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By B. N. Bose, M. F. Hawk

SINCE Davenport and Bain' introduced the isothermal transformation technique for the study of austenite decomposition in steels, a new field of investigation has opened up. Extensive research has been carried out on many different steels, but relatively little work has been done on eutectoid transformations in analogous alloy systems. The researches of Smith and Lindlief,² Mack,³ and Klier and Grymko²0 on the beta-phase transformation in copper-aluminum alloys, of Hibbard, Eichelrnan, and Saunders4 and Smith5 on the kappa-phase transformation in copper-silicon alloys, of Chaudron and Forester6 on the decomposition of "FeO," and of Wasserman7 on similarities between the iron-carbon, copper-aluminum, copper-tin, and copper-beryllium systems essentially comprise the field. The iron-nitrogen system, in view of its remarkable similarity to the iron-carbon system, is particularly attractive for the study of eutectoid decomposition. The present investigation is concerned with the study of isothermal transformation, proceeding by the familiar nucleation and growth processes, and of martensitic transformation characteristics of pure iron-nitrogen alloys. The kinetics of transformation and the morphology of the transformation products have been investigated, for these must be the factors determining the properties and behavior of the final product. The Iron-Nitrogen System he binary iron-nitrogen phase diagram has been a matter of considerable disagreement among vari01.1s investigators. However, the phase diagram according to Eisenhut and Kaupp8 and Lehrer10 is now considered essentially correct as reproduced in fig. 1. The important values, 2.35 pct nitrogen and 591°C, for the co-ordinates of the eutectoid point (obtained from this diagram and used in the re- search to be described) were confirmed in a concurrent study of Paranjpe, Cohen, Bever and Floe." The eutectoid decomposition involves the transformation of the ? face-centered cubic interstitial solid solution of nitrogen in iron to the a body-centered cubic interstitial solid solution of nitrogen in iron and the ?' nitride of iron. This nitride is essentially the compound Fe,N; it also possesses a face-centered cubic lattice but a considerably larger one than the ?; the nitrogen atoms in ?' are arranged in an ordered way in the centers of the unit cubes.8,10,11 A martensitic structure has also been reported8,12 in iron-nitrogen alloys and was studied in the research to be described here. Materials and Methods The specimens used in this investigation were prepared by nitriding "pure" iron. This iron was supplied by the Westinghouse Research Laboratories and is the product bearing their trade name "Puron"; it contains about 0.04 wt pct total impurities, the major portion of which is oxygen. Specimens were ribbons several inches long, a tenth of an inch wide, and 0.125 mm thick; this was the

Jan 1, 1951

By Paul Hunt

UP TO June, 1923, the Park-Utah mine had shipped about 94,000 tons of a direct-smelting ore of a gross value of $4,200,000, or about $45. a ton. These values were in gold and silver only, although the ore carried small amounts of lead, copper and zinc. Freight, treatment and deductions had averaged $15.40 a ton. At the expiration of the Pittman Silver Act there was in sight about 30,000 tons of a similar ore with a gross value of about $15 a ton in gold and silver, and a large body of partly developed lead-zinc ore of a gross value of about $20 a ton, 40 per cent. of which was represented by the lead-zinc content and the balance by the silver and gold. Mine costs had been high during the life of the Pittman Act, but as a large part of the profits had gone into equipment of the mine and the orebodies were large and had good walls, we knew that mine costs could be greatly reduced. We were therefore faced by the necessity of getting lower freight and smelter rates or of concentrating the ore. We did obtain better freight rates on lower grade ore, and a favorable smelting rate on the small tonnage of siliceous silver-gold ore, but this smelter rate could not be applied to the lead-zinc ore with any profit to ourselves. The Judge mill of the Park City Mining & Smelting Co., with which we were affiliated, was running to capacity; if we built our own mill it meant a 5-mile freight haul to a satisfactory millsite and a year's delay. Fortunately, the International Smelting Co. had just inherited a mill at Tooele which, with some changes, was about double the capacity required for its own ores. Flotation tests were run on Park-Utah ore and a contract entered into with a low base treatment charge per ton, the tariff being largely fixed by the metallurgical deductions. This contract has been admirably calculated so that the miner can follow a lean orebody to its limit. Such a procedure has no doubt made it difficult for the smelting company at times, but it has resulted in finding ore extensions that otherwise might have been missed, so in the long run it has profited too. A flat rate per ton would have been like mining up to the claim endlines in a great many of the stopes. In order to offer such a contract it can be inferred that the smelting company must have been able to make high recoveries and high-grade products on a very lean ore.

Jan 1, 1928

ASDIE from the John Fritz Medal, in which the Institute participates through its representation on the John Fritz Medal Board, the Institute itself has four awards it may make annually, as follows: the Robert W. Hunt Medal and Prize, the J. E. Johnson, Jr., Award, the James Douglas Medal, and the William Lawrence Saunders Medal. Robert W. Hunt Medal and Prize The partners of Robert W. Hunt established a fund which was presented to the Institute at a fitting ceremony on May 27, 1920, to establish an annual medal and a sum of money to be awarded under the following rules: 1. The award shall consist of two prizes: first of a gold medal, second of a sum of money; a certificate to accompany each prize. The money prize shall not be awarded to a member over 40 years of age, but under unusual circumstances, both prizes may be allotted to one person provided that he is not over 40 years of age. In general it will be understood that the Committee shall award the money prize to the younger men, rather than the medal. 2. The awards shall be made not oftener than once a year to that person or persons contributing to the Institute the best original paper or papers on iron and steel. The scope of the term "iron and steel" shall be determined by the subcommittee considering the awards. In general, papers dealing with the practical side of the subject have preference over those dealing with the theoretical side in recognition of the fact that Captain Hunt's main contributions to the industry have been in the improvement of production and quality of material. 3. A subcommittee of three to five, including the Chairman of the Iron and Steel Committee, shall be appointed by the Iron and Steel Committee annually to adjudge the award subject to approval. 4. The awarding committee shall submit its report to the Iron and Steel Committee at its October meeting, and the award shall be certified to the Secretary of the Institute in time to permit the presentation to be made at the Annual Meeting of the Institute. 5. The recipient of the award shall be designated "The Hunt Medallist." This prize is administered by the Iron and Steel Division. Awards of the medal have been made as follows: 1920—Robert Woolston Hunt. 1926—Charles Lewis Kinney, Jr. 1928—John A. Mathews. 1929—Edgar Collins Bain. J. E. Johnson, Jr., Award This award is made from the income of a fund of $3000 donated by Mrs. Margaret Hilles Johnson in memory of her husband, J. E. Johnson, Jr., who was a prominent engineer, author of two valuable volumes on iron blast-furnace construction and practice, vice-chairman

