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PROF RICHARD ÅKERMAN Stockholm, Sweden DR. FRANK DAWSON ADAMS Montreal, Canada PROF RICHARD BECK Friberg, Germany ANDREW CARNEGIR New York, N.Y. DR. JAMES DOUGLAS New York, N.Y. PROF HATON DE LA GOUPILLIERE Paris, France SIR ROBERT A. HADFEILD London, England PROF HANS HOFFER Leoben, Austria PROF HENRI LOUIS LE CHATELIER Paris France EZEQUIEL ORDONEZ Mexico City, Mexico ALEXANDRE POURCEL Paris, France DR. ROSSITTER W. RAYMOND New York, N.Y. DR. ING H. C. EMIL SCHROEDTER Dusseldorf, Germany JOHN E. STEAD Middlesborugh, England JAMES M. SWANK (Associate) Philadelphia, Pa. PROF DIMITRY CONSTANTIN TSCHERNOFF St Petersburg, Russia PROF TSUNASHIRO WADA Tokyo, Japan CHARLES D WALCOT Washingtion D.C.

Jan 1, 1917

YEAR OF ELECTION 1913. FRANK DAWSON ADAMS Montreal, Canada. 1921. WILLIAM CUTHBERT BLACKETT Sacriston, Durham, England. 1923. GELASIO CAETANI Rome, Italy. 1929. TAKUMA DAN Tokyo, Japan. 1920. HENRY STURGIS DRINKER Merion Station, Pa. 1922. FEDERICO GIOLITTI Torino, Italy. 1906. SIR ROBERT A. HADFIELD London, England. 1928. JOHN HAYS HAMMOND New York, N. Y. 1921. FRANK WILLIAM HARBORD London, England. 1917. HERBERT HOOVER Washington, D. C.. 1905. HENRI LECHATELIER Paris, France. 1900. WALDEMAR LINDGREN Cambridge, Mass. 1879. JOHN MARKLE New York, N. Y. 1921. C. MCDERMID London, England. 1913. EZEQUIEL ORDONEZ Mexico City, Mexico. 1909. ALEXANDRE POURCEL Paris, France. 1911. ROBERT H. RICHARDS Cambridge, Mass.

Jan 1, 1923

CONTENTS PAGE Bronze Bearing Metals. By G. H. CLAMER 1729 Pennsylvania Railroad Anti-friction and Bell Metals. By F. M. WARING . . 1733 The Tin-plate Industry. By D. M. BUCK. Discussed by G. H. CLAMER, J. W. RICHARDS 1735 The Aluminum Bronze Industry. By W. M. CORSE 1738 Bronzes, Bearing Metals, and Solders. By G. K. BURGESS and R. W. WOODWARD. Discussed by G. H. CLAMER, R. T. ROBERTS 1742 Babbitts and Solder. By G. W. THOMPSON 1751 The Cadmium Supply Of the United States. By C. E. SIEBENTHAL. Discussed by M. L. LISSBERGER, C. W. HILL, F.- F. COLCORD . . .. . . . . 1752 Solder, Its Use and Abuse. By M. L. LISSBERGER 1759

Jan 12, 1918

PROF RICHARD ÅKERMAN Stockholm, Sweden PROF RICHARD BECK Friberg, Germany ANDREW CARNEGIR New York, N.Y. DR. JAMES DOUGLAS New York, N.Y. PROF HATON DE LA GOUPILLIERE Paris, France SIR ROBERT A. HADFEILD London, England PROF HANS HOFFER Leoben, Austria PROF HENRI LOUIS LE CHATELIER Paris France M FLORIS OSMOND Paris, France ALEXANDRE POURCEL Paris, France DR. ROSSITER W. RAYMOND New York, N.Y. PROF ROBERT W. RICHARDS Boston Mass. DR. ING H. C. EMIL SCHROEDTER Dusseldorf, Germany JOHN E. STEAD Middlesborugh, England JAMES M. SWANK (Associate) Philadelphia, Pa. PROF DIMITRY CONSTANTIN TSCHERNOFF St Petersburg, Russia PROF TSUNASHIRO WADA Tokyo, Japan CHARLES D WALCOT Washingtion D.C.

