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By E. W. Newman

During 1943 and 1944, there was an urgent need for certain grades of optical calcite (Iceland spar) for instruments for ' military uses. To find a supply of this material, prospecting was carried out in Montana, California and Colorado. Although some production was obtained by the work in California, the best results were from prospecting the large calcite veins of south central Montana. The bulk of the optical calcite mind during World War II has come from that area. The Bureau of Mines took an active part in the search for optical calcite in Montana. It examined most of the known calcite veins in the 70-mile distance between Wilsall, on the Shields River: and Absarokee, on the Still water River, and conducted exploration on several of the deposits. The Geological Survey also took an active part by mapping many of the veins. Actual mining of the calcite was performed at first by Calcite Operators, Inc., and later by the Metals Reserve Co., through an agent. A sorting plant was established at Clyde Park, where custom material could be sold. These activities stimulated mining by private operators. To be suitable for military uses, the calcite mined had to meet rigid specificstions as to both size and quality. Individual crystals had to be clear and transparent and if in the form of rhombs had to measure at least 7/8 in. on each edge. Some color and a few inclusions in the calcite were allowable, but material with incipient or developed cleavages, or showing twinning other than parallel to the base, was unacceptable. History of Deposits The existence of large veins of calcite in south central Montana has long been known, and for many years the farmers of this region have used the common vein calcite for producing grit for chicken feed. According to reports, the fist optical calcite produced from Montana came from the Cartwright deposit near Grey-cliff,' but until recently the mining of optical calcite in Montana has been limited to spasmodic searching for small crystals suitable for making nicol prisms for saccharimeters and microscopes, or for mineral specimens. The possible need of substantial amounts of optical calcite for military uses began to appear late in 1942 and early in 1943, therefore the Polaroid company began searching for a source of supply in Montana and California. Work on the Wade property near Clyde Park was started on a small scale in the fall of 1942, by .4. H. Hansen, of Clyde Park. During the winter and spring of 1943, a modest quantity of optical calcite was mined and shipped to the Polaroid Corporation, Cambridge, Mass. Most of this was produced from the "Hansen vug," which was found close to the surface. Early in the summer of 1943, mining on the Wade property was undertaken by Calcite Operators, Inc., a company organized for mining optical calcite from the

Jan 1, 1948

By B. H. Cody

THE Morenci concentrator of the Phelps Dodge Corporation is a part of the project that was completed after five years had been spent in development of the open-pit mine, equipment and process testing in the former No. 6 concentrator, and construction of the reduction works. The reduction works, of which the concentrator is a part, is about a mile and a quarter southeast of Morenci, on the highway that leads up Morenci Canyon. The concentrator has a nominal capacity for the treatment of 45,000 tons of ore daily. The original plant, which has a rated capacity of 25,000 tons of ore daily and is now in its fifth year of operation, began production on Jan. 30, 1942. The addition, to increase the capacity 8o pct, began operation on Dec. 1, 1943. The equipment of the original plant has been described in MINING AND METALLURGY (May 1942). No changes in equipment were recommended for installation in the concentrator extension and only one major change, forced by a shortage of maintenance labor, has since been made. Metallurgical treatment has been altered in some ways as experiments progressed and as labor and economic conditions dictated. No complete description of the operation of the concentrator has been published, so this paper will record such operating and equipment changes as have been necessary, the operating methods that have been developed and the metallurgical results that have been obtained. Descriptions are given in the order of the processes with a flowsheet and an equipment list of each process for convenient reference. The questions asked by engineer visitors have guided the detail in which operation and maintenance are described. During the period Jan. 30, 1942 to Sept. 1, 1946, ore milled has totaled 43,595,253 dry tons, from which 1,643,885 tons of concentrate have been made, containing an indicated production of 783,164,809 lb of copper. The principal results obtained in operation of the concentrator during the years 1942 to 1945, inclusive, and to Sept. 1, 1946 are shown in Table 1. A graphic general flowsheet of the plant is given in Fig I. ORE The Morenci ore that is now being treated is a medium-hard monzonite porphyry in which the principal sulphide minerals are chalcocite and pyrite. A minor amount of covellite is present. Chalcopyrite and bornite have been observed under the microscope. The chalcocite occurs mainly as a coating on pyrite. Some of the coatings are so thick that the pyrite presents the appearance of being an inclusion in chalcocite. Some are less than one micron thick and are barely visible at 500 diameters magnification of a polished cross section. Some chalcocite is present as a dissemination in the gangue. Various oxidized copper minerals are present as a result of oxidation in place but they represent a minor proportion of the copper minerals of the ore body. Oxidation

