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By Michael G. Schill, Mark C. Fischer

Since its introduction several years ago in the United States, the high pressure belt filter press has proven to be a highly cost-effective dewatering device in a number of mining and industrial applications. To evaluate the process and economic factors associated with the dewatering of coal refuse, a comprehensive program of laboratory and on-site pilot studies has been conducted. This paper will summarize findings of this study and discuss advantages of the belt filter press over conventional dewatering methods. The conventional means of dewatering thickened coal refuse involves the use of vacuum disc filters or centrifuges. Due to the high amount of energy used to dewater refuse with these devices it was a logical course of action to apply belt filter press technology to this application, since a belt filter press will require less than 3.7 kW (connected).

Jan 1, 1982

By H. R. Banks

THE Sullivan concentrator has completed 20 years of operation. During this period a considerable amount of data has been accumulated concerning the characteristics of several types of flotation machines in their application to the problem of the differential separation of the lead sulphide, zinc sulphide and, in more recent times, iron sulphide, in the ore from the Sullivan mine. It is the author's intention to sketch briefly experiences encountered when the several types of flotation machines were introduced into the flow. ORIGINAL FLOTATION EQUIPMENT AND ORE The original flotation equipment consisted of four 18-cell lead-roughing machines, whose concentrate was cleaned in an 8-cell and recleaned in a similar 8-cell machine. Zinc concentration was carried out in four 18-cell machines. One 8-cell zinc re-treatment machine received the reground zinc middling. The 168 cells handled some 3000 tons of original daily feed. These cells were of the standard Minerals Separation type, equipped with 24-in. impellers. Spindles were driven through geared line shaft at a speed of 255 r.p.m. The impellers were the 45° type, except for the last three cells of the zinc-rougher machines, which were of sub-aeration type, with full bottom shroud and half shroud for the top side of the impellers. Four-pound air was introduced. This recognition of the benefit of intensified flotation operation for "gleaning" was an important phase in the early operation and will be discussed further on in this paper. Sullivan ore during this period is described as a finely disseminated mixture of four sulphides, totaling 90 per cent made up of 13.6 per cent galena, 14.4 per cent marmatite, 1 per cent pyrite and 61 per cent pyrrhotite. The specific gravity of the ore was approximately 4.4. There has been a gradual change in the ore content. The 10 per cent of nonsulphide constituents has increased to between 15 and 20 per cent and all three sulphides have dropped somewhat. Added equipment and changing technique have made possible the treatment of 8000 tons per day of mill feed instead of the 3000 originally handled. SPECIAL FEATURES OF FLOTATION AT SULLIVAN Sullivan flotation differs greatly from customary practice. The very heavy return of lead rougher middling and lead cleaner tailing, totaling at times 125 per cent of the new feed tonnage, has been the subject of much investigation. The practice is still employed.

Jan 1, 1944

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

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

Jan 1, 1942

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

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

Jan 1, 1942

By Gerald Edmunds, M. L. Fuller

The development of "fiber" or preferred orientations, during the plastic deformation of metals, and the relation of such structures to the anisotropic characteristics of worked metals has become a subject of common knowledge among metallurgists. Very little has been published, however, relative to variations existent throughout the cross-sections of rolled strips,1 and the influence that such variations may have. This paper presents such a study on a rolled zinc alloy.2 The significance of small differences in surface structure is shown in relation to bending properties. Experience with zinc and its alloys has shown that the outer radius of the bend, which is subject to tensile deformation, is the common region of failure. In considering relations of structural characteristics to bending properties it will suffice, therefore, to consider the ease and possible extent of tensile deformation resulting from various orientations. It is necessary in this connection to assume that on the average the individual crystals of a polycrystalline material act substantially as if their movements were unobstructed by the surrounding grains. This assumption is not strictly valid, but the error involved is unlikely to affect seriously the qualitative conclusions derived from its use. The mechanism of the plastic deformation of zinc crystals has been described by Mark, Polanyi and Schmid3 and by Mathewson and Phillips14 and is regarded as being accomplished by block movements or * Investigator, Rolling Mill Section, Research Division, New Jersey Zinc Co. f Investigator, X-ray Laboratory, Research Division, New .Jersey Zinc Co. 1 Variations of structure throughout the cross-section of wire have been reported in the literature. 2 This alloy contained, in addition to zinc, 1.0 per cent copper and 0.01 per cent magnesium. Its crystal form is hexagonal close packed, the sarne as that of pure zinc. 3 H. Mark, M. Polanyi and E. Schmid: Vorgange bei der Dehrlung von Zink-kristallen. Zlsch. f. Phys. (1922) 12, 58. 4 C, H. Mathewson and A. J. Phillips: Plastic Deformation of Coarse-grained Zinc. Proc. Inst. Met. Div., A. I. M. E. (1927) 143. C. H. Mathewson: Twinning in Metals. Proc. Inst. Met. Div., A. I. M. E. (1928) 7. The results of a further study of plastic deformation of zinc as related to twin-