Jan 1, 1929

By W. H. Gunniss

When the copper smelters were built, in Montana, all of the refractory products which were used in their construction were shipped in from Eastern factories. It was apparent that if a material suitable for the manufacture of these products could be found within the State, a saving of freight could be effected and a new industry built up. Prospecting for such materials was started and experiments were made with samples from numerous deposits. Considerable effort and funds were expended in an attempt to manufacture silica brick from Dillon quartz, a light colored sandstone that is found near Dillon, Mont., on the Oregon Shortline railroad. As a brick material the Dillon quartz was a failure, but it has proved very satisfactory as a silica cement. It is now being used in laying silica brick and for reverberatory furnace bottoms. A bed of quartzite that is particularly suited to the manufacture of high-grade silica brick was finally discovered at Browns Spur, 6 miles west of Anaconda. The material from this deposit is now being used in the manufacture of the Anaconda silica brick, which have gained a wide reputation for heat-resisting and lasting qualities. The analysis of an average sample of this quartz is: SiO2, 96.7; Fe2O3, 0.3; Al208, 2.5; CaO, 0.3 per cent. The very low percentage of fluxing ingredients makes this a most refractory material. All of the Anaconda silica brick are hand molded. Various types of brick machines have been tried, but the hand-mold process proved the best suited to the manufacture of silica brick from this material. The silica is first put through a jaw crusher and is then dumped into wet pans, where 4 per cent. of lime paste is added, to produce a bond. Without the lime the material would not be plastic enough to mold. After a few minutes' grinding in the wet pans the material is conveyed to the molder, who forces it into the molds by hand. The brick are then dumped on pallets and placed in the drier, where they are left. until dry enough to be set in the kilns. Some of the brick are re-pressed before being dried. They are burned about five days, in round down-draft kilns. It is not necessary to have as much heat in the kilns as the brick will be subjected to when in use in the furnaces. Montana refractories are used in smelters throughout the West. Prospecting for fire clays was also carried on. After experimenting with clays from several different deposits, it was found that a mixture of

Jan 1, 1914

By T. E. Leontis

Several publications1-7 during the past few years have demonstrated the markedly greater effect of cerium, as compared to all other alloying elements, in enhancing the strength and creep resistance of magnesium at elevated temperature either with or without the presence of other elements. In the work reported in Ref. 1-6, the cerium was added in the form of Mischmetal, which contains all the rare earth elements in essentially the same proportions as they occur in monazite sand, the principal ore of these metals. Mellor and Ridley7 have presented the creep characteristics at 200°C of magnesium alloys prepared both with pure cerium and with Mischmetal. Up to the present time, however, no comprehensive study of the effect of the various component elements of Mischmetal on the properties of sand-cast magnesium has been made. This hiatus in magnesium technology undoubtedly is associated with the difficulty in obtaining the rare earth metals separately. This investigation provides such a survey, the object of which was to determine which of the elements present in Mischmetal contributes the greatest effect in developing high strength and high resistance to creep at elevated temperatures. Toward this end the compositional variation of these properties has been determined as a function of temperature in the following alloy systems: 1. Magnesium-Mischmetal 2. Magnesium-cerium-free Misch- metal 3. Magnesium-didymiuin 4. Magnesium-praseodymium- lanthanum 5. Magnesium-cerium 6. Magnesium-lanthanum This designation, based on the names of the metals as furnished by the producer, is used throughout the paper in order to avoid the complicated system of listing all the elements present in the more complex alloys. The composition of the metals and the alloys is discussed in detail below. Preparation of Alloys ALLOYING INGREDIENTS The chemical composition of each of the six alloying ingredients used to prepare the alloys reported in this paper is given in Table 1. In each case, the percent total rare earths, percent cerium, percent neodymium, percent praseodymium, and percent thorium were determined in addition to the listed impurities. The percent lanthanum was determined by difference from the total rare earth content and consequently includes the other elements (samarium, terbium, yttrium, etc.) present in Mischmetal. These additional elements, however, seldom amount to more than 1 to 2 pet of the total rare earth content of Mischmetal. The iron content of the Mischmetal is considerably lower than that of the other metals. This grade of Mischmetal is now readily available. The metals are listed in the order of decreasing complexity. Elimination of the cerium from Mischmetal results in what the trade calls "Cerium-free Mischmetal." Carrying the separation a step further by eliminating the lantha-