Jan 1, 1917

I do not think too much emphasis can be placed upon creation of favorable climate for development of foreign mineral resources to feed the hungry maw of our industrialized nation. We have become dependent, not only upon the ten raw products indicated in Mr. Bancroft's article, but upon 71 mineral substances listed by DMPA as in short supply. Forty-four of these are metals, 9 are chemical minerals and 18 are nonmetallic minerals. Of this list only 8 are produced in any large quantity in the United States, and all are vital in peace-time industry. Even more, they are absolutely essential for defense. This represents our present needs. But if our consumption and requirements are projected over the next 25 years as is done by the President's Materials Policy Commission-The Paley Report-our future outlook becomes appalling. The divergence of consumption over production, even allowing for substitution and conservation, will widen in the future. This means our dependence upon foreign raw materials, mainly minerals, will grow. What are the chief foreign sources of minerals for our future needs? They are chiefly Latin America and the dominions and colonies of the Western European nations. The British Commonwealth countries contain in abundance those minerals which the U. S. lacks. Of 32 of the most critical minerals the Commonwealth is deficient in 7 and lacks only 1; whereas the U. S. is deficient in 18. Strikingly, our deficient minerals are abundant in the Commonwealth and several of their deficiencies are in excess in the U. S. Resources of the two nations complement each other. If Europe should be overrun by an unfriendly power that could control the destinies and resources of the European dominions and colonies, our industrial life would be placed in severe jeopardy. Therefore, I heartily endorse Mr. Bancroft's statements regarding the Point IV program, provided the program is wisely administered and implemented. It is from the underdeveloped countries, as pointed out by Mr. Bancroft, that most of our future mineral supplies will have to come. Many of the underdeveloped source countries are African colonies and dominions of Western European nations. Our present aid to Europe, therefore, is not, as many infer, a purely one-sided affair; it safeguards our future industrial development and security. Development aid directly to the underdeveloped countries through a well administered Point IV program, can do much, I believe, to safeguard our prosperity. I regard it as a wise investment for future U. S. mineral needs. Dr. Alan M. Bateman Department of Geological Sciences Yale University Mr. Howland Bancroft's article, The Broadening Road to Foreign Investment, appeared on page 666 of the July MINING ENGINEERING.

Jan 1, 1952

SAMUEL T. HOYT,? Minneapolis, Minn. (written discussion||).-The subject of grain inheritance in iron and steel is apparently one which can he considered from the point of view of the two laws governing the rate of formation of crystal nuclei and the linear velocity of crystallization, which have been investigated by Tammann and collaborators, and of the additional law of coalescence. According to the work of Tammann, both the nuclei number, which is taken to be the number of crystal nuclei to form per unit volume per unit time, and the linear velocity of crystalli-

Jan 5, 1918

By McHenry Mosier

MeRcuRy is one of the strategic metals of which the supply has been raised from critical uncertainty to more than enough for essential demands. Work by the Bureau of Mines has contributed substantially to increased production of mercury in the United States and to consequent accumulation of Government stocks. Other contributing factors have been higher prices for mercury and Government loans to operators. The Bureau has undertaken 13 exploration projects, 10 of which have been completed. This work has comprised 28,376 ft. of several types of drilling and 23,798 lin. ft. of surface trenching, and has indicated commercial ore containing 34,800 flasks of mercury and marginal ore containing 26,200 flasks, a total of 61,000 flasks; equivalent, respectively, to domestic production for 8 months, 6 months, and 14 months. As Government stocks are now adequate, domestic production (currently at the rate of 50,000 flasks per year) is gradually being curtailed through Government control of labor and operating supplies. Introduction Mercury was one of the seven metals designated as strategic by the Army and Navy Munitions Board in 1939, when Congress appropriated funds for the investigation of domestic sources of supply of war minerals. The Bureau of Mines immediately started a limited search for strategic minerals, but the first mercury project was not begun until December 1940. The U. S. Geological Survey assisted in the search for cinnabar by contributing information on domestic mercury deposits, preparing maps, and making geological studies of exploration projects. The present high rate of production of mercury in the United States was encouraged by the increase in price to $196 per flask at New York (Fig. I) and Government loans to operators for mine development and plant construction. The Bureau of Mines has issued, for restricted distribution subject to wartime controls, 13 War Minerals Reports on individual mercury deposits (listed in appendix A). In March 1942 it also published a Progress Report of the Metallurgical Division, R. I. 3627, Cinnabar-reduction Plants of the Southwestern Arkansas Quicksilver District. Uses of Mercury Mercury and its compounds have more than 3000 uses. Its principal use is as a catalyst in the manufacture of gases for chemical warfare; the next largest is in pharmaceuticals. Mercury is essential also for: (I) certain electrical apparatus, (2) industrial control instruments at many war plants, (3) munitions, including blasting caps, (4) insecticides in agriculture, (5) antifouling paint for ship bottoms, (6) dental preparations, (7) general laboratory use, and (8) amalgamation of free-milling gold ores.

