship between solids concentration and settling rate can be obtained from a single batch settling curve. Talmage and Fitch (1955), Yoshioka

Jan 1, 1982

By Hadyn W. J. Wren

The practical experience obtained from designing and commissioning of fully controlled coal preparation plants, using centralised mini computers is discussed. The importance of defining a workable operating philosophy is highlighted with particular reference to the problems associated with trying to achieve a total 'hands off' concept. These experiences with a centralised computer controlled system have led to a deeper understanding of the interaction between the operation and the control system and the role of local control and management information within the overall control philosophy of a highly automated process plant. The utilisation of an extensive fully distributed microprocessor control system with over 6500 digital and analogue signals split into six autonomous areas with a supervisory system to provide operator interface is described. The important aspects of project definition and design needs are outlined with particular regard for achieving maximum efficiency with minimum complexity. Views of future trends are offered, based on the experience of both centralised computer and distributed processor systems.

Jan 1, 1984

By G. M. Ritcey, M. J. Slater, B. H. Lucas

The recovery of uranium from acid leach slurries by continuous ion exchange, or solvent extraction using sieve-plate pulse columns, is compared. Differences in processing costs are of prime concern and can be related to differences in the unit operations of the two methods, as well as the chemical and physical properties of the slurry. Parameters are defined for the operation of the solvent-in-pulp process and the design of the continuous ion exchange column. Pilot plant operating experience with both recovery systems is described, and an overall assessment of the relative costs is presented.

Jan 1, 1973

By J. M. Karpinski, R. O. Tervo

A method and equipment have been developed for measuring the impact strength of grains of brittle materials. It is shown that brittle materials develop a characteristic particle size distribution when fractured by impact. A simple mathematical model has been found to describe this distribution, and one of the parameters of the model has been designated the r value. The r value is directly proportional to impact energy and, for fixed impact energy, it becomes a useful criterion of grain strength. Data are presented on the variation of the r value as a function of sample history, initial size, energy input and number of impacts. The results are interpreted in terms of the flaw theory of brittle fracture. The view is now widely held that brittle materials comprise a strong matrix, throughout which flaws or points of weakness are scattered at random. Failure always starts at one or more of these imperfections, and planes of fracture are established by the geometry of the flaw distribution. This view has been developed extensively by Weibull 1,2 and experiments of a confirmatory nature have been reported.3,4 Thus the process of fracture or size reduction of brittle materials can be regarded as a process of elimination or creation of flaws, and the concept of strength is intimately connected with the size and history of the specimen tested. One consequence of the point of view described above is that brittle materials will fracture to yield similar size distributions, although the impact energy to produce a given amount of fracture may vary greatly from one material to another. Generally speaking, experimental investigations of brittle fracture in solids have been confined to two extreme experimental situations. On one hand, we have tests on single specimens of well-defined, but artificial, geometry and, on the other, empirical data have been obtained on the feed-product relation in a variety of mills. The first situation necessitates specimen preparation, which in the case of brittle materials is equivalent to a priori size reduction, while the second one suffers from the disadvantage that little knowledge is gained about individual fracture events. Also, the statistical significance of single specimen tests may be questioned. Our approach lies somewhere between these two extremes. We test a large population of sized specimens and yet subject each specimen to a single fracture event. In 1956 G.H. Fetterley of Norton Co., Chippawa, Ont., made the empirical observation that product size distributions obtained from impacting sized grits can be described by the following equation where R is the proportion by weight of the grain that remains on a screen having an opening x on a side, x, is a parameter having the dimensions of length, and r is a number. This equation has since been derived on a theoretical basis by Gaudin and Meloy.5 They identify x, with the initial size of the test piece and r with the number of flaws per unit length. As will be shown below, our experiments indicate that both x, and r are functions of energy and hence they should more properly be called the effective initial size and the effective number of flaws respectively. Also, our empirical data give us no basis for assuming that r represents the effective number of flaws per unit length, rather than per unit volume. METHOD AND MATERIALS The impact test machine has been designed to feed specimens, essentially one at a time, into an evacuated chamber, where they fall freely and are struck with random orientation by one or the other of a pair of flat steel vanes. The vanes are mounted at opposite ends of a steel bar, which rotates at a closely controlled angular velocity about a vertical axis. Fig. 1 shows the flat circular vacuum chamber with the cover removed, and the horizontal steel bar with the steel vanes at the ends. The cylindrical pot in which the grains are collected after impact appears at the left. Fig. 2 shows the equipment assembled for a test. The vacuum chamber occupies the central position with the variable speed drive below the table surface, the vacuum pump at the extreme left