Jan 1, 1950

THE CHAIRMAN (E. G. SPILSBURY, New York, N. Y.).-The relation of the character of manganese ore to the surrounding rocks was called to my attention very strikingly in a recent investigation in Costa Rica. In the foothills of the main coastal range there is a large deposit of manganese which extends for over 150 miles along the coast. This is in a porphyry district and the occurrences are almost exclusively along the lines of contact between a recent diorite intrusion through the porphyries. Wherever that intrusion appears to have exerted great force, the line of contact is very clear between the porphyries and the diorites. Where the action has been slower and the lifting force of the intrusion more gradual, there has been a zone of fracture of very considerable width. Those ores which occur where the fractured zone has not been very extensive carry a, lower percentage of manganese than where it has been deposited along a wider zone of fracture. In the so-called narrow veins, which are really the predominant ones, the solution carrying the manganese has evidently attacked the silica in the intrusive rock, and the resulting ore is practically a combination of manganese and silica, running froth 20 to 30 per cent. of manganese and from 20 to 40 per cent. of silica: hence those ores are not likely for a long time to become a factor in our manganese supply :for this country. On the other hand, where the disturbance to the porphyritic schist has been more intense; the manganese deposits are not so extensive, but the ore is richer, running from 45 to 51 and 52 per cent. manganese, with a silica content of from 4 to 5 per cent. There seems to be some resemblance in these deposits to those of the Cuyuna range. EDMUND NEWTON, Minneapolis, Minn.-The State Bureau of Mines has been working on the problem of concentrating manganiferous iron ore for two years or more. I should consider hand sorting as the best form of treatment, because it is practised at all of the mines which ship ore for making alloys, but not, however, oil the ore that is being used for pig iron. Hand sorting, assisted by selective mining, is readily applicable to some of this ore because the gangue is practically the original rock and is easily separated. However, it is only in rather limited zones that we find clean patches of rock. Generally the silica exists as a skeleton of the original rock structure, in which the manganese has been precipitated; some of the silica may have been dissolved, but if any of the original rock remains, the silica must be eliminated by ore-dressing processes.

Jan 1, 1918

By W. D. Robertson, D. A. Koss, A. J. Goldman

THE significance of the hcp (E) structure, which appears when Fe-Cr-Ni alloys (stainless steels) are transformed martensitically, has been the subject of considerable study and speculation.'-7 It has been proposed that the hcp structure is an intermediate phase in the transformation: fcc (austenite) — hcp (E) -bcc (0, martensite). However, recent studies by transmission electron microscopy6,7 have indicated that the hcp structure may be a consequence of the large shear strain (10 deg) associated with the fcc to bcc transformation. That is, the transformation to a bcc structure is accompanied by extensive dissociation of dislocations in the parent austenite, which has a low stacking-fault energy.'-'' X-ray diffraction analysis of the transformed alloy reveals a pattern of lines corresponding to an hcp structure, together with the parent austenite and the bcc product. The fact that the hcp structure is observed only in association with the bcc product in these alloys1'4'6'7 lends support to the conclusion that the hcp structure is a secondary product of the transformation. But, the evidence is circumstantial and more definite resolution of the two possibilities mains to be obtained. If the hcp structure is an intermediate product of the transformation, as in 1) above, then two distinct Ms temperatures should be observed, Ms and To evaluate this possibility, three different techniques that are particularly sensitive to the structural changes accompanying such transformations have been used in an attempt to detect two transformation temperatures in an Fe-15.1 Cr-11.7 Ni alloy: 1) high-sensitivity differential thermal analysis, 2) the temperature dependence of resonant frequency (elastic moduli), and 3) internal friction of cylindrical specimens vibrating in either longitudinal or torsional modes. To obtain the necessary sensitivity, a differential thermal analysis technique was developed for the purpose, Fig. 1. The differential temperature between a nickel standard and the specimen was amplified to produce a sensitivity of 0.02OC (0.7 v) in temperature difference. The specimen and the standard were surrounded by a copper block and the entire assembly was immersed in a solution of methyl and ethyl alcohol, freezing point, - 140OC, which provided the necessary thermal stability to reduce temperature fluctuations to negligible proportions. A cooling rate of about 1.5OC per min was obtained by bubbling liquid nitrogen through the liquid bath. In order to calibrate the experiment with respect to the evolution of heat in the transformation from fcc to hcp structures, differential cooling curves were obtained for an Fe-19.8 Mn alloy, which transforms martensitically to E.'"-' a Ms(e) temperature of 145°C was clearly defined by a temperature

Jan 1, 1964

By F. S. Norcross

MANGANESE has long been considered one of the United States' most important strategic raw materials. Its indispensability in steel manufacture makes it vital to the nation's industrial life. Coupled with this indispensability is the fact that domestic producers have not been able as yet to supply more than a small part of the nation's manganese needs; consequently the United States has had to depend upon such distant foreign sources as the U.S.S.R., British India, the African Gold Coast and Brazil for the major portion of its ore. The great bulk of the mineral is consumed in the form of ferromanganese, an alloy that averages 8o per cent manganese and 20 per cent mainly iron and carbon. Manganese is used as a deoxidizer and desulphurizer in steel manufacture. By combination with the residual oxygen and sulphur of the bath, it helps to produce a clean, sound metal. Approximately 14 lb. of manganese, it is estimated, is used in making one ton of steel. For standard-grade ferromanganese, the ore should have a minimum of about 48 per cent Mn and preferably more. Beneficiation methods have not yet been developed for making the immense low-grade deposits in the United States salable at prevailing prices. Dependence upon foreign sources thrust the United States into serious difficulties during the World War. At the start of hostilities in 1914, the nation was obtaining about four-fifths of its ore from the Eastern Hemisphere. Domestic production had been negligible, amounting to only 3000 to 7000 tons a year. As the war continued, shipments from the East, endangered by sea attack and blockade, dwindled rapidly. Imports from Brazil mounted. In this grave emergency, the United States, starting almost from scratch and under the stimulus of high prices, succeeded by 1918 in producing a peak of 311,000 tons, about 3 5 per cent of its consumption that year. Since the war, the United States has depended upon foreign sources for more than nine-tenths of its high-grade ore. During 1936, 1937 and 1938, imports for consumption averaged 736,000 tons a year. During the same period, domestic shipments averaged 21,000 tons a year. Of the imports, the U.S.S.R. accounted for an annual average of 280,000 tons, the Gold Coast 208,000 tons, India 74,000 tons, and Brazil 72,500 tons. But India and Brazil, which in 1936 ranked third and fourth in the list of importers, were displaced in 1937 and 1938 by a new and much nearer source-Cuba. From less than 1 per cent of United States imports in 1931, the island republic increased its shipments to more than 27 per cent in 1938. Cuba's average for this three-year period was 97,000 tons, and its total for 1938 was 131,000 tons.