Jan 1, 1949

By McHenry Mosier

MeRcuRy is one of the strategic metals of which the supply has been raised from critical uncertainty to more than enough for essential demands. Work by the Bureau of Mines has contributed substantially to increased production of mercury in the United States and to consequent accumulation of Government stocks. Other contributing factors have been higher prices for mercury and Government loans to operators. The Bureau has undertaken 13 exploration projects, 10 of which have been completed. This work has comprised 28,376 ft. of several types of drilling and 23,798 lin. ft. of surface trenching, and has indicated commercial ore containing 34,800 flasks of mercury and marginal ore containing 26,200 flasks, a total of 61,000 flasks; equivalent, respectively, to domestic production for 8 months, 6 months, and 14 months. As Government stocks are now adequate, domestic production (currently at the rate of 50,000 flasks per year) is gradually being curtailed through Government control of labor and operating supplies. Introduction Mercury was one of the seven metals designated as strategic by the Army and Navy Munitions Board in 1939, when Congress appropriated funds for the investigation of domestic sources of supply of war minerals. The Bureau of Mines immediately started a limited search for strategic minerals, but the first mercury project was not begun until December 1940. The U. S. Geological Survey assisted in the search for cinnabar by contributing information on domestic mercury deposits, preparing maps, and making geological studies of exploration projects. The present high rate of production of mercury in the United States was encouraged by the increase in price to $196 per flask at New York (Fig. I) and Government loans to operators for mine development and plant construction. The Bureau of Mines has issued, for restricted distribution subject to wartime controls, 13 War Minerals Reports on individual mercury deposits (listed in appendix A). In March 1942 it also published a Progress Report of the Metallurgical Division, R. I. 3627, Cinnabar-reduction Plants of the Southwestern Arkansas Quicksilver District. Uses of Mercury Mercury and its compounds have more than 3000 uses. Its principal use is as a catalyst in the manufacture of gases for chemical warfare; the next largest is in pharmaceuticals. Mercury is essential also for: (I) certain electrical apparatus, (2) industrial control instruments at many war plants, (3) munitions, including blasting caps, (4) insecticides in agriculture, (5) antifouling paint for ship bottoms, (6) dental preparations, (7) general laboratory use, and (8) amalgamation of free-milling gold ores.

Jan 1, 1949

By H. Papazian, Robert A. Lad

SINCE it can be shown both theoretically'' : and experimentally that disordered Cu3Au has a greater internal energy than the ordered alloy, it might be expected that its chemical reactivity would be greater. Experiments were initiated' to test this hypothesis. This note will describe some recent results obtained in the study of the rates of corrosion of ordered and disordered polycrystalline Cu3Au by aqueous FeCl., The work of Robertson' has indicated that the attack by such solutions is intergran-ular and highly orientation dependent. It was of interest to see whether the order-disorder effect was great enough to overcome the variations from specimen to specimen which would arise from this type of attack. The polycrystalline alloy specimens (0.020 in. wire, 1¾ in. long) were preannealed in ½ atm H, at 700°C for 2 hr. The subsequent heat treatments to produce order and disorder were performed in M atm He. Disordered specimens were obtained by heating at 450°C for 2 hr and quenching in water. Ordered specimens were produced by heating for 2 hr at 450°, furnace cooling to 380°, and soaking at 380°C for 80 to 90 hr. Room temperature was reached by cooling to 150" at a rate never exceeding 7" per hr, and water quenching from 150°C. The specimens so produced exhibited electrical resistivities characteristic of the two states; of the order of 11.27x10 ohm-cm for the disordered, and 4.28x10 ohm-cm for the ordered specimens. The corrosion rates were studied at 30°C in ferric chloride solutions of several concentrations (?,¼, 1.5, and 1 molar). The specimens were attached to a stirrer during the tests. Tests were interrupted at intervals, and the specimen weight change was determined after washing and drying. Analysis of the solutions showed that the attack was limited to the copper. The higher corrosion rate for the disordered alloy, as illustrated in Fig. l, is typical of the results obtained. The effect of variation in ferric chloride concentrations is indicated in Table I for typical specimens. The variations in the ratio of reactivity for disordered and ordered specimens at the different concentrations are within experimental error, and the best value is estimated to be near 1.4. The experimental variation was due in part to the mode of attack, as mentioned, and in part to the fact that films were formed on the specimens under some conditions. Electron diffraction patterns of the films were very complex and indicated the presence of metallic iron, as did chemical analysis. In an attempt to eliminate the difficulties arising from the mechanism of attack, single crystal specimens were used. A greater reaction rate was again measured for the disordered specimens, but the reproduci-bility was no better than that for the polycrystalline metal. This would indicate that film formation was primarily responsible. It was concluded that the reaction with aqueous ferric chloride served to demonstrate that the reactivity of disordered Cu3Au is greater than that of the ordered alloy. However, the difficulties with film formation did not permit determinations of a precision great enough to warrant extension of the study to partially ordered alloy systems.