Jan 1, 1932

By J. G. Benford, E. B. Stanley

THERE have been numerous papers in the literature1 on the subjects of secondary and tertiary recrystalli-zation in silicon steels. Secondary re crystallization is believed to occur in silicon steel by either a surface-energy phenomenon such as in the usual development of cube texture or by a second-phase phenomenon such as in the usual production of cube-on-edge texture, (110)[001]. Tertiary recrystallization in silicon steel is thought to be a surface-energy phenomenon in which, for example, grains having a (110) plane parallel to the sheet grow at the expense of other grains in the matrix including those having a (100) plane parallel to the plane of the sheet. In all these instances, the orientations involve either a preferred (100) or (110) plane in the plane of the sheet. Until very recently, there had been no experimental evidence reported of the occurrence of a texture by secondary or tertiary recrystallization that involves a (111) plane in the plane of the sheet, although Kohler reported that grains having the (111) plane parallel to the sheet surface can also grow by a surface energy mechanism. Stickels observed a secondary texture in iron described as "near {554}(225)" about 5 deg from {lll}(211).3 Mee reported that in a vacuum-remelted commercial 3 pct Si steel {lll}(hkl) secondary recrystallization took place in a high vacuum and in pure hydrogen.4 Recently in our Laboratory, large-grained structures such as shown in Fig. 1 having an orientation near (111)[211] or (111)[2ii] have been observed. The arrows point to areas of relatively small matrix grains of the kind that the much larger (111) grains consumed while growing. It is of interest that the matrix grains of samples annealed at 2000°F were essentially the same size as those in samples annealed at 2200°F, a matrix-grain-size stability that is characteristic of secondary recrystallization processes. A torque disc taken from Grain 4 of the sample shown in Fig. 1 revealed a very flat magnetic-torque curve, as expected, with a maximum torque of 7000 dyne-cm per cu cm compared to the typical 180,000 dyne-cm per cu cm observed for conventional (110)[001] textured material. A back-reflection Laue pattern for Grain 4 is shown in Fig. 2 and indicates a near-perfect (111)[211] orientation. The other six numbered grains in the sample of Fig. 1 had a similar orientation. The small circles next to each number were the target areas for the X-ray beam. The starting material was an 0.011-in.-thick oriented silicon steel, (110)[001] texture, containing 3 pct Si. It was lightly pickled, cold-rolled to 0.005 in., and annealed 4 hr at 2200°F within a nickel box (not gas-tight) inside a tube furnace through which dry hydrogen was flowing. The samples were heated to 1500°F in 1 hr and then at 60°F per hr to 2200°F. There were other

Jan 1, 1969

By Frank C. Roe

Two cogent and ubiquitous facts have supported a constant search by the ore processing industry for better wear resistant materials in equipment. First, designs and types of equipment change or improve continually to meet the economic and physical demands of different and/or leaner ores. Second, practically all equipment is subject to impact and abrasion conditions that probably are more severe and extensive than in any other industry. Development and testing by operators and equipment manufacturers alike, has produced an extensive variety of longer lasting metal alloys, rubber, plastics, ceramics and other materials to improve equipment performance under different specific conditions. The need for diversified materials becomes obvious upon the simple realization that no two beneficiation operations are identical. Among the variables in the handling of ore are: 1. Size and weight of ore particles. 2. Hardness and sharpness of ore particles. 3. Concentration of ore particles in liquid or gas suspension. 4. Velocity and direction of particle impact toward equipment surface. 5. Coefficient of friction between ore particles and equipment surface. 6. Temperature of operation. 7. Chemical environment of operation.

Jan 12, 1967

By P. W. Neurath, R. E. Waite

INFORMATION is available on the effect of stress on permeability, coercive force, and hysteresis for a variety of materials' but for the technically important grain-oriented 3 pct Si-Fe' the stress effects are not adequately covered in the literature; in addition, most of the stress data do not permit estimation of what would happen to the 60 cycle watt losses of the material under stress. Direct measurement of these effects therefore has been made and appears to be of considerable theoretical as well as practical interest. Losses were measured on the central 25 cm portion of 40~3~0.035 cm samples which could be stressed in a small tensile machine built for this purpose. Under tension the following effects, illustrated in the figures by a particular example, were observed: 1—"Unstrained" material of commercially acceptable loss level shows no change or a small increase in loss at low elastic stresses. For the sample shown in the figures, this is illustrated during the initial run, where a 7 pct increase is observed (Fig. 1). 2—There is no additional change in loss when the sample is further strained up to the elastic limit (Fig. 1). Within that limit the loss-stress curve is reversible. This is not illustrated in Fig. 1. 3—Even in the plastic range only small increases in loss are observed as long as the sample is kept under stress (Fig. 2, point N); often no increase can be observed (Fig. 1). 4—A large increase in watt losses is observed after removal of the stress subsequent to plastic deformation (Figs. 1 and 2). 5—All, or nearly all, of the foregoing increase in loss due to plastic deformation can be eliminated by a reapplication of tensile stress but returns upon removal of this stress. This is illustrated in the third run (Fig. 3). This run remains within the elastic limit and shows the reversibility of the stress-loss curve under this condition. These findings have been confirmed on large Samples (approximately 200~10~0.035 cm and larger) except that under 1 no initial increase in loss was ever observed on these. The accuracy of the watt loss measurements is of the order of 1 pct. Neither bending of the sample in the tensioning device nor a redistribution of flux along the width of the sample accounts for these results. They therefore must be explained on the basis of either a change in the domain configuration due to stress or a change in the domain wall mobility. Acknowledgment The assistance of Mr. Robert L. TenBroeck with the instrumentation is gratefully acknowledged.