Jan 1, 1940

By G. E. Tardiff, A. A. Hendrickson

THE objectives of this communication are to present the solid-solution strengthening data for silver-base zinc single crystals and to evaluate the importance of strength contributions from several mechanisms through the use of this data combined with that for the silver-base aluminum case.' Some features of the yield point behavior of silver-base zinc crystals were previously reported.' Silver-base zinc alloys were prepared by induction melting 99.99 pct Ag with 99.9 pct Zn in high-purity graphite crucibles contained in argon-filled quartz tubes. After the first melting, the ingots were cut into short lengths, redistributed in the molds, and remelted in order to reduce solute-concentration variations. Alloy single crystals were then grown from the melt through the use of a modified Bridgeman technique which consisted of lowering the graphite crystal mold through a hot zone at a rate of 3/8 in. per hr. As in the melting operation, the molds were contained in argon-filled quartz tubes. Gage lengths 2 cm in length were introduced by both spark machining (circular cross sections) and abrading and acid etching (rectangular cross section) followed by electropolishing (a comparison of the critical resolved shear-stress values prepared by the two techniques showed no differences in strength values). The final cross-sectional areas of the crystals were approximately 5 sq mm. Prior to testing, the crystals were annealed at 600°C for 20 hr in argon atmospheres, furnace-cooled, and lightly electropolished. Crystal orientations were determined using the back-reflection method. The tensile testing was done on a Model FM Instron at a strain rate of 1(T4 per sec. Test temperatures of 77", 200°, and 400°K were attained by immersing the specimens in liquid nitrogen, dry ice-acetone mixtures, and silicone oil, respectively. The critical resolved shear-stress (CRSS) values for silver-base zinc crystals as a function of composition and testing temperature are given in Fig. 1. It will be noted that the CRSS for silver-base zinc solid solutions, as in the silver-base aluminum1 case, depends on temperature in a manner typical of fcc solid solutions: at high temperatures (-300°K and above), the CRSS is relatively temperature-independent but becomes strongly dependent on temperature at lower testing temperatures. A reasonable picture of solid-solution strengthening for silver-rich solutions at room temperature based on "direct" strengthening mechanisms3 is as follows. Since silver alloys have low stacking-fault energies, extended dislocations are expected and it is possible that Suzuki locking4 makes the major contribution to the room-temperature solute strengthening. This provides essentially temperature-independent strengthening since thermal motions of the dislocation line are not large enough to aid the dislocation in escaping the solute atmosphere extending over the fault width. An estimate of the

Jan 1, 1964

By M. D. Hassialis

THE claim is made in a number of patents1,2,3,4 that some compounds of the class known as aryl sulphides have collector properties. One of these patents generalizes the claim to include all aryl sulphides, whose generic formula is R-S¬R[=]-R’ (where x = r,2, . . . ), with the restriction that if the aromatic radicals R, R' contain substituent groups these groups may not contain nitrogen or oxygen. Moses, Hess, and Perkins cite as evidence for their claims the results of flotation tests on Anaconda and Miami copper ores using Biphenyl sulphide, ditolyl disulphide and dinapthyl disulphide as collectors. The use of alkyl sulphides as collectors has also been reported5 with the conclusion that the alkyl sulphides are better collectors than the corresponding aryl sulphides. The experimental work cited appears to confirm this contention. In order to test these claims with respect to diphenyl sulphide, a sample, purchased from the Eastman Kodak Co., was tested against Anaconda ore. The procedure followed was that of Moses, Hess, and Perkins. A sample of ore weighing 500 grams was placed in a laboratory ball mill. To this was added 220 grams of water, 0.06 grams of commercial diphenyl sulphide (1/4 lb. per ton of ore), and 0.8 grams of lime (3 lb. per ton of ore). The material was ground until 93 per cent passed a 65mesh screen. This pulp was diluted to 16 per cent solids. A sample of the diluted pulp was placed in a Minerals Separation type of laboratory flotation cell. After a 2-min. agitation period, pine oil was added and the froth collected for a period of 15 min. This test recovered 68 per cent of the copper, with a ratio of concentration of 6.8: 1. The tailing assay was 0.3 per cent Cu. Moses, Hess and Perkins attained a recovery of 75 per cent, with a ratio concentration of 12: 1. Although these results do not compare too well with those of Moses, Hess and Perkins, subsequent tests showed an improvement, as judged by vanning of the tails. It is concluded, therefore, that the patent results are confirmed. CONTACT-ANGLE TESTS In order to study the response of the various minerals, found in Anaconda ore, to commercial diphenyl sulphide, some contact-angle tests were made. Polished particles of bornite, chalcocite, chalcopyrite, pyrite and quartz were conditioned for 15 min. in a suspension of diphenyl sulphide in water. The concentration of this suspension was 0.284 grams per liter, this being the concentration of this reagent in the ball mill. The conditioned particles were rinsed with water (not rubbed with filter paper or boiled linen) and then tested against an air bubble in the bubble machine, with the following results: born-