Jan 1, 1957

By Joseph W. Leonard

Evidence is presented to show that certain coals can be super-cleaned, using present coal preparation processes, to reduce sulfur below levels that are commonly believed to be possible. The evidence points to the need to develop continuous sorting methods by which coal coming from a mine can be segregated so that different raw coal types can be processed separately to produce a super-clean coal in addition to coals cleaned to more common levels of sulfur. Evidence is presented and techniques discussed that may be applicable for making the method feasible.

Jan 1, 1976

By M. L. Hammond, G. M. Bowers

Silicon dioxide films have been prepared on silicon wafers by the oxidation of SiH, near 400°C. Results previously reported by Goldsmith and Kern7 have been qualitatively corrobovated using a system of different geometry, and significantly greater deposition rates have been achieved. The deposition rate is independent of thickness and nearly independent of the O2/SiH, ratio over a wide range; however, the rate is strongly temperature-dependent. The structure of the deposit depends upon the cleanliness of the substrate, and the electrical field strength of the deposited oxide depends upon the nature of the electrodes. MULTILEVEL interconnects in integrated circuits using aluminum metallization require an insulator that can be deposited at low temperature. Because the A1-Si eutectic is only 577°C, the maximum deposition temperature must be below about 500°C to prevent reaction of the aluminum with the silicon and with other materials in the integrated circuit. Many methods of depositing insulating films of SiO, and other dielectrics have been reported'-6 but the technique described by Goldsmith and Kern7 offers the simplest method of preparing SiO, films. The technique involves the reaction of SiH, and 0, to form SiO, films in the 300" to 500°C temperature range. Previous work using this gas system has been reported8 and the initial development work at Philco Microelectronics was done at the East Coast R&D Laboratories. 9 This paper corroborates some of the results of Goldsmith and Kern,7 shows that much higher deposition rates can be obtained than previously reported, and presents some observations on the structure of deposited SiO, films. EXPERIMENTAL CONDITIONS Fig. 1 is a schematic drawing of the apparatus used in this study. It differs from that of Goldsmith and Kern in that 1) the gases are mixed before they enter the reaction chamber, 2) there is no fritted glass diffuser, and 3) the wafers are stationary during deposition. The control thermocouple was in a well located 0.06-in. from the substrate, and three gas supplies were used: 1 pct SiH4 in N 2, O 2, and N 2. Water vapor must be excluded from the plumbing to prevent the formation of colloidal SiO, and the SiH4 must be diluted with an inert gas because SiH4-0, mixtures are extremely flammable above about 4 pct SiH The wafer temperature was determined by attaching a thermocouple to a test wafer and the temperature was maintained to +5 C. The conditions used in this investigation are listed in Table I. The temperature range was chosen for compatibility with the A1-Si system. The volume ratio of 0, to SiH4 is the actual volume of 0, delivered to that of SiH4, taking into account the initial dilution of the SiH4. This ratio, which was used by Goldsmith and Kern,7 is a useful indicator of the experimental conditions. The active/inactive ratio is the ratio of the volume of active gases, SiH4 and O2, delivered to the volume of dilution gas. The active/inactive ratio is an important parameter to specify for deposition rate determinations since it determines the amounts of reactants that arrive at the sample per unit time. Fairly high dilution ratios were necessary to achieve uniform deposits of SiO,. Most of the process characterizations were performed on the polished (111) face of 3 to 5 ohm-cm, n-type silicon wafers which were 0.009 in. thick; but the data approximately apply to deposition of SiO, on thin films of aluminum. It is difficult to obtain accurate deposition rate data over aluminum films because of coarsening the aluminum surface during exposure to 300" to 400°C. The deposited SiO, film fol-