Jan 1, 1964

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 T. H. Alden

A correlation has been found in rock-salt structure single crystals between the latent hardening, measured by the direct stress activation of oblique slip systems, and the stress-strain behavior in simple compression. Materials with high latent hardening, like LiF, strain-harden at a low rate (Stage I) even when severely constrained. KCl, in contrast, shows low latent hardening and a tendency to strain-harden at a high rate (Stage 11). This correlation suggests that oblique slip is essential for Stage II hardening of these materials. THE role of secondary slip in the strain hardening of metal single crystals is a topic of lively controversy. On the one hand are theories in which secondary dislocations participate directly in Stage II hardening in the fcc metals, for example through the production of sessile dislocations,1 forest intersections, or jog formation. Much of the experimental evidence on which these theories are based has been reviewed by Clarebrough and Hargreaves.~ On the other hand, a recent theory5 denies that secondary slip has an essential role in Stage II hardening or in the transition from Stage I to Stage 11. In the latter view, Stage I is not terminated by an increase in the activity of secondary systems but by the exhaustion of undeformed material.6 The experiments reported in this paper will not resolve this controversy since the materials being studied are cubic ionic crystals rather than metals. However, the results do show in an unusual way a direct connection between "secondary" (nonortho-gonal or oblique) slip and strain hardening in these materials. Specifically, a correlation has been found between two independently measured properties, first the latent hardening of oblique (110)(1i0) slip systems as measured by direct stress activation of these systems, and second the stress-strain behavior at small strains. From prior work, it was known that in most cubi-cally oriented rock-salt structure crystals, two orthogonal slip systems operate and exclude the other equally stressed pair, oblique to the first pair.7'8 This observation apparently indicates that a significant interference exists between slip on oblique (110) planes and a relatively small interference between orthogonal (110) planes. The present experiments were begun with the intent of obtaining a quantitative measure of this difference by means of a study of latent hardening in these crystals. I) EXPERIMENTAL METHODS The experiments were basically of two types, first the determination of stress-strain curves by compression along a single (100) axis, and second the measurement of latent hardening by compressive prestrain along one cube axis followed by the determination of the yield stress in a second (latent) cube direction. All tests were done at room temperature in an Instron machine by compression between lapped, parallel steel faces. Three specimen shapes were used. For long crystals (nominal dimensions, 1/8 in. square by 1/2 in. long) the ends were lubricated with an oil-graphite mixture. Superior results with short crystals (about 1/8 in. cube) were obtained using 0.003-in. teflon film.' Thin crystals (1/4 in. square by 3/32 in.) were used for latent-hardening measurements and similar results were obtained with either lubricant. Test specimens were cleaved from Harshaw single crystals which had been irradiated to a dose of lo8 roentgen using a cobalt-60 source. The irradiation raises the yield stress and tends to prevent plastic deformation during sample preparation.10 Prior to testing, the irradiation hardening was removed by an anneal at 400°C. Ideal compression specimens have flat, parallel faces. In short specimens particularly, satisfactory results demand a close approximation to this ideal. In the present work, cleaved surfaces were often used directly as compression faces. The degree of success using this method depends on two factors: 1) the smoothness of cleavage faces, and 2) the extent to which the crystal is deformed or crushed by the chisel during the cutting of a long crystal into short pieces. Unfortunately, only one material of those studied, LiF, was completely satisfactory. NaF, NaC1, KC1, and KBr behaved less well so that

Jan 1, 1964

By Carl Swartz

IN the course of a recent investigation1 to develop a more satisfactory white-metal. bearing alloy, a number of alloy systems were studied. The cadmium-nickel system showed characteristics desirable in a bearing alloy, and the system was therefore studied in some detail. EXPERIMENTAL METHOD Alloying cadmium with nickel offered no serious difficulty. After melting the cadmium, clean sheet nickel was added while the temperature was maintained at 500° to 600° C: A few crystals of ammonium chloride2 served to clean the nickel when the latter did not "wet" readily. In preparing the individual alloys for thermal and microscopic investigation, a "hardener" containing about 10 per cent nickel was used.

Jan 1, 1933

Sec. 1. The membership of the Institute shall comprise six classes, namely: 1. Members; 2. Honorary Members; 3. Senior Members; 4. Associates; 5. Junior Members; 6. Rocky Mountain Members. All shall be equally entitled to the privileges of membership, excepting that no member of any class whom residence shall be outside of the United States of America, except those residing in Mexico and Canada, shall be entitled to vote. SEC. 2. Members: A person to be eligible for election or transfer into the claw of Member must be at least 27 years of age and must have had at least six years' employment in the practice of engineering, mining, geology, metallurgy, or chemistry, during at least three years of which he must have held positions of responsibility in one or more of these fields. This shall not apply to Rocky Mountain members.

Jan 1, 1934

By H. Reginald Hardy, Y. S. Kim

Recent studies of inelastic behavior and acoustic emission in geologic materials further validate the concept that such materials may be considered to consist of an elastic media containing an array of pores and cracks. In the present paper this concept is investigated further by experiments in which the mechanical behavior of a number of geologic materials were studied in detail at low stress levels using ultrasonic pulse methods. Experiments were carried out on cylindrical test specimens of Indiana Limestone, Tennessee Sand- stone and Barre Granite under relatively low confining pressures (0-5000 psi). Analysis of data from these experiments indicated that there existed a low-level critical stress at which there appeared to be a transition in the mechanical behavior of the material. Under triaxial stress, results indicated that the differential critical stress was relatively independent of confining pressure, i.e., the mechanism responsible for the transition in mechanical behavior was governed by a maximum shear stress criteria.