Jan 1, 1956

By Jose A. Ruiz

INTRODUCTION For heterogeneous non-catalytic solid-gas reactions carried out in fluidized bed reactors, nominal bed temperature is an average value between gas and solid. For highly exothermic reactions, actual particle temperature can be up to hundred degrees above termocouple temperature, since heat dissipate at slower rate than heat generation during some steps of transformation. These micro instabilities at particle level can displace thermodynamic equilibrium from the desired phase to others. This effect is important when relatively narrow range of phase stability exists, like in sulphation roasting of sulphides, where bed discharge contains, in addition to the desired sulphate others metastable phases such as basic sulphate and ferrite. For example, for copper-iron sulphide concentration roasted below 680°C, no cupric ferrite is formed, as shown by Jakob et al., therefore the separate Kellogg's stability phase diagrams Cu-S-O represent the roasting (Fig.l). At temperature above this one, like 760°C for example, phase stability changes from CuSO4 to the basic sulphate Cu0•CuSO4. Solid state reaction between Cu0•CuSO4 and Fe203 also occurs to form cupric ferrite, Cu0•Fe2O3, therefore the Cu-Fe-S-O Kellogg's phase diagram of Fig. 1 (continuous line) represents this condition of roasting. Although both Cu0•CuSO4 and Cu0•Fe2O3 are metastable phases under normal operating conditions of sulphation roasting(1-10% SO2, 1-10% 02 and 680°C, points A and B,Fig. 1) sulphation of these species and particularly ferrite are slow and limited due to diffusional control. This explain why reactors discharge contains several phases: CuSO4, Cu0•CuSO4, CuO•Fe203 plus small amounts of CuS and FeS due to the baclonixed conditions of fluidized bed reactors. The presence of cuprous ferrite due to reducing conditions inside individual particles also occurs, but in very limited extent at the reaction interface, as it is demonstrated by the low soluble iron levels of calcines. On the other hand, the presence of cupric ferrites can be explained only due to the higher temperature achieved by particles, since below 680°C cupric ferrite formation does not take place. [ ] This phenomena also occurs for others non-ferrous metal sulphides concentrates roasted under sulphation conditions, such as 7n, Co and Ni. Therefore the prediction of discharge composition of fluidized beds is not possible based only on kinetics and mechanistics models alone or purely thermodynamical considerations, since all factors should be integrated to describe the overall phenomena. SINGLE PARTICLE TRANSFORMATION Assuming a first order reaction with respect to the gas and zero for solid, such as

Jan 1, 1984

By E. S. Bumps

A series of macrographs are presented for the purpose of graphically recording the strain phenomenon that accompanies the energy transition in the Charpy impact testing of a mild steel that is susceptible to strain aging. STRAIN patterns in mild steel Charpy impact specimens were obtained in order to determine whether, on the first appearance of plastic strain during deformation, the initial fracture cracks appear in the region of plastic strain or in the elasti-cally deformed regions between. Although this attempt to locate the initiation of cleavage was not successful, the observed strain patterns illustrating various stress conditions in partially deformed Charpy specimens are presented along with a discussion of the possible dependence of transition energy on the yield phenomenon. Earlier work on the development of strain patterns in mild steel have been reported by Fry1 and later by Jevon.2 Harris, Rinebolt, and Raring3 observed characteristic strain markings on the surface of Charpy V-notch impact specimens fractured above and below the transition temperature which they presented schematically. It is intended that the strain figures presented here will add to the literature a graphic correlation of strain with transition energy in impact specimens. Samples of % in. round hot rolled, 0.20 pct C steel were machined to standard 0.394 in. sq, V-notch Charpy impact specimens. Preliminary testing involved determination of transition temperature, Fig. 1, using a Sontagg impact tester. These data were subsequently used to select temperatures above, within, and below the transition range at which specimens were partially deformed. Partial deformation was obtained by either varying the energy or the testing temperature, see Table I. Macroscopic strain figures shown in Figs. 2 to 19 were produced by several metallographic repolish-ing and etching steps. The macroetchant used was as follows:4 120 g HCl, concentrated; 100 ml water; and 90 g cupric chloride. Strain figures were obtained on the outer surface and on sections through the central portion of the impact specimens in order to determine an approximation of the volumetric strain pattern. In the tensile strain figures reported by Jevon, it was found that strain etching would not work immediately following strain unless the material was heated to 200°C. The impact strain patterns presented here were obtained without this heating, but the specimens were not etched until ten months after straining. This confirms a discussion of Jevon's paper, in which it was pointed out that strain figures can also be developed after aging for long periods of time at room temperature. Hardness of the strained and unstrained portions, revealed by the etched pattern, was explored using R, impressions converted to R, hardness values. Discussion of Results In the impact test, as in the tensile test, some parts of the specimen yield and deform plastically, while other regions are deformed only elastically. The plastic deformation bears a relation to the imposed stress pattern. In the strain figures presented here, the plastically deformed regions are the dark etching ones. The strain figures are always symmetrical because the stress state in the Charpy-type specimen under impact loading is symmetrical. The difficulties encountered to produce initial cracks are intimated in Figs. 2 and 4. At a temperature of —75ºF, the stress was not sufficient to pro-