Jan 1, 1969

By Per Kofstad, Hallstein Kjöllesdal

The oxidation behavior of niobium (columbium) has been studied in the temperature range 500° to 1200°C and at oxygen pressures of 760,100, 10, 1, and 0.1 mm of Hg. The work comprises kinetic studies of the oxidation as well as structural investigations of the oxidized specimens by means of X-ray diffraction, electron diffraclion, electron microscopy, and metal1ographic techniques. The oxidation reaction has a highly irregular temperature dependence and is unusually sensitive to changes in the oxygen pressure. The complex oxidation behavior is suggested to be due to formation of different Nb2O5 modifications in different temperature regions. During oxidation oxygen is also dissolved in the metal. Formation of oxide whiskers take place on the oxide surface at temperatures above approximately 800°C. VARIOUS aspects of the oxidation of niobium have been studied.l-12 The investigations show that niobium has a complex oxidation behavior, and the oxidation

Jan 1, 1962

By P. R. Sperry

In an investigation of the decomposition of the solid solution in a cold worked high-purity aluminum alloy containing 7 pct Mg, aged at temperatures from 30o to 82°C, the nucleating sites at the earliest stages of precipitation were observed to be of two types. Nucleation occurred at the high angle grain boundaries both when the alloy was initially cold worked and when solution annealed. Nucleation also occurred at certain unique deformation markings which began to appear in abundance at approximately 30 pct reduction in thickness by cold rolling. These deformation markings were identified as deformation (kink) bands rather than as the usually assumed "slip planes." Zn material that was cold rolled 15 pct, only the grain boundary Fig. 2—A1-7 pct Mg alloy, cold worked 60 pct and heated at 230° C for 5 min. Etched with Perryman's reagent. X500. Reduced approximately 25 pct for reproduction. (a) Bright field illumination, precipitate deeply pitted. (b) Phase contrast, showing slip markings.

Jan 1, 1962

By Earl Greiner

THE constitution of the iron-silicon alloys containing from 14 to 33.4 weight per cent silicon has been studied by a number of investigators, whose results have been reviewed in a monograph published by the Engineering Foundation1. In these previous researches, the solubility of silicon in iron was determined by thermal, microscopic or magnetic methods and the compound Fe3Si2 was reported to be stable at tempera-tures from 0 to approximately 1030° C. This paper describes the results of an X-ray investigation of the solubility of silicon in iron and gives data which prove that the Fe3Si2 phase is unstable below 825° C. In order to obtain the present results on the solubility of silicon in iron, the authors have utilized the lattice constants of the alpha-phase iron-silicon alloys given in a previous publication2, and also some addi-tional data which will subsequently be described.

Jan 1, 1936

By Henry Fay

LAWRENCE ADDICKS, New York, N. Y., (communication to the Secretary *).-There are two points regarding gun erosion on which I want to say a few words: The first is about the analogy to hardening of wire by drawing and the second the possible role played by thermal conductivity of the metal. The ductile metals do not necessarily become brittle when cold-worked as it is possible to draw copper from 3. in. in diameter soft rod down to the finest hair wire without annealing. This results, as stated in the paper, informing a hardened core with a very hard skin. The electrical conductivity is depressed some 3 per cent. and the tensile strength nearly tripled. A soft copper wire 0.08 in. in diameter and 6 in. long may be twisted 150 or more turns before the wire will snap under torsion. A hard-drawn wire will break after perhaps a dozen twists, the skin breaking down at one spot. Just wiping the wire with a cloth clamp with dilute nitric acid has a remarkable effect in increasing the number of twists without appreciably lowering the tensile strength, showing the skin to be very thin. On the other hand, pickling the rod, from which the wire is to be drawn, in dilute nitric acid also greatly increases the number of twists which can be applied to the resulting wire. This indicates that the copper oxide scale produced when the wire bar is rolled hot is more or less rolled into the rod and may have much to do with the skin effect. We also know that if the conditions of drawing are not correct, the heat of deformation in the die may produce quite an annealing effect. The application of this analogy to what occurs in a gun to produce the effects noted offers some difficulty. The second point is that as the temperature of the surface of the gun bore has undoubtedly a great deal to do with the amount of erosion, one natural remedy would be to conduct the heat away fast enough to keep this temperature within desired limits. This brings up the question of the thermal conductivity of the metal of which the gun is made. We know that the conductivity of pure metals is greatly altered by alloying and that the alloy is usually, though not always, lower in conductivity than the metal before alloying. This is interesting when it is considered that the high-nickel and manganese-steel alloys show greater erosion as stated. Would it not be instructive to study the question from the point of view of heat conducted away from the eroded surface?