Jan 1, 1947

By Hugh D. Pallister, Richard W. Smith

The Alabama flake-graphite industry has flourished only in times of war when importations of foreign graphite for crucible use have been greatly curtailed or cut off. World War I was a boom period and in 1918 some 30 plants produced 7,795,475 Ib. of flake graphite. The industry languished following the war and no graphite was produced from 1929 to 1939. The Federal Bureau of Mines began investigating the Alabama graphite deposits in 1940 and worked out modern recovery methods that were applied to production during part of World War 11. A prospecting program disclosed reserves of over 25 million tons of graphtic schists. In 1942 the War Production Board authorized the enlargement of the only plant then producing flake graphite and the construction of two new plants. Production of flake graphite from these three plants in 1943 is estimated at 8,100,000 lb. Increased imports from Madagascar late in 1943 shut down one of the new plants and curtailed production at the other. Alabama flake graphite has not yet been able to compete with Madagascar graphite for use in the manufacture of any but small graphite crucibles. The future of the industry must depend on meeting the higher carbon content demanded for other uses. Introduction The flake-graphite deposits of Alabama are confined to a narrow belt extending for about 60 miles southwest from the northeast corner of Clay County across Coosa County to the edge of the Coastal Plain in Chilton County (Fig. I). The continuity of the beds is broken by a 10-mile gap between Millerville in Clay County and Goodwater in Coosa County. The Clay County beds extend about 27 miles northwest of this gap, with a width of 3 to 4 miles near Millerville and of less than a mile at the northeast end. The Coosa-Chilton are? is about 33 miles long with a fairly consistent width of 2 to 3 miles. Geologically the graphite belt lies near the northeast boundary of the outcrop of metamorphic rocks of the Ashland series, a complex group of intensely folded and faulted beds of pre-Cambrian age composed mostly of quartz-mica schist, in which the mica is predominantly muscovite; garnet-mica schist, in which biotite is more common; and hornblende schist. Flake graphite is found in commercial quantities only in the quartz-mica schist. The best graphite, both in quantity and quality, is found in schist cut by numerous small pegmatite stringers along the planes of the schistosity. The pegmatites themselves contain little graphite, but the adjacent country rock is normally rich. . The schist was derived through the recrystallization of shale during the intrusion of the pegmatites, the graphite being derived from amorphous carbon in the shale. The intrusion of the pegmatites, and therefore the size and quantity .of the graphite flakes, seems to have a structural control.

Jan 1, 1948

By Hugh D. Pallister, Richard W. Smith

The Alabama flake-graphite industry has flourished only in times of war when importations of foreign graphite for crucible use have been greatly curtailed or cut off. World War I was a boom period and in 1918 some 30 plants produced 7,795,475 Ib. of flake graphite. The industry languished following the war and no graphite was produced from 1929 to 1939. The Federal Bureau of Mines began investigating the Alabama graphite deposits in 1940 and worked out modern recovery methods that were applied to production during part of World War 11. A prospecting program disclosed reserves of over 25 million tons of graphtic schists. In 1942 the War Production Board authorized the enlargement of the only plant then producing flake graphite and the construction of two new plants. Production of flake graphite from these three plants in 1943 is estimated at 8,100,000 lb. Increased imports from Madagascar late in 1943 shut down one of the new plants and curtailed production at the other. Alabama flake graphite has not yet been able to compete with Madagascar graphite for use in the manufacture of any but small graphite crucibles. The future of the industry must depend on meeting the higher carbon content demanded for other uses. Introduction The flake-graphite deposits of Alabama are confined to a narrow belt extending for about 60 miles southwest from the northeast corner of Clay County across Coosa County to the edge of the Coastal Plain in Chilton County (Fig. I). The continuity of the beds is broken by a 10-mile gap between Millerville in Clay County and Goodwater in Coosa County. The Clay County beds extend about 27 miles northwest of this gap, with a width of 3 to 4 miles near Millerville and of less than a mile at the northeast end. The Coosa-Chilton are? is about 33 miles long with a fairly consistent width of 2 to 3 miles. Geologically the graphite belt lies near the northeast boundary of the outcrop of metamorphic rocks of the Ashland series, a complex group of intensely folded and faulted beds of pre-Cambrian age composed mostly of quartz-mica schist, in which the mica is predominantly muscovite; garnet-mica schist, in which biotite is more common; and hornblende schist. Flake graphite is found in commercial quantities only in the quartz-mica schist. The best graphite, both in quantity and quality, is found in schist cut by numerous small pegmatite stringers along the planes of the schistosity. The pegmatites themselves contain little graphite, but the adjacent country rock is normally rich. . The schist was derived through the recrystallization of shale during the intrusion of the pegmatites, the graphite being derived from amorphous carbon in the shale. The intrusion of the pegmatites, and therefore the size and quantity .of the graphite flakes, seems to have a structural control.

Jan 1, 1948

By J. E. Burke

RECENT investigations have elucidated many of the phenomena of the grain growth process, but have also revealed some conflicting and unexplained results. Beck and his co-workers1,2,3 have shown that grain growth continues with continued heating at one temperature until the average grain size approaches the thickness of the specimen, Plotting the logarithm of the average grain diameter, D, against the logarithm of the annealing time, t, they find the straight line relationship given by the equation: [D=Ktn [11] with possible small deviations at short annealing times. K and n are constants at constant temperature. On the other hand, Walker4 finds that, in alpha brass, the rate of growth falls off more rapidly than indicated by Eq I after long annealing, so that an equilibrium grain size is approached. Burke5 showed, using Walker's data, that time and temperature for grain growth are apparently related through an activation energy, H, according to the relationship: [t, Hr i '_ III t„ = R \T, - ~) [2]] where t1 and t2 are the annealing times necessary for the average grain size to increase from Do to D at temperatures T1 and T2 and R is the gas laws constant. In the case quoted, H had the value 60,000 cal per mol. The apparent validity of this relationship, at least up to 700°C, and the approximate value of H were later confirmed by Beck.' The results obtained by Beck, Kremer, Demer and Holzworth2 for aluminum and aluminum-magnesium alloys could not be satisfied by such a relationship, since the slope of the isothermal curves increased with increasing temperature. These data indicate and Beck, Holzworth and Hu6 later demonstrated experimentally that the only apparent factor controlling the rate of grain growth at constant temperature is the grain size. While many of the phenomena have been elucidated, a reasonably quantitative explanation of the process is lacking. There exists uncertainty even as to the primary driving force for grain growth, although there is a considerable body of indirect evidence that the interfacial energy of the grain boundary is responsible.7,8,10 Making implicit use of this assumption, several authors14,15 have pointed out that grain boundaries should migrate toward their center of curvature. Harker and Parker' have advanced this concept furthest, and show that one can expect grain boundary migration to occur only when the grain faces are curved, or when they meet at non-equilibrium angles. When the face is curved toward a grain A, for example, the atoms in the surface of grain B, on the other side of the boundary, are on the average more surrounded by the atoms of their lattice than the atoms on the surface of grain A. Because of thermal motion, the atoms at the interface will sometimes be attached to grain A and