Jan 1, 1943

By David A. Thomas, Eugene S. Meieran

MECHAMCAL, electrical, and other property measurements are often more easily made on wires than on sheets. In order to carry out transmission electron microscopy on the same material used for property determinations, we have developed a method for preparing thin foil specimens of wires. The technique was developed for 0.030 in. diam tungsten wires, and is a modification of the thinning techniques used by Wilsdorf, et al 1 A length of wire is first ground to about 0.010 in. thick by mounting the wire in low melting temperature wax, hand grinding a longitudinal flat, removing and reversing the wire in the mount, and then grinding a second parallel flat. The 0.030 in. wide and 0.010 in. thick strip is cut into 1/8 in. lengths to fit in the specimen holder of the electron microscope. Next the specimen is gripped in platinum-tipped tweezers (the anode) and placed 2 mm below a hol- low copper cathode with a 0.010 in. ID nozzle. Electrolyte, 10 pct NaOH, flows by gravity feed through the nozzle onto the specimen, as shown in Fig. l(a). Polishing is carried out until a shallow impression is made on one surface, and then the specimen is turned over and the opposite surface indented. The metal between the two impressions should be about half the specimen thickness, as is shown by the heavy line in the cross section in Fig. l(b). The entire specimen is then electropolishedin 2 pct NaOH until a hole appears at the location of the indentations. The apparatus is shown in Fig. 2, and is essentially the same as that used by Wilsdorf et al. at The Franklin Institute. Light is reflected by a mirror onto the bottom surface of the specimen! which is viewed by a stereoscopic microscope placed above it. Polishing is carried out until light is seen, indicating that a hole has formed, and then immediately stopped. The specimen is washed in water. alcohol, and ether, and is then ready for examination. The specimen should be reversed in its platinum clip during electropolishing to insure equal polishing on both sides of the impression. For tungsten, indenting at 120 v and 0.04 amp takes less than 1 min, and final polishing, at 10 v and 1 amp, less than 5 min. The portion of the specimen available for transmission microscopy surrounds the hole, as is seen by the dashed lines in Fig. l(b). Slight electroetch-ing accompanying electropolishing reveals the mi-crostructure, as seen in Fig. 3(a) by light microscopy. Low-magnification electron microscopy, as in Fig. 3(b), enables the same areas and grains to be viewed and identified when subsequently examined at high magnification. Fig. 4 is a typical structure of

Jan 1, 1963

By Walter Showak

The published phase diagrams for the copper-zirconium system1,2 indicate that the solid solubility of zirconium in copper is not accurately known. Studies made on relatively impure alloys by Pogodin, Shumova, and Kugucheva3 yielded a maximum solubility value of 1 wt pct Zr at the eutectic temperature. Allibone and sykes5 reported that an as-cast 0.2 wt pct Zr alloy is single phase at room temperature. Limited results obtained by Raub and Enge14 indicated that zirconium solubility in copper is less than 0.13 wt pct Zr at 940°C. Tn 1960, on the basis of a microstructural examination of several copper-rich Cu-Zr alloys, saarivirta6 placed the maximum solubility of zirconium in copper at 0.15 wt pct at the eutectic temperature, 980°C. The present note describes results obtained during a re-investigation of the Cu-Zr system for the purpose of accurately establishing the solidus and solvus curves and the eutectic temperature in copper-rich alloys. High-purity copper (99.99 pet) and zirconium (99.64 pet) consolidated reactor grade sponge were used to prepare several alloys, containing up to 2 wt pct Zr, by induction melting in graphite crucibles in vacuum and chill casting into a split steel mold. The melting procedure consisted of first melting the copper charge and then adding the bulk zirconium wrapped in pure copper foil. Chemical analyses were made of both the cold-rolled alloy ingots after homogenization at 925°C for 450 hr in evacuated quartz capsules and of small specimens which had been used in the phase diagram studies. 'The carbon content of each alloy was also determined and was found to be less than 0.001 wt pct in every case. Metallographic and electrical resistivity measurements were used as the primary methods for this investigation, although some thermal analysis studies were also performed. Heat treatments of all the alloys were carried out with the specimens wrapped in molybdenum or alloy foil (of the same composition as the specimen) and sealed in quartz tubes either in vacuum or under a purified helium atmosphere. Following high-temperature anneals for long periods of time, slight depletion of zirconium from the specimen surface was observed. Therefore, careful preparation of samples for microscopic examination and chemical analysis of the samples themselves was necessary to check the composition of samples used in determining phase boundaries. Points on the solvus curve were determined on quenched specimens by both isothermal reaction after solution heat treatment at 950°C for 8 hr and by isothermal annealing of alloy specimens at successively higher temperatures for times ranging from 24 to 500 hr. Liquation studies for positioning of the solidus and eutectic temperatures were performed by holding a pre-

