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By A. U. Seybolt, J. L. Walter

The effects of the addition of 0.5 pct ThO2 (by volume) on the grain structure and texture of heavily rolled tungsten sheet were studied. Powder metallurgy ingots were rolled to sheet, 0.001 in. thick, and samples were annealed at temperatures from 1200" to 2500°C. The heating rate to the anneal temperature was varied from 3°C per min to 6500°C per min. The orientations of the largest grains were determined by X-ray diffraction. The disposition and loss of the ThO2 particles were determined by electron transmission microscopy and the activation energy for remozlal of the thorium was measured by mass spec-troscopy. Heating rates below about 800 C per min produced large, highly elongated grains. Higher heating rates produced much smaller, less elongated grains. The grain structure and texture of the slowly heated samples were identical to the structures and textures of heavily rolled tungsten foil conventionally doped with aluminum, silicon, and potassium but the recrystallization temperature was about 200°C lower. There was stringer-like dispersion of larger ThO2, particles superimposed on a uniform dispersion of fine particles. The particles increased in size and decreased in number with time at temperature. The loss of particles was accompanied by formation of grain boundary voids and surface pits. The activation energy for removal of the ThO2 was about 40 kcal per mole. THE addition of small amounts of aluminum, silicon, and potassium to tungsten has a profound effect on the grain structure of heavily rolled sheet1 or drawn wire."4 Thus, "doped" tungsten sheet, rolled to 0.001 in. and recrystallized, develops a structure consisting of large, highly elongated grains of a specific preferred orientation.' It has been shown that the elongated grain structure was caused by a dispersion of particles, identified as mullite (Al6si2O13),1,4 in strings parallel to the rolling direction in sheet or to the wire axis. Identical results were obtained for iron which was doped with glass and rolled to 99 pct reduction of thickness and recrystallized.5 Again, the glass particles were disposed in strings parallel to the rolling direction. The strings retarded boundary migration in the lateral direction but grain growth was able to proceed relatively unhindered along the direction parallel to the strings.1,5 In both the doped tungsten and the glass-doped iron, the particles were highly plastic during the high-temperature deformation. Since mullite melts at about 1800°C and the glass employed melts at about 810ºC, the particles were probably molten during the recrystallization anneals (above 1800°C for the doped tungsten and 850°C for the glass-doped iron). There are indications in the literature that particles not plastic at hot-working temperatures (up to about 1550°C for tungsten) may also impart elongated grain structures by primary recrystallization of worked alloys. Examples are dispersions of tantalum carbide in chromium,6 and ThO2 in nickel where elongation ratios of recrystallization grains of up to 20:l were obtained.7 Strings of ThO2 particles in W-ThO2 wire have been seen by Rieck.8 In view of the available evidence, it was of interest to extend the previous studies of doped tungsten and glass-doped iron to include W-ThO2 sheet materials. Of specific interest was the grain structure, preferred orientation, recrystallization temperature, and disposition of the thoria particles. EXPERIMENTAL PROCEDURE A) Material Preparation. About 380 g of blue tungsten oxide (approximate composition WO3) was wet with a sufficient amount of aqueous solution of Th(N03)4 to provide 0.5 vol pct ThO2. The wet mixture was stirred to distribute the doping material uniformly throughout the powder. Stirring was continued while the mixture was heated until it was completely dry. The dried, doped mixture was then reduced to tungsten powder by heating at 850°C for 2 hr in a stream of dry hydrogen. The doped tungsten powder was hydropressed in a rubber sack at pressures of 50,000 psi to produce an ingot approximately 2 cm diam by about 5 cm long. Next, the pressed cylinder was heated in hydrogen for 2 hr at 1350°C to render it strong enough for machining. The cylinder was machined to a square cross section of 1.6 by 1.6 cm with rounded corners. Finally, the bar was heated for 2 hr at 2150°C in hydrogen to provide a sufficiently dense mate rial to withstand the hot-rolling operation. Prior to rolling, the ingot was reduced in thickness by about 20 pct by forging at 1550°C. This served to increase the density of the material and to widen it slightly for better rolling characteristics. The forged ingot was then rolled at 1550°C to a reduction of 45 pct of thickness, following which the rolling temperature was reduced to 1300°C and the slab rolled, with several reheats, to 0.050 in. Further reduction was accomplished at 800°C in tungsten sheet packs to a total reduction of about 99.85 pct. B) Annealing Treatment and Observation of Structure. Small samples of the rolled foil were annealed in one of two ways. Some of the samples were suspended in a covered tungsten can and annealed at temperatures from 1200" to 2200°C for various times in vacuum of l0-7 to 10-6 mm Hg. The can was heated by induction and temperatures were determined by optical pyrometry