Jan 1, 1948

By J. Suiter, H. F. Ryan

H. F. Ryan and J. Suiter (CSIRO)—In this paper the authors have presented "a physical model which has as its central hypothesis the solution strengthening of regions along grain boundaries in the order of tens of angstroms thick", and their calculations have used 40Å as the zhalf-width of this boundary region. Selection of this value by the authors suggests that they were unaware of a number of recent field-ion microscope observations of grain boundary structures (e.g., Refs. 29 and 30). The accompanying figure, Fig. 9, shows a portion of an ion micrograph of a tungsten specimen containing a grain boundary, and the regular arrangement of atoms in various crystal planes in each grain can be seen, except in the boundary zone which is not more than two atom diameters in width. Since it is expected that solute atoms will segregate only to the region where the lattice is disturbed, it would seem that a value of 4Å for the half-width of the boundary region would be more appropriate than the value of 40Å assumed by the authors. If the former value is used in Eq. [8] of their paper to obtain curves showing solute concentration in the grain boundary as a function of temperature, the resulting curves differ significantly from those obtained by the authors. Although there are only relatively slight changes in the regions corresponding to higher temperatures (i.e., grain boundary concentrations of approximately 1 at. pet), at lower temperatures the curves are no longer realistic. For example, the curve corresponding to u = 7000 cal per mole gives a solute grain boundary concentration in excess of 100 pet at a temperature of approximately 360°K, and "flattens out" at a grain boundary concentration of about 300 pet! Similar results are obtained with each of the other curves. Ion microscopy of dilute solid-solution alloys has shown that solute atoms give rise to image points which in most cases are of higher intensity than those of the solvent atoms.31 If the same behavior occurs when the solute atoms are present in much lower concentrations then ion microscopy should provide a sensitive tool for studying the segregation of impurities to the grain boundary regions. Although many grain boundaries in tungsten have been examined after different thermal and mechanical treatments, there has not been, as yet, any systematic study of such segregation. In general the micrographs show no clear indications of marked grain boundary segregation, but occasionally areas are found where the grain boundary contains an appreciable number of image points of high intensity in a very narrow zone, see Fig. 9. If it is assumed that these correspond to impurity atoms then it is possible to estimate the impurity concentration both in the grain boundary and within the body of the grains. Application of this method (to a larger area

Jan 1, 1965

By David J. Mack, A. H. Kasberg

The transformation characteristics are found to resemble a similar binary alloy. The differences are due to the alpha iron particles. While strength properties of the isothermally transformed alloys are high, ductility is low, resulting in high notch sensitivity. The elastic modulus can be varied widely and correlates with strength. Abnormal grain growth sometimes occurs. A CONSIDERABLE amount of work has been done on the isothermal transformation of high purity aluminum bronzes using the methods pioneered by Davenport and Bain.' The first isothermal study of these alloys was made by Smith and Lind-lief,' but more recently Mack", " and Klier and Grymko5 have continued the work. In commercial aluminum bronzes, one or more elements are always added to refine the ß grain size and to improve the mechanical properties. The effect of these elements on the isothermal transformation has not been reported in the literature. No systematic study of the properties of isother-mally transformed aluminum bronzes has apparently been reported, although adequate information is available on their properties after more conventional heat treatments. The fact that a eutectoid alloy will reject face-centered cubic a during isothermal transformation at appropriate temperatures2'" warrants investigation of the properties of such structures. Another cogent reason for determination of properties is the fact that the modulus of elasticity of the eutectoid alloy varies widely with the nature of the heat treatment." Preliminary experiments7 indicated that a high purity eutectoid alloy would not give reproducible results in property determinations because of ex- cessive ß grain growth during heat treatment, a single ß grain frequently occupying the entire cross-section of a standard test bar. For this reason a commercial aluminum bronze containing iron as a grain growth inhibitor was used. The isothermal transformation diagram of the alloy was first determined. On this basis, the heat treatments necessary to produce representative structures were selected and the properties determined. Material A commercial alloy (Ampco Grade 20) of the following composition was used: Cu, 83.68 pct; Al, 12.31 pct; Fe, 3.68 pct; Ni, 0.28 pct; and Mn, 0.03 pct. This alloy proved to be very close to the eutectoid composition and may be compared with the accepted value of 11.8 pct A1 in the binary Cu-A1 system. Comparison is valid only because of the "negative replacement effect" of the iron? Since traces of excess y² are present, the alloy is slightly hyper-eutectoid. The material was received in the form of 3/4 in. round, hot extruded bars. Specimens of approximately ? in. thickness were cut from this stock and drilled to allow suspension in the salt bath. The structure of the as-received material varied from 5 to 40 pct a + y2* in a matrix of ß. The amount of a + y² present was dependent upon the ß grain size of the extruded material. The coarse grained portions did not form as much a + Y, as did