Jan 1, 1962

By P. W. Bakarian

PREVIOUS determinations1,2,3 of the texture of magnesium and its alloys have shown only slight variations in the principal features of the structure. This investigation presents pole figures for magnesium and two of its alloys, in which differences of some magnitude will be shown. Schmid and Wassermann have considered the texture of magnesium in analogy with that of zinc-also a hexagonal lattice. Whereas the zinc texture is said to be derived primarily through basal slip and secondarily through {102}† twinning, the {102} twinning is considered impossible at the later stages of the rolling in magnesium because of its smaller axial ratio. This state of affairs appears reasonable for pure magnesium, but for alloy textures the situation is more complex. A double orientation similar to that found in zinc has been reported by J. D. Hanawalt,4 and the addition of small amounts of calcium to magnesium and its alloys to produce a double texture was noted by J. C. McDonald.5 The pole figures of this investigation, using an improved X-ray technique, show these various textures. The dependence of directional properties of rolled sheet on modifications of texture is well recognized. Correlation of physical properties with existing texture should be even more significant if quantitative valuations are attached to the various areas on the pole figures. Such a quantitative technique is developed herein. EXPERIMENTAL METHOD Two alloys were used, besides high-purity magnesium. In each case, the metal was extruded to bars 32 in. thick and hot-rolled to a thickness of about 0.075 in. It had been established previously that such a reduction was more than sufficient to eliminate the extruded structure. The rolling proceeded in the same direction as that of the extrusion, without any cross rolling. The temperatures corresponded to normal commercial practice, averaging around 600°F. A unique method of preparing the sample was developed in this work. Instead of using a flat specimen, a stem of the metal was cut out of the rolled sheet in the desired direction (rolling direction) as shown in Fig. 2. From a sheet of 0.075 to 0.065-in. gauge, the stem was cut to a square cross section with a jeweler's saw, rounded with a file and polishing paper to a diameter of 0.060 in, and evenly etched in dilute hydrochloric acid to a diameter of 0.038 ± 0.001 in. In this way, a cylinder of the original sheet with its axis in the desired direction was produced. By using this type of specimen for the pin-point pictures, any variance in the absorption of the diffracted beam at the various angular settings of the specimen, was completely eliminated.*

Jan 1, 1941

By J. B. Cohen, M. B. Beaver, R. J. Black

RECENT investigations have shown that face-centered cubic metals may deform by twinning. Blewitt, et al' found that at 4.2"K the mode of def~rmation of single crystals of copper changed at large strains and markings formed on (111) planes. Later they- emonstrated by X-ray diffraction and metallography that the markings were twins and showed that favorably oriented single crystals of copper deformed by twinning at 78°K. They also observed twinning in silver and gold deformed at 4.2 and 78°K. Wagner3 obtained evidence for twinning from the peak shape of diffraction lines of silver cold-worked at 78°K, but twins small enough to cause such effects are not likely to be detected metal-lographically. In the work reported here lamellar structures were observed in deformed silver-gold alloys. They appeared to be mechanical twins, but metallography could not establish this conclusively. Their tendency to form depended on strain rate, temperature and composition. Specimens of silver-gold alloys (0 to 83 wt pct Au) were deformed plastically. One set was worked by hammering under liquid nitrogen, at room temperature and at intermediate temperatures. Another set was compressed slowly in liquid nitrogen to the same reductions as those produced by hammering. Tensile specimens (0.015 x 0.120 x 1.5 in.) of various compositions and approximately equal grain size (0.011 to 0.016 cm) were tested at -195°C and at room temperature. In microsections of all specimens deformed by hammering at —195°C thin lamellae appeared, Fig. 1. They were aligned in definite directions in each grain. In some grains they had two orientations. Where lamellae intersected, a displacement was apparent. Near the center of the left margin of Fig. 1 shear has taken place beyond the fully developed intersecting lamella. Many lamellae resembled Neumann bands in alpha iron. They were parallel to one side of triangular etch pits in the matrix (as in Figs. 1 and 2). The individual lamellae were narrow and had little substructure. This suggested that they did not result from concentrated local slip. The shape of etch pits within the lamellae differed from that of pits in the matrix, as can be seen in Fig. 2; this indicated a difference in orientation. Specimens slowly deformed at —195°C contained regions in which the lamellae were clustered. In these specimens some lamellae were bent and presumably had formed before the termination of the deformation. Structures of greater width than the lamellae were also seen.4 More lamellar structures formed on impact than during slow compression to a given reduction. This was true of all compositions. The structures became less abundant with increasing temperature of deformation. None was observed after extension to fracture at room temperature, but they could be pro-

Jan 1, 1959

The Gooseberry Mine is located 38 krn (24 miles) by road east of Reno, 13 km (8 miles) south of Interstate 80. The mine was originally discovered in 1906 and remained in the control of the Martin family of Fresno, who worked the-property with Mexican ranch hands for 68 years. Westcoast took over the property in 1976 from Apco Oil Corporation. During the time the Martins operated the mine, a 305 m (1,000 ft) inclined shaft was sunk with drifts developed on eight levels exceeding a total of 3,000 m (9,000 ft) in length. It is interesting to note that for over one -half century all development ore was stockpiled. West- coast, the United States mining subsidiary of Home Oil Company Ltd., Calgary, Alberta, completed sinking another vertical shaft to the 396 m (1,300 ft) level. Development work between 122 m and 305 m (400 ft and 1,000 ft) levels has proved the existence of a fine ore body over 300 m (1,000 ft) long. The silver-gold ore grade is fairly consistent in the vertical section, but copper, lead and zinc may show slight increases with depth. Average width of the ore bearing portion of the vein is 2.5 m (8.3 ft). Stoping is by cut-and-fill method. Average silver values within the ore zone have increased from the 152 m (500 ft) level to the 305 m (1,000 ft) level, although the gold values do show some decrease. It is not possible for the geological staff to predict the depth of the ore. However, several years of ore reserves have been proved in the existing mining areas. Important ore minerals are argentite, native gold, and electrum. Trace amounts of galena, chalcopyrite, and sphalerite are associated with the precious metal mineralization. The vein is mainly composed of calcite and quartz. Mine-run underground ore is dumped from the hoisting skip into a coarse ore bin followed by a jaw crusher, an impact crusher, and a 600 mt (650 st) fine ore bin. The mill has a capacity of 317 mt per day (350 st per day). Two-stage grinding is done by a rod mill followed by cyclones with the underflow sent to a ball mill in closed circuit with the cyclones. Cyclone overflow after conditioning receives a primary float in four 1.7 cu m (30 cu ft) cells and a second stage of conditioning ahead of 24 0.8 cu m (30 cu ft) secondary flotation cells. No cleaning stages are used. Flotation tailings are cycloned for a sand-slime separation with the sands used as underground stope fill and the slime portion to tailing dam storage.