Jan 3, 1917

By C. J. McHargue, J. C. Ogle

Lightly deformed columbiun single crystals which contained only parallel hoins or purullel and intersecting trains were annealed at 1000' and 1600"C. No re-crystallizntion occurred in specimens hawing only parallel twins. Only noncoherent twin boundaries nzipated at 1000°C but both coherent and noncoherent ones moved al 1600°C. Recrystallization occurred within a few minutes at twin intersections at 1000°C. The orientation 01 the recrystallized grains differed front that of both the matrix and deformation twins, but could he derired by (110) and/or(112) rotations. ALTHOUGH twinning in metals has been extensively studied, there have been no definitive studies of the annealing behavior of crystals containing deformation twins. Some effects observed after annealing deformation twins have been summarized by Cahn1 and Hall2. Any or all of these phenomena are observed: 1) The twins may contract so that the sharp edges of the lens become blunted, and eventually the twin may disappear entirely. 2) The twins may balloon out at an edge, giving rise to a large grain having the same orientation as the twin. 3) The specimen may recrystallize; i.e., new grains are nucleated and grow at the expense of the twins and the crystal immediately adjoining the twin. Such grains have orientations which are not present before. Contraction has been observed in iron,3 titanium,3, 4 beryllium,5 zinc,8, 7 Fe-A1 alloy,' and uranium.9 Long anneals at high temperatures are required to have any appreciable effect in these metals and only thin twins are absorbed. Lens-shaped twins are absorbed from the edges: the thin, almost parallel-sided twins are usually punctured in several places and each piece contracts independently. Absorption is very gradual and no sudden cooperative jumps have been observed. The expansion of a twin into a larger grain of identical orientation is unusual, but such growth has been observed in iron,"'" zinc,6 and uranium." Crystals which have been deformed simultaneously by slip and twinning recrystallize first in the area adjacent to the twin. New grains appear faster where the twins intersect: but isolated twins, especially if thick, can also give rise to new grains. This type of recrystallization occurs in zinc.6, 7, 12, 13 and beryllium.14 Reed-Hill noted, in a single crystal of magnesium, the nucleation of a recrystallized grain at a twin intersection which had the same orientation as the second-order twin and which grew into the highly strained matrix.15 Short-time annealing has been reported to cause no change in the deformation twins in vanadium,16 columbium, 17, 18 tantalum,19 tungsten,'' and zinc.7 The purpose of this investigation was to note the effects of annealing on the coherent and noncoherent boundaries of deformation twins in columbium and to locate the nucleating sites for recrystallization. The orientation relationships, which the new recrystallized grains have with the parent crystal and the deformation twins, were also determined. EXPERIMENTAL PROCEDURE Single crystals of columbium were obtained by cutting large grains from electron-beam-melted buttons which contained 10 to 50 ppm C, 10 to 100 ppm O,, 1 to 10 ppm H2, and 10 to 15 ppm N2. The crystals were hand-ground and chemically polished until all grain boundaries were removed. The specimens were mounted in an epoxy resin and a face of each crystal was mechanically polished on a Syntron polisher using Linde A and then Linde B polishing compounds. After all faces were mechanically polished, the crystal was electrolytically polished to remove all distortion due to cutting and grinding. Laue photographs were taken of all faces of the crystals to determine the quality and orientation of each crystal. The crystals were compressed about 10 pct at -196 C in a specially constructed compression cage with an Instron tensile machine. Each crystal was separated from the top and bottom anvils by teflon films which acted as a lubricant. With the specimen crystal in position, the entire cage was cooled to -196°C by being submerged in a Dewar containing liquid nitrogen. The crystals were compressed at a rate of 0.02 in. per min and the load was recorded on a strip-chart recorder. After deformation the crystals were mechanically polished on 600-grit paper and Pellon cloth with Linde A and Linde B polishing compounds. The crystal faces were chemically polished and then etched. The twin planes were identified metallographically from an analysis of the twin traces on two surfaces. Annealing was carried out by placing each crystal in a columbium bucket made from the same electron-beam-melted material as the crystal itself and suspending the bucket by a tantalum wire in a quartz tube. After a vacuum of 10-7 Torr was attained, a furnace at 1000" or 1600 C was raised into position and the crystals held for various lengths of time. The crystals were repolished and etched after annealing to remove any surface contamination. Approximately 0.010 in. was removed during this process. The resulting surface was examined metallographically for microstructural changes due to annealing. A microbeam Laue camera mounted on a Hilger Micro-focus X-ray unit was used to determine the Orientstions of the recrystallized grains. This X-ray micro-beam camera had a 0.002-in.-diam collimator and incorporated the ideas of both and and chisWik21 and Cahn.22