Jan 1, 1953

By R. M. N. Pelloux

This study of aluminum-copper alloys had two aims: 1) To determine the effect of the amount and distribution of a second phase, CuAl2, on the creep-rupture strength, ductility, and fracture characteristics of the alloys. The work of Gemmell and grant' on single-phase aluminum-copper alloys provided a basis for the present study. 2) To attempt to provide a relation between the microstructure and strength of two-phase alloys deformed at comparatively high temperatures (greater than 0.45 T,). The creep behavior of the two-phase magnesium alloys Mg;Ce and Mg-A1, has been treated by Roberts. 9 In work reported by Sully and Hardy4 and by Underwood, Marsh, and Manning~ on A1-Cu two-phase alloys, and also in a portion of the work of Gemmell and grant,' aging took place during the creep tests. 'In the present work, overaged aluminum-copper alloys were subjected to creep deformation at two temperatures, 500 and 700OF. The overaging treatments to produce the precipitate dispersions were performed prior to the test, at temperatures which were the same as the ultimate respective test temperatures. Hence, the present study is concerned with the creep behavior of stable (in contrast to "underaged") two-phase A1-Cu alloys, i.e., alloys in which no depletion of the solid-solution matrix occurred during: creep. MATERIALS AND PROCEDURE A 2 and a 3 pct Cu alloy, supplied by Alcoa, were studied; Table I shows the compositions. The grain size of the specimens, 0.9 to 1.0 mm, was achieved by annealing the machined test bars for 2 hr at 1000°F, followed by furnace-cooling to 900°F, and homogenizing for 4 hr. Both compositions are in the single-phase condition at 900°F. Two types of overaged dispersions, termed "over-aged I" and "overaged 11" were prepared after the grain size and the homogenization anneals. The overaged I alloys were prepared by quenching to room temperature after homogenization, aging at either 500' or 700°F for 72 hr, and air-cooling to room temperature. The overaged I1 alloys were prepared by furnace-cooling after homogenization, to either 500' or 700°F, and holding at the necessary temperature for 72 hr. The times for furnace-cooling from 900°F to 700° and 500°F were, respectively, about 2 and 3.5 hr. The structures of the A1-2 pct Cu alloys are shown in Fig. 1 (overaged I) and in Fig. 2 (overaged 11). A comparison of Figs. 1 and 2 shows that in the overaged I alloys the precipitate particles along the grain boundaries are much more closely spaced and the grain boundaries are straighter than they are in the overaged I1 alloys. Further, the particle size and spacing in the grains are smaller than in the overaged I1 alloys. Microstructures of the A1-3 pct Cu alloys have not been shown; the structures of these alloys differed from those of the A1-2 pct Cu alloys only in that the distribution density of the particles was greater. The creep specimens had a gage section 1 in. long with a diameter of 0.155 to 0.195 in. Before testing, specimens were electropolished in a solution of 100 cc glacial acetic acid, and 30 cc of 60 pct perchloric acid, at 40' to 50°F, at 24 v. The specimens were kept refrigerated prior to testing to avoid precipitation at room temperature. Constant stress creep tests were conducted; the load was applied 75 min after heating of the specimens to test temperature had begun. EXPERIMENTAL RESULTS Creep-Rupture—Fig. 3 shows the log stress-log rupture life plotfor the overaged alloys studied, and also for the underaged A1-2 pct Cu alloy.' At 700°F, the stress-rupture life relationship is nearly independent of both the amount of precipitate (i.e., composition) and of the type of overaging treatment (i.e., precipitate dispersion). At 500°F it is apparent that the increase in rupture life that was ex-

Jan 1, 1960

The first record of coal anywhere in the Appalachian regions of which we now know is along the north fork of the Potomac River, above the mouth of Savage River, on a map entitled, A Plan of the upper Part of Potomack River call Cohongorooto Survey'd in the Year 1736. Benj. Winslow1 two "Cole-mines" are shown, one just above Green Island and the other just below Hopwood Run. Winslow was in charge of a surveying party to "Lay out the Bounds of the Northern Neck of Virginia," or Lord Fairfax's Grant, his party locating the liver above the mouth of the Shenandoah, while another party located it below that point, and then around Chesapeake Bay and up the Rappahannock River. The results of the two surveys were combined in a map called, The Courses of the Rivers Rappahannock and Potowmack, in Virginia, as surveyed according to Order in the Years 1736 & 1737, made by Wm. Mayo, which does not show the "cole-mines;" this map was used with the report of the boundary commission which was sent to London in the case before the Privy Council. The boundary line decided upon was surveyed on the ground in 1746, just ten years after the original one. The results of this work were shown on A Map of the Northern Neck in Virginia, According to an Actual Survey begun in the Year MDCCXXXVI, and ended in the Year MDCCXLVI, Drawn by Peter Jefferson And Robert Brooke, Surveyors, which is now in the Colonial Office in London. This map shows the "cole-mines" in the same location as on Winslow's map, and taken from his record, of course, as that part of the survey was not retraced. Faulkner, who examined all of these records in his review of the case in 1832, refers to the notes of the original survey as "No. 10. The original field notes of the survey of the Potomac River, and the mouth of the Shenandoah to the head spring of said Poto¬mac River, by Mr. Benjamin Winslow." While the notes of the 1746 survey are in the London records and photographic copies of them are in several libraries in this county, the notes of the 1736 survey cannot be found anywhere. (For Chas. J. Faulkner's report, dated Nov. 6, 1832, see Kercheval's History of the Valley of Virginia, pp. 160-173. Jas. W. Foster's Maps of the First Survey of the Potomac River, 1736-37, in Wm. and Mary College Quarterly History Mag., April, 1938, gives a complete history