Jan 1, 1952

By A. V. Deforest, C. W. Macgregor, A. R. Anderson

One of the important problems in the design of structures and machine parts subjected to rapidly applied loads is the determination of the strength and ductility of the material itself under such conditions. Realizing the need for such information, many investigations have been carried out in the past. Most of these experiments have been made using notched bars in bending either with the Charpy or Izod impact machine. While yielding valuable data on the effect of notches in the energy absorption of the material and on the condition of heat-treatment, this form of test does not lend itself readily to a determination of fundamental stress-strain relations. For this and other reasons, more attention has been paid recently to the tension impact test. An extensive literature already exists on the subject and only those investigations somewhat closely related to the present paper will be mentioned. For a more comprehensive list, the reader is referred to the Symposium on Impact Testing or the A.S.T.M., 1938. The work of Mann.' Clark and Dätwyler,2 Nádai and Manjoine,3 Winlock and Leiter,4 Deutler,5 and Brinkmann,6 however, deserves especial mention. In most of the previous investigations on the subject, when stress-strain relations were obtained under high rates of loading, it was the common procedure to determine stresses based on the original area and strains based on the original length. Stress-strain curves were then constructed by P ALo plotting So = 1/A0 as a function of eo = ALr,o where A0 and Lo refer to the original area and gauge length, respectively. At present there exists a paucity of true stress-strain data in the impact problem. The advantages of constructing so-called true stress-strain curves in order to reveal the fundamental physical properties of the material for the tension test were discussed recently by one of the authors.7'8 It was shown that the true physical behavior of the material in the tension test could best be represented P by plotting the average true stress, S = 2P as a function of 6 = q' = log —r = log ~9L where P, A, L, S, E, and q' refer to the load, the cross-sectioned area while the load P is applied, the actual gauge length, the average true stress, the true strain and true reduction in area, respectively. Besides giving a better physical representation, the method has certain additional advantages in that the stress-strain curve so plotted becomes a straight line from the maximin load point to fracture. The construction of such curves, however, while comparatively simple for the slow rates of loading customarily used in the tension test, presents certain dificulties for tensile impact in that both loads and diameters are required throughout the test. The continuous measurement of test-piece diameters to fracture under impact conditions offers considerable experimental difficulty. In order to make it feasible to

Jan 1, 1942

By A. V. Deforest, A. R. Anderson, C. W. MacGregor

One of the important problems in the design of structures and machine parts subjected to rapidly applied loads is the determination of the strength and ductility of the material itself under such conditions. Realizing the need for such information, many investigations have been carried out in the past. Most of these experiments have been made using notched bars in bending either with the Charpy or Izod impact machine. While yielding valuable data on the effect of notches in the energy absorption of the material and on the condition of heat-treatment, this form of test does not lend itself readily to a determination of fundamental stress-strain relations. For this and other reasons, more attention has been paid recently to the tension impact test. An extensive literature already exists on the subject and only those investigations somewhat closely related to the present paper will be mentioned. For a more comprehensive list, the reader is referred to the Symposium on Impact Testing or the A.S.T.M., 1938. The work of Mann.' Clark and Dätwyler,2 Nádai and Manjoine,3 Winlock and Leiter,4 Deutler,5 and Brinkmann,6 however, deserves especial mention. In most of the previous investigations on the subject, when stress-strain relations were obtained under high rates of loading, it was the common procedure to determine stresses based on the original area and strains based on the original length. Stress-strain curves were then constructed by P ALo plotting So = 1/A0 as a function of eo = ALr,o where A0 and Lo refer to the original area and gauge length, respectively. At present there exists a paucity of true stress-strain data in the impact problem. The advantages of constructing so-called true stress-strain curves in order to reveal the fundamental physical properties of the material for the tension test were discussed recently by one of the authors.7'8 It was shown that the true physical behavior of the material in the tension test could best be represented P by plotting the average true stress, S = 2P as a function of 6 = q' = log —r = log ~9L where P, A, L, S, E, and q' refer to the load, the cross-sectioned area while the load P is applied, the actual gauge length, the average true stress, the true strain and true reduction in area, respectively. Besides giving a better physical representation, the method has certain additional advantages in that the stress-strain curve so plotted becomes a straight line from the maximin load point to fracture. The construction of such curves, however, while comparatively simple for the slow rates of loading customarily used in the tension test, presents certain dificulties for tensile impact in that both loads and diameters are required throughout the test. The continuous measurement of test-piece diameters to fracture under impact conditions offers considerable experimental difficulty. In order to make it feasible to

Jan 1, 1942

By B. Blumenthal

THE present investigation was planned as a survey of the lead-rich portion of the ternary lead-antimony-silver system by thermal analysis. Since, however, a rigorous application of the conventional thermal analytical method is time consuming, an attempt was made to speed up the investigation by reducing the time required for a single thermal analysis. This was done by increasing the rate of cooling to 12° to 18°C. per minute. Since such a rate does not permit even an approach to equilibrium conditions, the melt was stirred vigorously by a stirrer operating at the high rate of 665 r.p.m. This proved to be effective in obtaining cooling curves with distinct points of arrest and of excellent reproducibility, which satisfactorily compare with those obtained at a rate of 1° to 2°C. per min. with or without slow stirring (Fig. 1). By this method the lead-rich end of the lead-antimony system and a series of ternary alloys in sections parallel to the lead-antimony side of the ternary system were investigated and it was observed that the two branches of the' liquidus curve of the .binary alloys did not intersect at the eutectic temperature. An equivalent effect was observed in the ternary system. The eutectic temperature of the binary lead-antimony system was found to be 252.0°C., which confirms the recent investigation by Pellini and Rhines,1 who determined the eutectic temperature to be 251.5°C. The observation that the curves of primary crystallization of the lead-antimony system do not intersect at the eutectic temperature was previously made by Dean.2 Dean explains the phenomenon by assuming the existence of a compound Sb4Pb. He felt that super-cooling was not the cause of the phenomena because he was unable to influence them by inoculation. The X-ray investigation by Solomon and Morris-Jones,3. the metallographic investigations by Stead,4 Charpy,5 Gontermann,6 and Dean, Zickrick and Nix,7 and the numerous investigations of physical properties, definitely disprove the occurrence of any compound. The work of Dean was not confirmed by Broniewski and Sliwoski,8 whose experiments did not show any irregularity and who report a eutectic composition of 13 per cent antimony and a eutectic temperature of 250° to 252°C. at a rate of cooling of about 6°C. per min. Abel, Redlich and Adler9 then report a eutectic composition of 12.1 per cent upon reviewing the previous, publications and adding a few of their own cooling curves. In 1934 Quadrat and Jiriste10 found from careful analyses of the bottom portion of slowly cooled hypereutectic melts that the eutectic contains only 11,4 to 11.5 per cent antimony. (Previous analyses by Stead4 in 1881 gave 13 per cent:) Weaver," however, reported in 1935 that cooling curves indi-