Jan 1, 1971

By D. A. Rice, M. C. Fuerstenau

Flotation data indicate that sulfonate and amine adsorb physically on manganese oxide; oleate also adsorbs physically if the zero point of charge is sufficiently high. Chemisorption of oleate occurs on pyrolusite between pH 8 and 9, and possible mechan- isms of collector adsorption involving metal ion hydrolysis are discussed. The flotation characteristics of most metal oxides1-15 have been examined with standard collectors such as fatty acids and sulfonates. From these studies it would appear as though electrical phenomena are important when shorte r-chained collectors are involved. For example, Iwasaki, Cooke, and Choi9 have shown that dodecyl amine and dodecyl sulfate float iron oxide above and below the zero point of charge, respectively. In another system, D.W. Fuerstenau and Modi10 have shown that dodecyl sulfate, dodecyl

Jan 1, 1969

By Nicholas J. Grant, Rolf Nordheim, Bill C. Gissen

The system Cb-Re was examined in detail utilizing pure metals, careful melting techniques, and heat treatments. Metallographic and X-my methods were utilized for phase identification. In addition to soli-dus determinations, the composition limits and mode of formation of the intermetallic compounds 0 and X were determined. The binary constitution diagram Cb-Re has been the subject of a number of investigations.'-7 Two intermetallic phases have been described and tentative diagrams have been proposed. It was the aim of this investigation to obtain a complete and more accurate diagram through the use of purer alloys and improved techniques. The diagram worked out by Knapton7 was published after our experiments were concluded. EXPERIMENTAL METHODS The starting materials were Re powder of 99.95 pct purity, supplied by the Chase Brass and Copper Co., and Cb rondelles of 99.6 pct purity, supplied by the Electro Metallurgical Co. Typical analyses are given in Table I. The alloys were prepared from compacted Re powder and Cb rondelles; for critical compositions master alloys were used. The melts varied from 5 to 50 g and were melted nonconsumably in an Heraeus arc furnace, under ti-tanium-gettered laboratory grade argon. It was necessary to invert the buttons and remelt, followed by crushing and further remeltings, the number of which depended on the nature of the fracture of the alloy. The weight of each alloy was carefully checked after each melting operation. It was found that significant weight losses occurred only when loose Re powder was used. These losses amounted to a maximum of 3 wt pct in such instances, but did not occur after the charge was once molten, regardless of the composition. Typical loss of weight after 4 remelts, including crushing, amounted to 0.2 wt pct. Oxygen pickup during successive melting cycles did not appear to be significant, since the weight gain values never exceeded 0.01 wt pct. Control of the composition of the alloys was not too difficult; however, the problem of homogenization was a far greater one. Optimum alloying conditions were finally achieved by a combination of master alloy production and repeated crushing and remelting cycles. The compositions of the alloys utilized to determine the constitution diagram are listed in Table 11. The weight balance method was used ultimately as the sole analytical method, since repeated checks indicated that it was accurate to 0.2 pct, if the weight losses were small. The results were double-checked by a metallographic study of the homogeneity of the samples, since this was presumed to be the more serious factor. Heat treatments at 1200°C or lower were accomplished by sealing the specimens in Vycor tubes, heating in a Globar furnace, followed by air cooling. This was considered to be an adequate quench because of the very low temperatures involved. For temperatures of 1200" to 1900°, alloys were homogenized and heat treated in a tungsten-filament resistance vacuum furnace. From 1900" to 2750" a tantalum-tube resistance furnace was utilized, operating under a vacuum of 105 mm Hg. The temperature measurements up to 1200" were made by means of platinum-platinum 10 pct Rh thermocouples, with an accuracy of 5°C. For temperature measurements greater than 1200°C, optical pyrometers were used. They were calibrated against a standardized instru-

Jan 1, 1962

MISCELLANEOUS U.S. 0,029,598 - Extraction of vanadium values from vanadiferous iron oxide ore. A pelletized mixture of ore, limestone and bentonite is roasted in an oxidizing atmosphere to form calcium vanadates, the calcine ground, the ground material leached with aqueous ammonium carbonate or sodium carbonate to produce a vanadium-rich solution while leaving an insoluble residue of calcium carbonate and/or calcium bicarbonate along with undissolved iron values, and the solution separated and treated for its vanadium content. This patent is a reissue of U.S. Patent No. 3,853,982, dated Dec. 10, 1974. C. B. Bare and J. W. Pasquali, assigned to Bethlehem Steel Corp. Mar. 28, 1978. 7 pp. (423-68). Filed: 3-3 1-77 (783,352).

Jan 1, 1979