Jan 1, 1942

By J. D. Wood, J. T. Smith

ALLOYS with a dispersed second phase in a metallic matrix are generally much stronger than the matrix itself. Plastic deformation in dispersion-strengthened alloys is usually confined to the matrix phase when recovery processes are active, while in the absence of recovery both phases may yield.' The alloy system studied in the present research was WC-12 wt pct Co and consisted of noncoherent WC particles dispersed in the cobalt matrix. Some particle-to-particle contact existed but not enough to produce a continuous WC skeleton. The microstruc-ture of the WC particles was characterized by very straight edges, forming a trapezoidal shape in any plane of polish. Previous investigations with WC-Co alloys at room temperature have shown that fracture of the WC particles occurs in transverse rupture testing.' Room-temperature slip was reported for WC particles after indentation for hardness measurements.3 Elevated-temperature deformation of WC particles in a WC-12 pct Co alloy was suggested by recent electron microscope studies of specimens deformed at 900' to 1000°C.4 In highly deformed alloys, the WC edges were serrated in contrast to the usual straight or smooth appearance. WC-12 pct Co and WC-15 pct Co alloys have been previously studied under elevated-temperature com-pressive-creep conditions by the present authors. Electron microscope studies of two-stage replicas from deformed specimens showed no evidence of slip or fracture of the WC particles. These specimens were brought to temperature and allowed to equilibrate prior to the application of the creep load. It was believed that the load-application rate, a crosshead speed of 0.005 in. per min on an Instron universal testing machine, was sufficiently low that recovery within the cobalt matrix was sufficient to limit the deformation to this matrix. A series of experiments was performed to evaluate the influence of loading rate on the deformation of WC-Co alloys. A WC-12 pct Co alloy was selected for these determinations. The average WC particle size was 4.45 p with an average linear separation between particles of 0.59 p. The selected temperature was 800°C and was monitored with a Chromel-Alumel thermocouple attached to the specimen. Testing was conducted in an argon-atmosphere chamber to prevent oxidation of the WC-Co specimens. This chamber was mounted on an Instron universal testing machine equipped to apply the load at a fixed rate. Each specimen was loaded to 110,000 psi compression stress at 0.05 and 0.5 in. per min. The loading rate was monitored prior to insertion of the test chamber and was found to be almost precisely the nominal rate selected. The specimens were raised to temperature and held to equilibrate with the surroundings, and then the load was applied and held for 4 hr to duplicate the exposure time utilized for the creep specimens. The time to reach full load at a crosshead speed of 0.005 in. per min was some 500 sec and was reduced to 50 and 5 sec as the loading rate was increased to 0.05 and 0.5 in, per min, respectively. The model developed by Ansell,' when recovery processes do not occur, considers that fracture or deformation of the dispersed particles is necessary to relieve back stresses on dislocation sources and allow dislocations piled up against particles to sweep out in the matrix to cause plastic deformation; he further states that, even at elevated temperatures, the dispersed-particle deformation is necessary for yielding in the absence of recovery. For the case of straight dislocation segments piled up against a straight barrier, such as the straight-sided WC particles, the shear stress, 7 exerted on a particle is: where h is the spacing between particles (0.59 p), a is the applied stress (110,000 psi), p, is the shear modulus of the matrix (6.7 X lo6 psi at 80O°C), and b is the Burgers vector of the matrix dislocation. From Eq. [I], the shear stress, 7, exerted on the WC particles when no recovery occurs is of the order of 6 X lo6 psi at 800°C. The limiting stress, F, that will