Jan 1, 1943

By J. D. Price, W. M. Bertholf

One of the chief difficulties with which the operator of a coal washing plant has been forced to contend is the handling of the very fine coal. First he has the problem of separating the fine coal from washery water. This is usually accomplished by the use of settling cones or Dorr thickeners: in either event the separated fine coal contains a high amount (40 to 80 pct) of water and, somewhat loosely, dependent upon the size of the coal particles present, may be known as sludge or slurry. His second problem is the satisfactory further dewatering of such separated sludge and/or slurry. At the coal washing plant of the Colorado Fuel and Iron Corp., washed coal from the Deister Plat-O tables is sluiced to a stationary inclined de-watering screen provided with 3/16 by 1-in. slots, and the coarse coal passing over this screen is conveyed by a Baum-type elevator and a flight-type distributing conveyor to a battery of Carpenter centrifugal driers. The fine coal and water passing through the openings of the primary dewatering screens, plus the fine coal passing through the screens of the centrifugal driers (and no small portion of which is the result of the disintegrating action of these driers) is pumped to two 30-ft Link Belt settling cones. The sludge recovered as underflow from these cones was formerly dewatered on stationary screens having 1/16 by 1-in. slots and discharged on top of the coarse washed coal in the Baum drainage conveyor; but after a relatively few hours of op eration the circulating load of fine coal on this conveyor built up to a point where it became necessary to reduce the quantity of feed to the washing tables. The original arrangement of our coal washing and dewatering equipment is shown in Fig 1. In order to regain the loss in active throughput which had been caused by this circulating load, an installation of six vibrating filters was made during the year of 1936. This resulted in an increase in normal tonnage of washed coal from 1430 to 1750 tons per 8-hr shift, a gain of slightly over 22 pct. This increase in throughput has made a very substantial decrease in the " conversion cost" per ton of washed coal. Since the vibrators were installed, we have gained about 2,000,000 tons in production, compared to what would have been produced in the same number of shifts at the former rate. Putting it in slightly different form, we have saved in the past 12 yr the cost of 1400 operating shifts in the washery. Fig 2 shows the location of the vibrating filters as applied to the original flowsheet. It will be noted that the sludge from the bottom of the settling cones is passed through a distributing box and thence to the filters. The de-watered coal from the filters is de-livered to the conveyor receiving the dried coal from the Carpenter driers.

Jan 1, 1950

By A. Raman

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

Jan 1, 1967

By Herbert H. Uhlig

ALTHOUGH the mechanical properties of high-carbon manganese-iron alloys, particularly the Hadfield manganese steels, have been established, the literature discloses discrepancies in the reported properties for the low-carbon alloys. Hadfieldlo summarized the existing data up to 1927, including the investigations of Guillet, Arnold, Strauss, Burgess and Aston, and reported his own values for alloys containing for the most part from 0.06 to 0.15 per cent carbon. He noted: From these comparisons it will be seen that while there is a broad and general agreement as to the character of the alloys at the different manganese percentages, there are disparities in individual cases, especially as regards the degree of toughness or brittleness displayed by an alloy with certain percentages and with particular types of treatment. These differences are not always readily explainable. Ib His data showed that alloys containing 4 to 10 per cent manganese water-quenched from 1000°C. were brittle and hard with maximum brittleness at about 7 per cent. Slight improvement in ductility was obtained with compositions from 10 to 17 per cent manganese. Alloys containing up to 17 per cent manganese slowly cooled rather than quenched from 870°C., he found, were slightly improved in ductility with significant improvement in alloys analyzing 4.1 and 4.8 per cent manganese. Recently Walters, Kramer and Loringa reported mechanical properties for alloys made up from electrolytic manganese and ingot iron and containing from 0.02 to 0.04 per cent carbon. They showed that a tempering treatment at 540°C. (1000°F.) for one hour significantly improved the ductility of compositions ranging from 6.7 to 20.7 per cent manganese. The differences of these compared with Hadfield&apos;s results they considered to originate in this tempering treatment plus the fact that Hadfield&apos;s alloys contained higher carbon and phosphorus (0.06 to 0.15 per cent C; 0.06 to 0.07 per cent P compared with 0.02 to 0.04 per cent C, <0.001 per cent P). In this paper it is shown that of the low- carbon alloys (0.02 to 0.03 per cent) containing from 3.3 to 21.5 per cent manganese moderately or rapidly quenched from 1000°C. some are brittle or ductile, depending on presence or absence of hydrogen. Hydrogen is readily absorbed at high temperatures, and much of it is retained when the alloys are cooled to room temperature. The presence of hydrogen in the range of composition from 10 to 18 per cent manganese is a major factor in determining relative ductility. At 22 per cent manganese, and also at compositions below 10 per cent manganese, factors other than or in addition to hydrogen play a role. These are discussed. Also data are presented to show that hydrogen absorbed by the high-carbon alloys of Hadfield composition is without effect on their mechanical properties.