Jan 1, 1981

Duval Corporation, the owners of the Sierrita, Esperanza, and Mineral Park copper operations in Arizona, first acquired the mineral rights to their Battle Mountain, Lander County, Nevada, property in 1962. Development of the mine commenced in mid - 1965, and the copper operation began at the end of 1968. The ore, a mixture of chalcocite and chalcopyrite, was milled and floated at a rate of 3, 175 mtpd (3,500 stpd). Because of low copper grade and price, the plant was shut down after about ten years of operation. Attention was then turned to an adjacent low-grade precious metal ore body which contained 2.74 g Au and 3.4 g Ag per mt (0.08 oz Au and 0.10 oz Ag) and minor amounts of copper. Test work revealed recovery by Carbon-In- Pulp treatment would amount to approximately 2.8 mt (90,000 oz) each of gold and silver per year. A rapid engineering and construction schedule resulted in the world's largest, as of late 1980, Carbon-In- Pulp plant being put on-stream in January 1979, with a capacity of 2.720 mtpd (3,000 stpd). Fortunately, the original crushing and grinding plant with all its infra structure was available, and the only modification needed was the addition of a gravity circuit to remove coarse free gold ahead of Carbon- In-Pulp treatment. One of the four primary 500 mm (20 in.) cyclone underflows in the primary ball mill circuit is directed to a secondary ball mill where its product is again cycloned. The cyclone underflow is screened at 3,360 microns (6 mesh) with the undersize being treated on two Pan American 1.07 m by 2. 14 m (42 in. by 84 in.) jigs. Hutch product is further concentrated on two Wilfley tables, a magnetic separator, and on a third Wilfley table where approximately 930 g (30 oz) of gold are recovered each day for amalgamation, retorting, and smelting. Returning to the grinding circuit, the final cyclone overflow is sent to the original plant tailings thickener to obtain proper pulp density for Carbon-In-Pulp treatment. Thickener underflow, at about 40% solids, is then conditioned with air and lime in a series of two 8.5 m by 9.75 m (28 ft by 32 ft) 15O cone bottom Pachucas for oxidation of pyrrhotite. The pulp is then split into two streams for cyanidation for 48 hours in two lines of eight Pachucas of the same size. Pulp is transferred from tank to tank by auxiliary air lifts. Cyanided pulp is then sent to a series of six C. I. P. mechanically agitated tanks with one hour retention in each tank. Originally these

Jan 1, 1981

E. P. Pfleider, University of Minnesota I would like to ask Bob Merrill whether he considers that horizontal concave curvature of a slope has any stabilizing effect, such as Jenike 1 suggested several years ago. R. H. Merrill, U. S. Bureau of Mines, Denver Federal Center The stabilizing effect is due to the restraint offered to radial movement by the curvature. We found in laboratory tests that if we constrained the rock with the same stresses as those measured in the pit then it would sustain a maximum stress about two or four times greater than when the same rock type was unconstrained. We are therefore definitely of the opinion that a constrained situation in a slope is favorable towards stability. G. A. Leonards, Purdue University I was interested in Mr. Lane's observations concerning the correspondence between rate of slide movement with rise of reservoir. Perhaps the most interesting feature is that the rate of movement at the time the rock slope failed was less than the rate at an earlier time when it did not fail. This is difficult to explain from current slope stability theory. K. S. Lane, U. S. Army Corps of Engineers I believe that reduced rate of movement is the result of the progressive type of failure, such as described by Patton and Deere. which occurs along the sliding surfaces. It is difficult to analytically define the progressive failure condition for inclusion in slope stability conditions, but its existence should be recognized in design. We should also realize that many apparently stable slopes undoubtedly contain overstressed regions. To design a slope with no overstressed region would be uneconomical and conservative. D. H. Deere I would pose the question-"What is the meaning of a factor of safety of one?" We were involved in the design of a large, irregularly shaped, underground cavity with an unsupported span of several hundreds of feet. Tests on rock specimens indicated a strength of 1300 lb per sq in. The RQD would have been between 90 to 100 percent indicating excellent structural continuity. In-situ stress determinations indicated an approximately hydrostatic state of stress at a level of 1400 lb per sq in. Calculation of stress concentrations at the walls indicated that the stresses there would be about 3000 to 4000 lb per sq in. Admittedly the rock is in a confined condition everywhere except at the very skin of the wall and the rock walls would thus on the average be somewhat stronger. Allowing for the effect of restraint the factor of safety was found to be less than 0.5 over a region several feet into the wall. Construction was started, using rockbolts only to support the walls. Failure around the immediate skin occurred after each