Jan 1, 1967

By Molly Gleiser, John Chipman

The standard free energy of formation of WC was obtained from determination of the equilibrium WC + CO2 = W + 2CO between 1215° and 1266°K. Its uallie is -8340 * 300 cal Per mole over the above range of temperature. AS a part of a program devoted to measuring the stabilities of the carbides, a study was made of the free energy of formation of tungsten carbide, WC. The homogeneity range of this compound is very small,' and it is generally accepted and is dealt with here as a stoichiometric compound. The heat of formation, ?H°f, of WC has been accurately measured by Huff, Squitieri, and snyder.2 The only attempt, however, to measure the free energy of formation of this compound was made by Schenck, Kurzen, and wesselkock3 who brought tungsten carbides into equilibrium with H2 and CH4. Unfortunately their results are not sufficiently accurate nor consistent enough to permit the calculation of free energies. METHOD Heating mixtures of tungsten and carbon powders in hydrogen for 4 days at 1050°C led to formation of some WC without any trace of W2C. It was deduced, therefore, that at least below this temperature W2C will not be formed during experiments with mixtures of tungsten and WC. This was subsequently shown to be correct. The method chosen was the measurement of the equilibrium of the reaction

Jan 1, 1962

By D. F. Toner, P. E. Gage, D. J. Mack

MUCH work has been done on the decomposition of the p phase at the eutectoid composition, 11.9 pct Al, in the Cu-A1 system by Smith and Lind-lief,' Mack,' Klier and Grymko,3 Haynes,4 and others. In all of the mechanisms proposed by these workers for the decomposition of the ß phase, it was stated that the a phase must precipitate rich in aluminum with respect to the equilibrium composition of 9.4 pct A1 at 565°C. To check this hypothesis, it was necessary to have a master curve relating equilibrium aluminum content of a to lattice parameters of a. A number '' binary Cu-Al alloys of increasing amounts of aluminum were prepared by Ampco Metal Inc. These alloys, received as-cast, were given a 30 pct reduction of area by hot-working and then annealed at 900°C for homogenization and slowly cooled in the

Jan 1, 1956

By P. R. Sahm, T. V. Pruss

Mixtures of fine GaSb and Gds as well as preal-loyed GaSbl,As, powders were hot-pressed at 690°C and 25,000 psi. Dense alloys with compositional gradients of less than 5 pct were obtained from mixtures containing about 20 mol pct GaAs. For x < 0.2, there were increasing compositional gradients, and for x > 0.2 a GaAs-rich second phase appeared in the microstructure. Densification as well as alloying wlechanisms were enhanced by dissociation and, possibly, oxidation reactions of the powders. Densification of coarse prealloyed material, however, primarily depended on plastic flow phenomena and required temperatures just below solidus and pressures of 50,000 psi Thermal and electrical properties were measured. Although in no case was the figure of merit of melt growth materials approached closer than to within 25 pct, the better overall thermoelectric properties were found in coarse-grained, prealloyed materzals which had been compacted to near theoretical density and where grain regrowth had been induced. Similar results are believed to hold in other binary 111-V compound systems if processed under similar conditions. The densification of unalloyed GaSb powders during pressure sintering (= hot pressing) was shown to depend strongly on powder particle size.&apos; Fine powders displayed a "liquid skin effect" that enhanced compaction through the presence of liquid gallium, whereas coarse powders compacted predominantly by plastic flow. The liquid skin effect, in particular, appeared attractive for alloying GaSb with other, higher-melting, III-V compounds, and to densify these in a one-step operation. This is of special interest in the case of III-V compound alloys as the conventional techniques of melt growth or long-time annealing of powders2 is very time-consuming, especially in cases where a large separation of liquidus and solidus can be expected, such as in GaSbl alloys.2 It was felt that experimentation with this system, a particularly unfavorable example, would allow us to extrapolate to several other, more favorable, cases. Uses of Ill-V alloys are most evident in thermoelectric energy conversion devices.&apos; For this reason certain thermal and electrical properties were measured and compared to those of melt-grown material and to hot-pressed prealloyed powders. EXPERIMENTAL PROCEDURE The pressure-sintering apparatus has been previously described.&apos; Using this equipment, both powder mixtures of GaSb with GaAs and prealloyed GaSbl-,As, powders were hot-pressed. The mixtures were pre- pared from cast GaSb and melt-grown GaAs. The prealloyed material was obtained from stoichiometric melts, initially heated to 1200°C in an evacuated quartz ampoule, and then annealed in the solidus-liquidus interval. A typical annealing cycle consisted of a heating to 850°C (1 hr), extended successive annealing at 750°C (65 hr), and slow stepwise cooling (25 hr) to below solidus. The GaSb, GaAs, and GaSbl-,As, materials were ground in a vibrational mill to particle sizes below 500 . A jet mill reduced these further where necessary. Fine powders were analyzed by Coulter counting for their size distribution. Average sizes by volume were calculated from the data. Mixing of the powders, where necessary, was carried out through rapid vibrational motion. The hot-pressing operation consisted of a degassing period of 15 hr, in most cases at 690°C, followed by several hours of compression, normally 25,000 psi at 690°C for powder mixtures and 50,000 psi at 710°C for prealloyed powders. The chemical compositions were confirmed by X-ray fluorescence analysis. To estimate the degree of solid solution achieved, lattice parameters were determined and interpreted according to Vegard&apos;s rule. In addition, optical microscopy helped to correlate the relative amounts of the phases present as well as the degree of porosity to the measured density. To reveal grain boundaries, polished surfaces were etched4 with H 2 O:H 2 O:HCl = 2:l:l. In several cases microscopic concentration gradients were monitored by electron-probe analysis-. RESULTS AND DISCUSSION Alloying and Densification of GaSn-GaAs Powder Mixtures. After preliminary experiments showed that no appreciable alloying took place in mixtures of coarse GaSb (22.5 p) and fine GaAs (2.5 p) powders, hot pressing of mixtures was confined to fine powders only (3.1 and 2.4 p, respectively). Alloying and densification apparently occurred simultaneously with a grain regrowth mechanism which depended on the presence of a liquid phase.&apos; The liquid phase was provided by the dissociation of GasbS particles into liquid gallium and antimony above 555°C. This not only enhanced grain regrowth and densification, as in unalloyed GaSb,&apos; but took on additional importance here for the alloying process. Alloying was speeded up by the resulting liquid-solid interaction as compared to the very slow solid-state diffusion process normally expected at these temperatures.&apos; The results obtained with a series of powder mixtures have been compiled in Table I. It is seen that for mixtures with less than 20 mol pct GaAs, x < 0.2, the compositional ranges increased and for x > 0.2 a GaAs-rich phase and free antimony appeared in the microstructure in sizable amounts.