Jan 1, 1944

By R. F. Decker, J. R. Mihalisin

Phase transformations in a series of relatively pure nickel-titanium-aluminum binary and ternary alloys were studied. The purpose was to clarify age-hardening mechanisms, especially in predominantly titanium-hardened compositions. The micro-structures, as determined on a tirne-temperature-transformation basis by light and electron microscopy and X-ray diffraction, were correlated with room temperature and hot hardnesses. The stability of the ? phase under nonequilibrium conditions was shown to be important in this system. MANY of the alloys designed for service in the temperature range of 1200oF (649°C) to 1800°F (980°C) are austenitic iron-.nickel base alloys hardened by titanium and aluminum. The control of high-temperature properties of these alloys has been advanced by the knowledge of microstructures provided by the equilibrium diagrams of Taylor and Floyd1 and Taylor.2, 3 However, there have been notable instances in the predominantly titanium-hardened alloys where the correlation of properties with microstructure and the equilibrium diagrams has been unsuccessful. Mihalisin and carrol14 have noted in electron microscope studies of commercial alloys of this type that a fee phase precipitates and transforms to 71 (hep Ni3Ti) in stress-rupture tests. Bieber5 found that this fee phase remained in nickel-chromium-titanium alloys even when aluminum was excluded. Age hardening in iron-nickel base alloys has been attributed to 71 by Craver, Aggen, and Dyrkacz,6 ? (fee phase based on Ni3Al) by Beattie and Hagel7 and both phases by Lena,8 Yet, on the basis of the nickel-titanium-aluminum equilibrium diagram of Taylor and Floyd shown in Fig. 1, it has been difficult to understand the presence of ? in low aluminum alloys. Furthermore, the characteristic coarse dispersion of 71 has not been commensurate with the marked aging response. Also there have been anomalous grain boundary transformations in the iron-nickel base alloys which have markedly reduced notched stress rupture properties.9 These have been related to boron content and residual cold work. Recently, Golubtsova and Mashkovich,10 Buckle and Manene11 and Bogaryatskii and Tyapkin12 have noted a transition fee Ni3Ti in titanium-hardened nickel-base alloys. It was apparent from the latter studies that a transition phase was important in the nickel-titanium-aluminum system. The purpose of this study was to identify this phase, measure its transformation characteristics and kinetics, and attempt to correlate these findings with age hardening. It was believed that time-temperature-transformation studies, because of their adaptability to transition phases, would be of most value for this investigation. Accordingly, this method of study was undertaken on relatively pure nickel-titanium-aluminum alloys with controlled variations in boron content and residual cold work. EXPERIMENTAL PROCEDURES Compositions were selected from the nickel-titanium-aluminum isothermal section of Taylor and Floyd.&apos; These compositions are plotted in Fig. 1 and were selected to obtain equal aging potential of approximately 15 pet by volume of the equilibrium precipitate. The materials were vacuum melted from

Jan 1, 1961

By G. T. Higgins

PREVIOUS workers1,2 have found evidence of exaggerated grain growth or secondary recrystallization on annealing sponge zirconium at temperatures high in the a, phase field, but no details of the orientation relationship between the secondary grains and "as-recrystallized" matrix were reported. In other hexagonal metals, namely dilute Mg-A13 and Cd-zn4 alloys, secondary recrystallization has been observed in which the secondary grains are related to the primary recrystallized structure by rotations about the c axis. These rotations are thus comparable with the rotations about the (111) axis observed in the secondary recrystallization of fcc metals. In the current work secondary recrystallization has been observed on annealing iodide zirconium at 800°C and the associated changes in crystallographic texture have been examined. The material employed was arc-melted iodide zirconium of the following composition: Impurity O H Fe Hf Pb I Ni C1 A1 ppm by wt 130 5 230 98 23 28 200 39 30 This was received as 0.25-in. plate, and, prior to the annealing studies, was cold-rolled to 0.040 in. Specimens 1 in. sq were chemically polished and annealed for various times at 800°C in a vacuum better than 5x 10-6 Torr. For metallographic examination specimens were first chemically polished and then anodized8 to enhance contrast between the grains when examined under polarized light. Changes in crystallographic orientation associated with the development of secondary grains were followed by (1011) and (0002) pole-figure determinations using a conventional Schulz goniometer in reflection. Filtered Cr Ka radiation was employed and great care was taken to avoid spurious re- sults due to the close proximity of the Bragg angles for the (1011) and (0002) reflections. Figs. 1 and 2 illustrate the change in grain structure on annealing at 800°C. After 24 hr the structure has ceased to be equiaxed due to the development of certain grains in preference to others. It is notable that the secondary grains do not grow to the extent observed in sponge zirconium.1,2 This appears to be due in part to the fact that normal grain growth is inhibited in the less pure sponge zirconium, with the result that the driving force for secondary recrystallization remains high, while at the same time the number of grains able to develop in the presence of the impurities is also smaller. As a consequence, in sponge zirconium those grains that do develop preferentially are able to grow into the fine -grained matrix without impingement, while in iodide zirconium the preferential growth of many grains leads to early impingement. The pole figures determined for specimens annealed for 5 min and 24 hr at 800°C are illustrated respectively in Figs. 3 and 4. These indicate that the dominant feature of the initial recrystallized texture consists of basal planes at an angle of 321/2 deg to the sheet surface, with a (1120) axis lying parallel to the