Jan 1, 1967

By Herbert Hoover, Harlod Washburn

This paper is in the nature of a rough preliminary report on the progress that has been made in the application of the mass spectrometer to various problems arising in the petroleum industry. A few years ago the authors considered a number of the problems that were arising in the qualitative and quantitative measurement of small amounts of hydrocarbons. The methods available of making analyses by chemical techniques appeared to leave much room for improvement. Without going into the reasons at this point, attention was turned to the possibility of employing physical instead of chemical methods of accomplishing the desired results. A preliminary investigation disclosed that the mass spectrometer presented a possibility of solving many problems which could not easily be accomplished by other methods. Work was begun in developing the necessary apparatus and technique. A great deal of encouragement and many valuable suggestions were received from Dr. Robert A. Millikan, Dr. W. R. Smythe, and Dr. W. N. Lacey, of the California Institute of Technology, and from Dr. E. 0. Lawrence, who recently received the Nobel Prize, of the University of California. The authors particularly wish to acknowledge the very great willingness of these outstanding scientists to be helpful in solving many of the problems that were involved. So far as the authors are aware, this was the first application of the mass spectrometer to commercial work. The results were considerably better than had at first been anticipated. Briefly, it is possible to run a qualitative and quantitative analysis of an unknown mixture of hydrocarbon gases, with an accuracy of better than plus or minus 5 per cent of each of the various constituents. An exceedingly high degree of sensitivity has been obtained, and a relatively short time is required to complete an analysis. Furthermore, it is unnecessary to separate a mixture of gases into its various components in order to complete the analysis. The Mass Spectrometer The mass spectrometer should not be confused in any way with the optical 01 grating type of spectrograph now in general use. The operation of the mass spectrometer is entirely different in principle and bears practically no resemblance to the optical or grating instruments. The original conception and development of the mass spectrometer dates from and is generally credited to Aston, of Cambridge, England. An early accomplishment of his research, about 20 years ago, was the discovery that the inert gas neon was actually a mixture of two kinds of atoms, one of the atomic weight 20 and the other of atomic weight 22. These two components occurred mixed in such proportion as to yield the usual atomic weight of 20.2. The study was continued and most of the elements were shown to be mixtures of components whose atomic weights can, to in

Jan 1, 1941

By Frank Foote, E. R. Jette

In recent years the constitution of the high-silver aluminum-silver alloys has been extensively investigated. Hansenl has reviewed the literature to 1935. More recently, Obinata and Hagiya,2 Hofmann and Volk,3 Taziri4 and Tishchenko5 have confirmed the general features of the phase diagram in the region around 25 atomic per cent aluminum. In this paper we present the results of high-precision measurements of lattice constants of the silver-rich alpha solid solution in the homogeneous range and the neighboring two-phase regions. These results are used to establish the nature of the solid solution, the identity of directly measured densities with those calculated from lattice constants and the homogeneity limits of the alpha solid solution with respect to three different neighboring phases. A study of the earlier investigations indicated that the last two subjects in particular required new and accurate data. Experimental Procedure Preparation of the Alloys.—The alloys were made from high-purity silver and aluminum. The silver was "Proof Silver," 99.999 per cent pure, supplied by the U. S. Metals Refining Co. The aluminum was 99.97 per cent pure (contained Si, 0.009 per cent; Fe, 0.0016 per cent; Cu, 0.004 per cent) and was supplied by the Aluminum Company of America. The lattice constants of these two materials have been reported by Jette and Foote.6 Weighed amounts of the two metals were placed in alundum crucibles and melted in vacuo in a high-frequency induction furnace. The melts were allowed to cool in the crucible, the ingots thus obtained weighed about 10 grams. These ingots were then filed clean, hamered, again cleaned and given a homogenizing anneal in vacuo of from 6 to 15 days at temperatures ranging from 500" to 695°C. The ingots were air-cooled from the annealing temperature. Lattice-constant Measurements.—Carefully prepared filings for X-ray analysis were sealed into evacuated quartz or Pyrex tubes and annealed for various periods of time at suitable temperatures. The furnaces used were vertical, rapid-quenching furnaces, the samples being quenched by crushing the sample tube under water by means of a heavy plunger. The general X-ray technique has been previously described6 The cameras were of the symmetrical, back-reflection, focussing type. Ka, radiation from a cobait-nickel alloy target was used. The wave-length values were taken from the second edition of Siegbaum's book.7 A correction for the index of refraction was applied and the lattice constants were calculated by the method of Cohen.8, 6 The lattice constants were calculated to a common temperature of 25°C., using the value of the linear expansion coefficient of pure silver as 18.9 X 10-6. Presumably the expansion coefficient for

Jan 1, 1941

By P. W. Bakarian

Previous determinationl,2,3 of the texture of magnesium and its alloys have shown only slight variations in the principal features of the structure. This investigation presents pole figures for magnesium and two of its alloys, in which differences of some magnitude will be shown. Schmid and Wassermann have considered the texture of magnesium in analogy with that of zinc—also a hexagonal lattice. Whereas the zinc texture is said to be derived primarily through basal slip and secondarily through {IO2}† twinning, the {102} twinning is considered impossible at the later stages of the rolling in magnesium because of its smaller axial ratio. This state of affairs appears reasonable for pure magnesium, but for alloy textures the situation is more complex. A double orientation similar to that found in zinc has been reported by J. D. Hanawalt,4 and the addition of small amounts of calcium to magnesium and its alloys to produce a double texture was noted by J. C. McDonald.5 The pole figures of this investigation, using an improved X-ray technique, show these various textures. The dependence of directional properties of rolled sheet on modifications of texture is well recognized. Correlation of physical properties with existing texture should be even more significant if quantitative valuations are attached to the various areas on the pole figures. Such a quantitative technique is developed herein. Experimental Method Two alloys were used, besides high-purity magnesium. In each case, the metal was extruded to bars 1/2 in. thick and hot-rolled to a thickness of about 0.075 in. It had been established previously that such a reduction was more than sufficient to eliminate the extruded structure. The rolling proceeded in the same direction as that of the extrusion, without any cross rolling. The temperatures corresponded to normal commercial practice, averaging around 600°F. A unique method of preparing the sample was developed in this work. Instead of using a flat specimen, a stem of the metal was cut out of the rolled sheet in the desired direction (rolling direction) as shown in Fig. I. From a sheet of 0.075 to 0.065-in. gauge, the stem was cut to a square cross section with a jeweler's saw, rounded with a file and polishing paper to a diameter of 0.060 in. and evenly etched in dilute hydrochloric acid to a diameter of 0.038 + 0.001 in. In this way, a cylinder of the original sheet with its axis in the desired direction was produced. By using this type of specimen for the pin-point pictures, any variance in the absorption of the diffracted beam at the various angular settings of the specimen, was completely eliminated.*

Jan 1, 1942