Jan 1, 1969

By S. Leber

Pole figures and pole distributions were used for the quantitative detevinination of the preferred orientations in swaged tungsten rods and the effect of subsequent wire drawing on the texture. In the swaged rod, the preferred orientation could best be described as a pseudo (111-112) [110] cylindrical texture. A secondary component was assigned the indices (110) [001]. Further reduction by swaging retained these cylindrical textures. Wire drawing caused lattice rotations about the wire axis, converting the cylindrical texture into a normal fiber texture. The conversion was initiated and proceeded lnost rapidly in the center of the wire. The (110) /001] component was converted into a (110) fiber texture by wire drawing. The effective rotations were about axes contained in the lransverse plane. The preferred orientation associated with tungsten wire usually has been assumed to consist of a (110) fiber texture. This implies rotational randomness around the wire axis. Leber1 has shown that rotation about the wire axis may be restricted resulting in a preferred orientation designated as a cylindrical texture. Specific crystal planes tended to remain aligned parallel to the wire surface. This texture seemed to be the result of the swaging operation used in the intermediate stages of fabrication. Bhandary and cullity2 detected similar textures in swaged iron wires. Peck and Thomas3 suggested that the preferential alignment of crystal planes parallel to the wire surface was the result of tangential flow, characteristic of swaging. Wire drawing, following swaging, twisted the crystals about axes parallel to the wire axis, converting the cylindrical texture into a normal fiber texture.4 In this investigation, quantitative techniques were used to more accurately characterize the cylindrical texture and to study its conversion into a normal fiber texture. PROCEDURE The material investigated was lamp-quality tungsten. Three ingots were rod-rolled and swaged to 112 mils diameter, and were then drawn to 10-mil wire. Samples were obtained after each drawing pass. (110) and (200) pole figures were obtained from samples prepared as shown in Fig. 1. To form the sample shown in Fig. l(a), l-in. lengths of wire were glued side by side to form a l-in. square. The composite was ground and electropolished to form a diametral reference surface. For certain specific tests, samples were prepared as shown in Fig. l(b). This composite was made from 10-mil-thick strips prepared by grinding on parallel longitudinal planes. The polished reference surface in this case was, in essence, the wire surface. The two forms of samples [~igs. l(a) and l(b)] were related by a 90-deg rotation around the wire axis. Because of ease in preparation, most data was obtained from the diametral samples. The X-ray data were obtained using a Siemen's pole-figure goniometer. These data were not corrected for absorption or defocusing effects, since only the angular locations of the intensity maxima were of interest. Regions of the pole figure more than 80 deg from the center were not investigated. Partial monochromatization was achieved by the use of unfiltered copper radiation and a krypton-filled proportional counter. No evidence of spurious white radiation effects5 could be detected. Therefore, more elaborate X-ray techniques were not required. Intensity levels were chosen to show all pertinent details of the orientation distributions. The reference plane for the pole figures was the diametral section. The orthogonal reference directions, shown in Fig. 1, were the wire axis, the radial axis per-

Jan 1, 1965

By G. P. Conard, R. C. Hall, J. F. Libsch

The 50 pct Fe-50 pct Co alloy undergoes a transformation from disorder to an ordered structure of the CsCl type reportedly in the vicinity of 732OC. During this process, the coercive force goes through a maximum, apparently as a result of strains associated with the coherent nucleation and growth reaction. This magnetic alloy also shows a marked increase in the ratio of residual to saturation induction, which is associated with annealing to a high degree of order with the continuous application of a magnetic field. The increase in ratio can be explained on the basis of a decrease in 90' domain boundaries and, perhaps, by an increase in anisotropy resulting from lattice distortion. THE 50 pct Fe-50 pct Co alloy undergoes a disorder-order transformation which has been reported to occur in the vicinity of 732°C1,2 The ordered structure is the CsCl type.' This magnetic alloy also shows a marked increase in the ratio of residual to saturation induction as a result of heat treatment in a magnetic field, sometimes called a response to magnetic anneal.'-' The purpose of this investigation was to study the course of the ordering reaction, the nature of the response to .heat treatment in a magnetic field, and the relation, if any, between ordering and the response. Procedure The method of approach in this investigation was to produce an initial structure as completely disordered as possible and then gradually to order the alloy by isothermal anneals at various temperatures under different conditions of the applied magnetic field. Magnetic, magnetostriction, and X-ray analyses were of primary importance in determining the property and structural changes resulting from the isothermal anneals. Rings of the 50 pct Fe-50 pct Co alloy were prepared from the elemental powders by a powder metallurgy technique, further details of which may be found in ref. 7. The initial structure was produced by annealing the specimens for ½ hr at 1000°C, cooling to and holding for ½ hr at 900°C (in the a range above the ordering temperature), and water quenching. Isothermal anneals were performed at 600°, 675°, 720°, and 740°C. For example, rings were heated to 600°C, held for a predetermined period of time, and cooled by natural cooling at a rate slightly slower than an air cool (average of 20" to 25°C per min). The tests (magnetic, etc.) were made after each heat treatment. All high temperature treatments were performed in a purified hydrogen atmosphere. The treatments at the various temperatures were carried out under one or more conditions of an applied field including 1—no field, 2—field of 20 oersteds applied on cooling only, and 3—field of 20 oersteds applied continuously during heating, holding, and cooling. Magnetic measurements were made using the standard Rowland ring technique8 with a maximum field strength of 100 oersteds. The magnetization curve, induction at 100 oersteds (B.), residual induction (Bt), and coercive force (Hc) were determined. All magnetic analysis data were based on an average of the results from three rings. A strain gage technique9 as used for the measurement of magnetostriction. The X-ray determination of the relative amount of ordered phase present was made on the ring specimen used for magnetic measurement. This was done by the back-reflection method using a rotating specimen (because of the large grain size) with unfiltered CoKa radiation and a 7 hr exposure time. Intensity measurements of the ordered line (300) were made by comparing visually the films so obtained with standard films prepared by exposing for different lengths of time a specimen given a long time anneal (high degree of order). Results In all instances the saturation induction (induction at 100 oersteds) was found to increase slightly with annealing time. This effect was small and appears to be the increase in saturation induction to be expected on ordering.10-13 The residual induction behavior was markedly influenced by the field condition during annealing, Figs. 1, 2. For the condition of no applied field, the ratio of residual to saturation induction remained essentially constant for short annealing times but showed a significant increase at longer times. With increasing annealing temperature, less time was required to produce this increase in the ratio. In the case of the 600°C anneals, the increase did not occur until approximately 20 hr, Fig. I, while on annealing at 740°C the increase was immediate, Fig. 2. Slight decreases in the ratio may be observed at 100 hr for specimens treated at 720°C and at 1 hr for those treated at 740°C. Specimens annealed in a field of 20 oersteds showed a residual to saturation induction ratio consistently higher than that for the specimens annealed without the field. The first anneal with the field (¼ hr) caused an abrupt increase in the ratio at all temperatures; thereafter, the increase in the ratio was generally similar for specimens annealed