Jan 1, 1970

By J. Van Steveninck, A. C. Pols, R. Feenstra

In the course of time, an increasing number of investigations on jet cutting all kinds of material, such as rock,1,2,3 metal,4,5 and wood6 have been reported to serve various applications. A number of papers have been published on these subject, 7,8,9 some of which refer to jets purposely containing abrasives, termed 'jetted particle drilling'.7 Since such abrasives complicate fluid handling considerably and do not appear to be absolutely necessary for making holes, only conventional drilling fluids have been considered. A large part of our investigation has been performed with the aid of three laboratory-type drilling machines, which permit tests on both micro-bits (1 ½ in. ) and full-scale bits (6 ½ -9 5/8 in. ) . In view of the application of jets in deep holes, care has been taken to simulate hydrostatic pressures as they exist in the field on the hole bottom. These have been found to have a major effect on the bit-penetration rate for various drilling fluids.

Jan 6, 1974

The annual report f the Secretary of the Navy for the fiscal year, ending June 30, 1917, but including operations and recommendations up to Dec. 1 of that year, contains the following remark about the activities of the Naval Consulting Board. The members of the Institute who are members f this Board are William L. Saunders, Benjamin B. Thayer, Thomas A. Edison, Thomas Robins, Lawrence Addicks, Joseph W. Richards, W. R. Whitney, assisted by 47 other members f the Institute, in the capacity of associate members of the Naval Consulting Board. During the year, the work of this board, organized and approved by Congress in 1915, has increased very materially in importance and volume, its meetings have been frequent and the work of its individual members has been such in some cases as to occupy almost their entire time in the service of the Government. Some time before the active entry of this country into war the board called a special meeting to which were invited some 50 of the leading scientists and industrial managers, whose special study fitted them to advise on the methods of meeting the

Jan 2, 1918

By Robert F. Mehl

Jan 1, 1944

By Robert F. Mehl

Jan 1, 1944

JOSEPH W. RICHARDS, Chairman. J. E. JOHNSON, JR., Vice-Chairman. ARTHUR S. CALLEN, Secretary, 453 Chestnut St., So. Bethlehem, Pa. SUB-COMMITTEES IRON ORE DWIGHT E. WOODBRIDGE, Chairman. ERNEST F. BURCHARD, WILLIAM KELLY, CHARLES F. RAND, FELIX A. VOGEL. BLAST FURNACES II. A. BRASSERT, Chairman. WILLIAM H. BLAUVELT, AMBROSE N. DIEHL, JAMES GAYLEY RICHARD V. McKAY. STEEL WORKS HENRY D. HIBBARD, Chairman. GUILLIAEM AERTSEN, C. F. W. RYS, .1. S. UNGER. FRANK D. CARNEY, A. A. STEVENSON, WILLIAM It. WALKER. MECHANICAL TREATMENT CHARLES A. BUCK, Chairman. ROBERT W. HUNT, GEORGE MESTA, FREDERICK W. WOOD.

Jan 6, 1915

By Cloyd M. Smith

A FEW years ago, the Ventilation Committee established the practice of presenting one topic each year for discussion at the annual meeting. The practice has met good response on the part of committee members and I suggest that it be continued. The topic chosen for this year, "Underground Anemometry," is a topic which has bothered me for more than 20 years. It seems to me that the coal industry is content to rely on slipshod methods for measuring the rate of flow of air underground, so I prefaced my discussional charge to committee members with the statement that I regard air measurements made in the usual way, with hand held anemometer, as no good. Agreements and disagreements came in from more than a dozen engineers, some of whom are with operating companies, coal and metal; some with manufacturers; others with government agencies.