Jan 1, 1968

By J. Eric Belford

The Kidd Creek orebody is a massive base metal sulphide deposit with surface dimensions of 168 m by 670 m. The steeply dipping ore- body has been evaluated to a depth of 1 524 m. To date, the mining of the orebody has been divided into three stages. The first stage of mining was an open pit operation which supplied ore from 1966 until 1977 when a depth of 219 m was reached at the widest or north end of the orebody. The second stage of mining, called No.1 Mine, was the development of an underground mine to replace the pit and recover the ore from the floor of the pit to a depth of 792 m. Development of the underground mine started in 1969. Full production of 273 000 tonnes per month was attained in 1977. The third stage of mining called No.2 Mine, was initiated to accommodate a production expansion and included the development of a second underground mining operation to recover the ore from the bottom of No.1 Mine, i.e. the 2600 level; to a depth as yet undetermined but most likely the 4600 foot level. Development of the No.2 Mine began in 1974. Full production of 91 000 tonnes per month will be achieved in 1982. The choice of the 2800 level as the partition between the two underground mines was based on the following factors: The 2600 level is the lowest level which can conveniently be mined through the No.1 Mine crusher on the 2800 level. Development and trial stoping methods for mining at depth could be evaluated in the 2600 to 2800 block utilizing the existing hoisting facilities of No.1 Mine. Early development of the ore in the 2600 to 2800 block would provide additional mill feed sooner than could be achieved by developing from No.2 Shaft. The underground mining plan then is to mine from the pit floor down to the 2600 foot level and at the same time mine from the 2800 level down to at least the 4600 foot level. PLANNING The Kidd Creek operations are designed to follow a logical mining sequence. The grade of ore supplied to the concentrator is the result of following the mining plan. The philosophy of mining has been to mine downward in horizontal slices. In the case of No.1 Mine the slices are 122 m thick while in No.2 Mine the slices will be 183 m thick. The point of this approach is to mine the pillars immediately after creating them rather than allowing them to stand, deteriorate and generate uncontrollable situations. Two types of ore are handled separately to optimize recoverable values in concentrates. The &apos;A&apos; type ore is a copper zinc ore with some silver and little lead. The &apos;C&apos; type ore is a zinc silver ore with some lead and copper

Jan 1, 1981