Jan 1, 1956

By A. J. Weinig

The Liberty Bell cyanide precipitate is unique in that it is apt to vary widely in composition in the course of very short periods of time, and a method of refining and melting that would prove highly satisfactory at one cleanup would yield7almost a hopeless "mess" at a second. Table I gives a general conception of the wide range in grade and composition of those raw precipitates. It is evident that no one standard flux could be expected to produce a high-grade bullion with such a widely variable precipitate, and that any method of treatment with acid requires most careful consideration. Refining by Acids Naturally, our first efforts to improve our precipitates were directed along the lines of acid treatment. Table II embodies the results of careful sampling and analysis of one cleanup at the time when wet refining reached its maximum development at this mill. We have now discarded all methods of wet refining, successfully replacing them by a more scientific method of flux calculation described herein, but it is believed that a general description of this wet refining is warranted as it throws some interesting side lights on acid refining in general. Table I.—Range of Composition of Raw Precipitates Per Cent. Gold and silver.................................... 25.0 to 75 Zinc.............................................. 18.0to 30 Lead............................................. 0.5 to 52 Copper........................................... 0.5 to 20 Silica............................................ 1.0 to 5 Calcium oxide...................................... 4.0 to 8 Sulphur.......................................... 0.5 to 8 Column A gives the analysis of the raw precipitate; column B, that of the precipitate after heating with steam, with frequent addition of hydrochloric acid until a point was reached where the batch had a strong tend-

Jan 1, 1917

LIST OF THE MEETINGS OF THE INSTITUTE AND THEIR LOCALITIES FROM ITS ORGANIZATION TO OCTOBER, 1904 Transactions Number Place Date Vol Page I Wilkes-Barre, Pa * May, 1871 I 3 II Bethlehem, Pa August, 1871 I 10 III Troy, N Y November, 1871 I 13 IV Philadelphia, Pa February, 1872 I 17 V New York, N Y * May, 1872 I 20 VI Pittsburg, Pa October, 1872 I 25 VII Boston, Mass February, 1873 I 28 VIII Philadelphia, Pa * May, 1873 II 3 IX Easton, Pa October, 1873 II 7 X New York, N Y February, 1874 II 11 XI St Louis, Mo * May, 1874 III 3 XII Hazleton, Pa October, 1874 III 8 XIII New Haven, Conn February, 1875 III 15 XIV Dover, N J * May, 1875 IV 3 XV Cleveland, 0 October, 1875 IV 9 XVI Washington, D C February, 1876 IV 8 XVII Philadelphia, Pat June, 1876, V XVIII Philadelphia, Pa October, 1876 V 9 XIX New York, N Y February, 1877 v 27 XX Wilkes-Barre, Pa * May, 1877 vi 3 XXI Amenia, N Y October, 1877 vi 10