Jan 1, 1949

By J. W. Powell, F. H. Spedding

A complete review of the use of chelating agents in the sepa ration of rare earths by ion-exchange is given as well as a concise description of the recent pilot-plant operations of the Ames Laboratory. The two chelating agents which show the greatest promise are ethylenediamine-N,N,N',N'-tetraacetic acid and N'-(2-hydroxyethyl)ethylenediarnine-N,N,N '-triacetic acid. The first successful separations of rare earths by ion exchange were reported in a collection of papers which appeared in the November, 1947, issue of the Journal of the American Chemical Society.1'9 Some of this work was performed at the Ames Laboratory of the A.E.C., the remainder at the Oak Ridge National Laboratory. The processes developed at Oak Ridge, as well as some of the early Arnes methods, employed 5 pct citric acid-ammonium citrate eluant at low pH and were carried out on either H+-state or NH:-state resin beds. These techniques were successful for the separation of small quantities of either naturally occurring or radioactive rare earths and are still used for the isolation of rare-earth activities from fission products. Concentrated citrate is not economical, however, for use in moderate or large-scale rare-earth separations. For this reason, the Ames Laboratory turned its attention to lower concentrations and higher pH's in order to make more effective use of the eluting agent.10-14 Although elutions have been performed successfully over a wide range of conditions, 0.1 pct citrate at a pH of 8.0 is highly recommended for use on H+-state resin beds.15,16 Elu-tion with 0.1 pct citrate in the pH range from 5 to 9 brings about the separation of the constituent rare earths into a series of flat-topped elution bands which progress down the resin bed, head to tail, without actually pulling apart as do the rare-earth peaks which develop when trace quantities are eluted with 0.25M (5 pct) citrate at low pH's. Because of this, elution with 0.1 pct citrate at pH 8.0 do not produce pure rare earths unless sufficient quantities are present to provide developed bands which are at least several inches long on the columns. Although other eluting agents have proved more effective than citrate solutions, articles concerning the use of citric acid for separating rare earths still appear in the literature occasionally. For example, Ketelle and Boyd17 reported some further studies on the separation of rare earths with 5 pct citrate in 1951. They used 270 to 325 mesh Dowex-50 columns at 100°C and a pH of 3.28. vickery18 compared the effectiveness of a number of eluants for the separation of rare earths on NH+4 state Dowex-50 in 1952. He found that citric acid was more efficient than acetic, malic, tartaric, and aminoacetic acids. In 1953, Mayer and Freiling18 reported that citrate was inferior to malate, glycolate, lactate, and EDTA for the resolution of Sm-Eu and Y-Tb mixtures on 250 to 500 mesh, NH+4-state, Dowex-50 at 87°C. pinta20 used 5 pct citrate in the pH range 2.8 to 3.4 to obtain some rare earths for analytical work the same year. Trombe and Loriers21 reported the use of citric acid in their laboratory to separate rare earths in kilogram quantities. Lariers and Quesney22 reported some separations with citrate in 1954. They used 5 pct citrate at pH 2.8 to separate yttrium and the yttrium-group rare earths from the cerium-group rare earths. briers23 used 5 pct citrate at pH 3.2 and 90°C as late as 1956 to isolate thulium in fair purity. For the separation of tracer quantities of rare earths, Mayer and Freiling19 have recommended pH 5.00, 0.24M lactate at 87 °C on 250 to 500 mesh, NH+4-form Dowex-50. Freiling and Bunney24 have also employed lactic acid for the separation of fission-product rare earths. Cunninghame, Size-land, Willis, Eakins, and Mercer25 have reported a 4-hr separation of Y, Eu, Sm, Pm, Nd, and Pr with 1M lactic acid at pH 3.25 on Zeokarb-225 at 87°C. Stewart, et al.,26 reported separation factors for rare earths distributing between Dowex-50 and 0.25M glycolic acid. stewart27 also reported a 30-61 separation of Y, Tm, Er, Tb, and Lu tracers with buffered, 0.25M glycolic acid containing 0.05 pct Aerosol OT. The resin bed was 400-mesh Dowex-50 (X12). The pH of the ammonia-buffered eluant was 3.5. Various aminopolyacetic acids have also been used to obtain varying degrees of separation of the rare earths. In 1951, Fitch and Russell28 investigated iminodiacetic acid (IDA) and nitrilotriacetic

Jan 1, 1960

For more than 100 years, the Republic of Chile has been one of the leading copper-producing countries of the world. Between 1877 and 1880 Chile accounted for over 50 pet of total world copper production. Today it has the world's largest known reserves of copper ore and a capability of producing over 600,000 tons per year. This capacity can and will be increased as the world demand for copper grows steadily during the remaining years of this century. The Potrerillos mine of Andes Copper Mining Co., a subsidiary of The Anaconda Co., was developed in the rugged, high Cordilleras in the early 1920's, and the townsite, concentrator, leaching plants, smelter, railroad, power and port facilities were completed so that it came into full production in 1927. Since then and until the closing o f the mine in June of last year, 1,762,192 tons o f copper were produced.