Jan 1, 1967

By W. D. Von Gonten, R. L. Whiting

Regression analysis was used to correlate the physical properties of 478 sandstone and 90 carbonate core samples. Porosity, permeability, electrical formation resistivity factor, capillary pressure and the sonic velocity of the shear and compressional waves were measured. Prediction equations for porosity, permeability and electrical formation resistivity factor were found which should be useful in understanding the relationships between the physical properties of porous media in formation evaluation. INTRODUCTION The physical properties of porous media are important to the petroleum engineer and geologist. To evaluate fully the potential and behavior of a subsurface formation such as a petroleum reservoir, certain physical properties of the porous medium must be known. The problem of accurately determining physical properties of subsurface formations has not been solved because many determinations must be made by indirect measurements and because of the difficulties caused by complex pore structure and presence of clays in most naturally occurring porous media. Due to the difficulty in measuring some of the physical properties of porous media, it would be advantageous to be able to predict a certain physical property of a rock from other physical properties of the rock which could be measured more easily and more accurately. Since most potential reservoir rocks are heterogeneous, relationships between the physical properties are very complex and thus far no satisfactory correlations based on theory or laboratory models have been developed. It appears that empirical relationships obtained by measuring the physical properties of a large number of samples of naturally occurring porous media and applying regression analysis to develop equations for one physical property in terms of other rock properties is the best approach. REVIEW LITERATURE The three physical properties used as dependent variables for correlating purposes were porosity, permeability and formation factor. Since formation factor is more difficult to determine, a brief review of the literature is provided on this property. The first work on determining formation factors was published by Archie1 in 1942. He defined this property of a porous medium as F - Ro/Rw......(1) where Ro is the resistivity of the porous medium when completely saturated with a brine of resistivity Rw. Archie found the best correlation between formation factor and porosity was the following equation, where is the porosity fraction and m is the constant characteristic of the rock. The value of m was 1.3 for unconsolidated sand packs, and ranged from 1.8 to 2.0 for consolidated sandstones. In 1950 Patnode and Wyllie2 and De Witte3 observed that the formation factor as determined by Eq. 1 was valid only when the porous medium contained no conductive solids such as clay or shale. When conductive solids are present the formation factor is also dependent on the resistivity of the saturating fluid. Therefore, in samples containing conductive solids the formation factor decreased as the resistivity of the saturating fluid increased. Because of this. the measured formation factor was called the apparent formation factor and was designated Fa. Patnode and Wyllie proposed the following equation,

By John P. Dolan, Charles A. Einarsen, GiIman A. Hill

his paper discusses how the following formation characteristics can be determined mathematically from drill-stem test pressure charts: true formation pressures, effective permeability of the entire section tested, well productivities, wellbore damage, and possible detection of barriers (faults, pinchouts, etc.). This paper also presents a practical method for im-mediate determination of eflective permeability and well-bore damage from successful double shut-in pressure tests. A list of recommendations for improving the reliability of drill-stem rest pressures is also presented. INTRODUCTION A drill-stem test is a temporary completion designed to sample the formation fluid and to establish the possibility of commercial production. Early pressure recording devices were used merely to verify proper operation of the testing tool. Until recently the accuracy of the pressure gauges has been insufficient for any reliable quantitative use of the recorded pressures. In view of the need for more reliable formation evaluation and as a result of the recent interest in exploration work employing the concept of hydrodynamic en-trapment,1,2,3,4 better pressure recording gauges are now in use. These devices can record pressure within 1 per cent above 1,000 psig and can detect differential pressures as low as 1/2 psig. In addition to formation pressure, several other reservoir characteristics can be determined from DST charts; namely, well productivity, formation permeability, wellbore damage, and the possible existence of bar- riers (faults, pinchouts, changes in permeability, etc.). This paper presents a practical method to interpret DST pressure charts for formation pressures and many other reservoir properties, a method that has been developed in analyzing approximately 4,000 DST charts during the last five years. The techniques used are a composite of published articles on drill-stem testing5,6, together with well-known pressure build-up analysis methods. THEORY It has been shown7,8 that the following equation may be used for analysis of pressure build-up curves: Po - Pw = 162.6 qu/kh log ( to + ?/?) .....(1) When this equation is applied to the curves obtained in drill-stem testing, the assumptions and boundary con-ditions are more nearly realized than in conventional flow and build-up tests on producing wells. Zak and Griffen9 have recently discussed in detail the use of this equation in analyzing DST charts. One of the problems with DST curves is the lack of reservoir data for precise analysis. Therefore, it is necessary to develop empirical rules and field methods for analyzing DST charts in quantity. For this reason, the empirical methods presented in this paper have been developed, and their derivation is found in Appendices A and B. METHOD USED FOR ACCURATE READING OF DRILL-STEM TEST CHARTS In order to apply the pressure build-up theory to DST charts, it is necessary to obtain a digitized expression for the pressure and time data recorded by the pressure gauge. These data may be either provided by the service company or interpolated by projecting a

Jan 1, 1958

By F. N. Rhines, W. S. Pellini

In many of the otherwise well established alloy phase diagrams the solidus curves (temperatures at which liquid first appears upon melting) have not been located accurately, chiefly because the experimental techniques that have been most popular for determining solidus temperatures have been both cumbersome and subject to large errors. C. E. Homer and H. Plummerl have described a sensitive and at the same time a very simple technique for locating the solidus curves in a number of alloys of tin. Their method consists simply in noting the temperature at which a specimen of the alloy ruptures under the influence of a light bending force. Although this method is not new, it has been little used for this purpose in the past; nevertheless, it appears so attractive in its possibilities of speed, simplicity, and precision that the investigations presently to be described were undertaken to verify its merits. The redetermination of the solidus and eutectic temperatures of the lead-antimony system was employed as a medium of experimentation. New values obtained in this way are believcd to be sufficiently precise to warrant a revision of the currently accepted lead-antimony phase diagram (Fig. I). Determinations of the solidus of the lead-rich lead-antimony alloy series have been published by X. S. Dean2 and by E. E. Schumacher and F. C. Nix. Their points are represented in Fig. I. In their work the solidus was not located at antimony collcentrations greater than 2 per cent; the curve was presumed to meet the eutectic horizontal at an antimony concentration of about 2.5 per cent. In the present studies the solidus has been traced to 3.5 per cent, where the eutectic horizontal is intersected (Table I and Fig. I). Within the range investigated by Dean and by Schumacher and Nix the agreement with their values is good. H. Seltz and B. De Witt,4 on the basis of activity measurements, have calculated that the intersection of the solidus and the eutectic reaction horizontal should lie at 3.86 per cent of antimony. The following determinations of the eutectic temperature have been reported: Roland-Gosselin,5 228°C.; Ewen,6 228OC.; J. E. Stead,7 24g°C.; Campbell,8 228°C.; W. Gontermann,9 245&apos; to 252°C.; R. Loebe,lo 245°C.; E. Heyn and 0. Bauer,ll 245°C.; H. Endo,12 250°C.; R. S. Dean,= 247&apos; to 258°C.; E. Abel, O. Redlich, and J. Adier,13 245°C.; W. Broniewski and L. Sliwowski,14 250&apos; to 252°C.; H. Seltz and B. De Witt,4 25o°C. A temperature of 247°C. appears to have been generally accepted in recent years; it is the value most frequently obtained by the method of cooling curves. Values below 247°C. have usually been obtained by inferior cooling-curve techniques; those above 250°C., by the method of heating