Jan 1, 1910

By Robert G. Johnson, Richard J. Prosen

THE present work was done in connection with a program for investigating metal-to-ceramic braze techniques using the well-known reactivity of titanium with certain ceramic oxides. The investigation extended over the range of 0 to 30 pct Ti. The indium was obtained from the Indium Corp. of America and was specified to be 99.97 pct pure. The titanium was supplied by Metals Disintegrating Co. and was stated to be 99.5 pct pure. Each 2 to 4 g quantity of the alloy compositions studied was prepared using a mixture of 300 mesh powders pressed into pellet form. The pellets were heated in thin-walled molybdenum crucibles using a resistance-wound furnace in a vacuum less than 10-4 mm of Hg. Little reaction occurred between the molten alloy and the crucibles at the temperatures and short time intervals used. Only slight spectroscopic traces of molybdenum were found in the melt after a typical period of heating. The points shown on the phase diagram of Fig. 1 represent thermal arrest measurements. The phase boundaries shown are consistent with the thermal arrest and X-ray data obtained. The temperatures were determined using a Pt-Pt 10 pct Rh thermocouple with the junction spot-welded to a short molybdenum rod. The rod was almost completely immersed in the liquid metal, so that good thermal contact with the melt was achieved. The small mass of the crucible and its contents made it possible to obtain many heating and cooling curves in a few minutes time, an advantage which helped to minimize the effects of indium evaporation at the higher temperatures. A Brown strip chart recorder was used to display the thermal arrest curves. To check the technique, the melting point of 99.999 pure Al was measured and found to be within 1 of 660.2c, the accepted melting point. The upper limit of temperature with this technique was about 900°C beyond which the evaporation rate of indium became great enough to alter appreciably the alloy composition during the runs. A peritectic transition was found at 796°+ 5°C from 1.5 to 30 wt pct Ti. It was not found at 0.5 or 1.0 pct. A small super-cooling effect was observed. The melting-point transition to the B + L phase was found up to 20 pct Ti but not at 25 pct. Within the 1 deg accuracy of the measurement, the transition temperature was that of pure indium, 156°C. The liquidus line to the left of the 1.5 titanium point was located only approximately. The two crossed circle points at 1.0 and 0.5 pct Ti place a lower limit on the liquidus line and were determined by observing visually the cessation of vibrations in the melt caused by the damping effect as B-phase crystals were formed during cooling. The B-phase boundary was found at 23.8 pct Ti by X-ray analyses of small single crystals of the B phase isolated from 2 pct Ti melts. The compound was found to be Jetragonal with lattice dimensions of c = 3.052A and a = 10.094W. From the unit cell dimensions and the measured density of 6.42 i 0.05 g per cc, the compound was determined to be In4Ti3 which has 23.8 pct Ti. The calculated density of 6.44 g per cc is obtained assuming 2 mol

Jan 1, 1962

GENTLEMEN : Herewith are transmitted the reports of your Treasurer and the Chairmen of your standing committees on Admissions, Membership, Papers and Publications, and Library for the calendar year 1931. To these reports you are referred for further details of the year's activities. Finances.-Depressed industrial conditions prevailing throughout the year were reflected in a substantial decline in current revenue. Aside from interest on sundry special funds (but including that from the Life Membership, Library, and General Reserve Funds) total receipts amounted to $168,274, compared with $194,636 in 1930. The principal items of decrease were $17,000 in advertising income from the monthly magazine MINING AND METALLURGY, and about $9,600 in dues and initiation fees. Of this shrinkage $4,000 is accounted for by decrease in the number of new members enrolled; and $5,600 by diminished income from current dues and arrearages. This naturally has coincided with an \ increase in delinquency and "drops" or suspensions for nonpayment of dues. The decline in advertising income, amounting to 38 per cent as compared with that of 1930, in general paralleled the experience of all technical and trade publications; and it is problematical whether 1932 will show as large a return from advertising as did 1931.

Jan 1, 1932

By T. E. Leontis, D. H. Feisel

MAGNESIUM alloys containing rare earth metals have received considerable attention during the past several years because of the need for light alloys having high strength and creep resistance at elevated temperatures. Although much of the work reported earlier has dealt with alloys containing Mischmetal, it has been shown in two previous papersl, V hat distinctly different effects are produced by various rare earth metals and rare earth metal mixtures on the properties of magnesium. For example, much higher strengths are obtained in magnesium alloys containing didym-ium (essentially neodymium plus praseodymium) than in alloys made with Mischmetal, which contains all the rare earth metals in the proportions in which they occur naturally in the monazite ore. Mg-rare earth metal alloys are characterized by a relatively coarse grain size, which greatly impairs castability. The addition of zirconium as a second alloying ingredient has been shown8,7 to refine the grain size, which also produces a distinct improvement in the strength properties. Certain Mg-Mischmetal-Zr and Mg-Mischmetal-Zn-Zr alloy compositions which are currently being produced commercially have been discussed in dytail by Nelson and Strieter,8,4 who also present some in- formation on a Mg-low Ce-Mischmetal-Zr alloy, and by Nelson.8 A patent issued to Jessup, Emley, and Fisher9 emphasizes the superiority of Mg-didymium-Zn-Zr alloys over the corresponding alloys made with Mischmetal. The purpose of this paper is to present the results of an extensive investigation concerned with the effect of increasing amounts of zirconium on magnesium sand casting alloys containing several different rare earth metal mixtures in varying amounts. The effect of the addition of zinc to some of these alloys is also being reported. Preparation and Testing of Alloys The alloys studied in this investigation were prepared in small laboratory melts according to the melting procedures described by Nelson1" as the Crucible Method. Electrolytic magnesium having the composition shown in Table I was used as the starting material. The rare earth metal alloying ingredients used in preparing these alloys were essentially of the compositions listed in Table 11. Some of the didymium-containing alloys were prepared using a Mg-didymium hardener. The rare earth metal content of this hardener analyzed 1.2 pct Ce, 10.4 pct Pr, 80.8 pct Nd, and 7.6 pct La. The zirconium was added in one of three forms: 1) as sponge zirconium obtained from the Bureau of Mines; 2) as a fused salt consisting of 50 pct ZrCl, and 50 pct alkali chlorides from which the zirconium is reduced by the magnesium; or 3) as a Mg-Zr hardener. The alloying procedures and melt hand-

Jan 1, 1958