Jan 4, 1960

Jan 1, 1881

Jan 1, 1916

Jan 1, 1953

By R. L. Orr, O. D. Sherby, J. E. Dorn

Creep data for pure metals at temperatures above those at which rapid recovery occurs (above about 0.45 the melting temperature) are correlatable by means of the equations and These correlations were applied successfully to data for aluminum, iron, nickel, copper, zinc, platinum, gold, and lead as well as for simple alloys. For a given metal, AH is a constant about equal to the activation energy for self-diffusion. THE early recognition that creep is stimulated by thermal activation prompted numerous investigators', ' to apply the same laws that are valid for the viscous behavior of liquids to analyses of creep data. To a good first approximation these laws are summarized by the equation were i is the creep rate; T, the absolute temperature; R, the gas constant in cal per degree per mol; T, the applied stress; AH, the activation energy in cal per mol; S', a constant dependent on the entropy of activation, the frequency of activation, and the contribution of each activation to the strain; and B', a constant dependent upon the size of the flow unit that is activated. Although Eq. 1 describes the flow of viscous fluids very accurately, its application to the creep of solids has been disappointing. Two reasons for the failure of Eq. 1 for creep are now known: First, the decelerating creep rates during primary creep demand that the internal structures of the metals are changing and that these changes might be reflected by changes in one or more of the three creep parameters S', AH, and B'. Consequently when the conventional methods of evaluating these parameters are employed by comparing the secondary creep rates at a series of temperatures and at a series of stresses, the true effects of temperature and stress are masked because of simultaneous changes in one or more of the creep parameters. Second, as will be illustrated more fully later, three distinctly different types of investigations have shown that the stress term for high temperature creep enters the analysis as and not as t/T. This rather unexpected result points sharply to a significant fundamental difference between the mechanisms for the viscous behavior of fluids and the high temperature creep of metals. More recent extensive investigations",'4 on the creep of high purity aluminum and several of its dilute a solid solutions have shown that where E is the total creep strain; temperature compensated time = for a constant temperature test; t, is the initial stress in a constant load test or the constant true stress in a constant stress test;" and t is the duration of test. • Eq. 2 is valid for either constant stress or constant load tests; but the total creep curve is difierent (i.e. the function, f, is differentl for each test. The fundamental origin of the validity of Eq. 2 is thought to arise from some equivalence of substructures in constant load creep tests at equal values of 0 or E. Both X-ray and metallographic examination revealed that practically identical lattice distortions and subgrain sizes are obtained for the same creep strain under the same load over wide ranges of test temperature.' Furthermore the room temperature tensile properties following equal creep strains at different temperatures under constant loads were also identical, illustrating that identical substructures were indeed obtained.' " A second type of correlation was obtained by differentiating Eq. 2 with respect to time, giving For the secondary creep rate, denoted by i,, But Eq. 2 reveals that 0, is a function of a, alone because the secondary creep rate in a given constant load test is always reached at a fixed value E,". Therefore where is the function that was introduced a number of years ago by Zener and Hollomon." Eq. 4 is not only valid for creep but will permit correlations between constant load creep and tensile data where e, is the rate of tensile straining and (TC is the engineering ultimate tensile strength.

Jan 1, 1955

By William D. Manly, John Towers, Paul A. Beck

RECENT work on grain growth in high purity aluminum and in a solid solution type alloy of aluminum and magnesium' showed that the isothermal increase of the average grain diameter D with time follows the equation [D = K(to + A)-Eq I] Here [to] is that portion of the total annealing time [t], which is available for grain growth, i.e. the annealing time less the time necessary for complete recrystallization. The parameters A and n depend only on the temperature. A has the dimension of time, and is usually of the same order of magnitude as the time for recrystallization: R. In some instances R may be substituted for A in Eq I. This is the case for example at long periods of annealing or at high temperatures, where both A and R become small in comparison with t. In such instances Eq I is simplified to [D-K-tnEq2] For high purity aluminum the exponent n increases in the ratio of about 1 to 5 in the temperature range of 350° to 600°C. 70-30 brass has been long known to exhibit grain growth of the continuous type, such as occurs in pure metals. For this reason, it was of interest to determine whether grain growth in brass also follows Eq I and 2 as it does in aluminum. Isothermal grain growth data for 70-30 brass were published in recent years by R. S. French2 and by H. L. Walker3 Fig I shows a log D vs. log t plot of French's data, together with the 500, 600 and 100°C data by Walker for 42.8 pct reduction by rolling. In such a log D vs. log t plot Eq 2 corresponds to a straight line with a slope of n. As seen in Fig I, the data of French and the 600°C data of Walker can be represented by straight lines. However, the 500 and 700°C data of Walker give curved lines and the average slope of his 500°C line is very different from the slope of the line representing French's data for the same temperature. Furthermore the curvature of the 700°C line suggests a tendency for grain growth to stop after 8 hr. If confirmed, this would constitute a definite deviation from Eq 2, not explainable on the basis of the specimen thickness effect found in high purity aluminum.1 Walker's specimens were 0.125 in., i.e. 3.18 mm thick, while the deviation occurs at a grain size of approximately 0.4 mm. A further point of divergence arose recently, when J. E. Burke suggested4 on the basis of Walker's data, that, instead of Eq 2, grain growth in 70-30 brass follows the equation [D-D. =K• t,Eq3] Here D, is the grain size as recrystallized at the temperature in question. Although it was possible to show5 that, for pure aluminum, for which isothermal grain growth has been carefully investigated, Eq 3 is incompatible with the experimental facts, the situation remained somewhat obscure with respect to 70-30 brass. In view of the discrepancies between the