Jan 1, 1943

By W. S. Pellini, F. N. Rhines

In many of the otherwise well established alloy phase diagrams the solidus curves (temperatures at which liquid first appears upon melting) have not been located accurately, chiefly because the experimental techniques that have been most popular for determining solidus temperatures have been both cumbersome and subject to large errors. C. E. Homer and H. Plummerl have described a sensitive and at the same time a very simple technique for locating the solidus curves in a number of alloys of tin. Their method consists simply in noting the temperature at which a specimen of the alloy ruptures under the influence of a light bending force. Although this method is not new, it has been little used for this purpose in the past; nevertheless, it appears so attractive in its possibilities of speed, simplicity, and precision that the investigations presently to be described were undertaken to verify its merits. The redetermination of the solidus and eutectic temperatures of the lead-antimony system was employed as a medium of experimentation. New values obtained in this way are believcd to be sufficiently precise to warrant a revision of the currently accepted lead-antimony phase diagram (Fig. I). Determinations of the solidus of the lead-rich lead-antimony alloy series have been published by X. S. Dean2 and by E. E. Schumacher and F. C. Nix. Their points are represented in Fig. I. In their work the solidus was not located at antimony collcentrations greater than 2 per cent; the curve was presumed to meet the eutectic horizontal at an antimony concentration of about 2.5 per cent. In the present studies the solidus has been traced to 3.5 per cent, where the eutectic horizontal is intersected (Table I and Fig. I). Within the range investigated by Dean and by Schumacher and Nix the agreement with their values is good. H. Seltz and B. De Witt,4 on the basis of activity measurements, have calculated that the intersection of the solidus and the eutectic reaction horizontal should lie at 3.86 per cent of antimony. The following determinations of the eutectic temperature have been reported: Roland-Gosselin,5 228°C.; Ewen,6 228OC.; J. E. Stead,7 24g°C.; Campbell,8 228°C.; W. Gontermann,9 245&apos; to 252°C.; R. Loebe,lo 245°C.; E. Heyn and 0. Bauer,ll 245°C.; H. Endo,12 250°C.; R. S. Dean,= 247&apos; to 258°C.; E. Abel, O. Redlich, and J. Adier,13 245°C.; W. Broniewski and L. Sliwowski,14 250&apos; to 252°C.; H. Seltz and B. De Witt,4 25o°C. A temperature of 247°C. appears to have been generally accepted in recent years; it is the value most frequently obtained by the method of cooling curves. Values below 247°C. have usually been obtained by inferior cooling-curve techniques; those above 250°C., by the method of heating

Jan 1, 1943

By J. S. Bryner

INTRODUCTION IN the study of metallographic specimens in the electron microscope, there is need for a method of locating the same field in both the light microscope and the electron microscope. This need arises chiefly from the fact that in the electron microscope the magnification and degree of resolution are so much higher, and the field so much smaller than in the light microscope that it is often difficult, if not impossible, to identify positively what is being observed. The difficulty is increased by the fact that, because a transparent film replica of the metal surface must be used in the electron microscope, micro-constituents can be identified not by their color but only by their texture and contours. For these reasons it is desirable to obtain a series of photographs showing the same field in both microscopes in order that the appearance of common microstructures and micro-constituents in the electron microscope may be identified and catalogued for future reference. The need for a method of locating the same field in both microscopes arises also when it becomes desirable to enlarge in the electron microscope for more detailed study a particular interesting structure observed in the light microscope. Using the standard polystyrene-silica1,2 replica technique, in which the silica film replica is fished from the ethyl bromide on a 1/3 in. diam 200-mesh specimen screen, the possibilities of locating a particular area on the film in the electron microscope are rather remote. The desired structure may be obscured by the wires of the specimen screen or unrecognizable at the high magnification. A solution to the problem would be provided if a specially designed specimen screen, containing an opening which could be absolutely identified and quickly located in the electron microscope, could be fastened to the silica film replica in such a position that the desired field on the specimen would be located at the identifiable opening in the specimen screen. The design for such a specimen screen, a method for producing it, and a technique for fastening it to the silica film replica are described below. DESCRIPTION OF METHOD The Specimen Screen A simple design for a specimen screen containing an opening easy to identify and locate in the electron microscope is one with two lines of openings at right angles in the form of a cross. Such a screen is shown in Fig I. The opening at the center of the cross is identified easily and can be located quickly in the light microscope and in the objective image of the electron microscope. The specially designed specimen screens for this work were produced in quantity by electroforming. On both sides of a polished strip of copper 1 X 3 X 1/8 in., twenty patterns of the cross of openings were punched with a diamond point micro-hardness tester, using a load of magnitude

Jan 1, 1948