Jan 1, 1948

By Richard A. Sheppard

Zeolites-crystalline hydrated aluminosilicates of the alkalis and alkaline earths-are important rock-forming constituents in sedimentary rocks and are potentially valuable industrial minerals. They have a framework structure that encloses interconnected cavities occupied by the relatively large cations and water molecules. The cations, chiefly sodium, potassium, and calcium, and the water have considerable freedom of movement within the structure and give the zeolite their cation- exchange and reversible-dehydration properties. Some zeolites have essential contents of barium, strontium, or magnesium. The basic structure

Jan 1, 1975

Map

Jan 1, 1938

By Arthur L. Crawford

PLAGER gold is perhaps the most difficult of the common mineral deposits to evaluate. Not only are the erratic pay streaks a source of never-ending uncertainty, but the spotty distribution of the gold in iso¬lated nuggets is a perpetual source of error and disappointment to the sampler. Experienced engineers have long realized this difficulty and have been wary in predicting assay values except in the most general terms, and then only after extensive and usually expensive sampling. During the past year I have had the opportunity of checking a number of gold placers, and from the results obtained I believe that the microscope may be employed to advantage in placer sampling.

Jan 1, 1933

By Ali M. Heidarieh Zadeh, Raghu N. Singh

The paper presents a stability investigation of shaft intersections and pit bottom roadways in the vicinity of upcast and downcast shafts at a colliery in the U.K. Aschemeof instrumentation was aimed at monitoring the strata displacement surrounding the pit bottom roadways and shaft intersections with a view to ascertaining the origin of the strata movement and effectiveness of the control measures. The bore- hole instrumentation results together with a theoretical analysis suggested that the cause of instability could be attributed to the drivage of a roadway within the shaft pillar. A semi-empirical technique was used to calculate the amount of support resistance required to reinforce the pillar to take additional abutment load. A rock bolting system was designed to provide a required increase in thrust capacity of the roadway support. The results indicated that roadway closure was effectively controlled after installation of bolts indicating efficacy of the control measures adopted.

Jan 1, 1982

By S. E. Maddigan

MANY experimental and theoretical investigations have been made on the processes involved in annealing and recrystallization of metals. Most of these, however, have treated the time element as constant and heat-treatments used have been for relatively short times. Aside from the early work by Carpenter and Elam,1 the few that have investigated the effect of time on the processes have usually done so for fairly short time periods. During recent years the growing interest in long-time creep properties of metals and alloys under stress has made increasingly important a better knowledge of the recrystallization during prolonged heating. The recrystallization temperature of 70-30 brass given by Clark and White2 in 1932 was somewhat above 400°F. (204°C.) but under 500° (260°C.), whereas in our laboratory recrystallization has been observed in creep specimens at 204°C, the lowest temperature of Clark and White's range. Since the creep properties are quite different above and below the recrystallization temperature, erroneous conclusions can readily be drawn by the application of short-time recrystallization data to creep problems. It was thus considered of both practical and theoretical value to make long-time annealing studies near the minimum recrystallization temperature. In this way useful additions could be made to data on recrystallization temperatures and, since the reactions in this range are relatively slow, additional insight could be obtained into the factors involved in annealing. Several comprehensive reviews of recrystallization processes have been written,3-5 therefore only a brief review of the generally accepted facts will be given here.

Jan 1, 1940