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The St. Lawrence Seaway and power project has received the support of the Canadian Parliament, with the House of Commons approving a bill that authorizes the Government to proceed with construction of the seaway, with or without U. S. cooperation. Itogan Mining Co., third largest gold mine in the Philippines, reopened in December under the management of Marsman and. Co. The 'mine was almost totally destroyed during the occupation. The International Materials Conference committee on copper, lead, and zinc has recommended against stockpiling during the: first quarter of 1952 because of the current demands for defense needs. The General Services Administration has told producers who have contracts calling for delivery of copper to the stockpile during the first quarter of 1952 that they do not need to make those deliveries.

Jan 1, 1952

By Horace V. Winchell

The St. Helens mining-district, indicated in sketch-map, Fig. 1, is chiefly in Townships 9 and 10 North, Ranges 5 and 6 East of the Willamette meridian, in Skamania county, Wash. There is no railroad or even a wagon-road at present connecting it with any base of supplies; access is usually by wagon-road for about 50 miles from the town of Castle Rock to Spirit lake, and from that point by pony-trail from 6 to 10 miles farther. History. Nearly 20 years ago two German farmers, totally inexperienced in prospecting, penetrated this region upon a hunting-and fishing-trip. Their attention was drawn to numerous joints and crevices filled with black, glistening tourmaline, and con-

Jan 1, 1913

By M. T. Worley

This paper reports investigative work conducted to develop a method of estimating the groundwater influx from a homogeneous permeable formation into a vertical mine shaft during sinking. A method of analysis was developed using data obtained from pumping tests and a modification of the Theis non-equilibrium interpretation technique. Excess influx of groundwater into mine shafts has long been one of the more important problems encountered in the development of a mining property. Much work has been done on methods of preventing such influx and on pumping schemes to control inflow if preventive measures fail. The fundamental aspects of the problem, on the other hand, seem to have been neglected. The purpose of this paper is to review the fundamentals of groundwater flow and to propose a rapid method of analyzing hydrologic data in order to estimate influx from a homogeneous permeable formation into a mine shaft. Such an estimate of the quantity of water to be encountered is of value in planning grouting, pumping and other programs designed to control that influx. It is emphasized that the proposed method of analysis should be regarded only as a tool to be used in evaluating the problem before investing the capital necessary to begin development of a property. FUNDAMENTALS OF GROUNDWATER FLOW In order to effectively approach the problem of estimating influx into a mine shaft, a knowledge of the fundamentals of fluid flow through a porous medium is necessary. Darcy, in 1856, developed an empirical relationship to explain the flow of water through sand filters. This relationship V = k (dh/dl), is the basis for all other flow formulae. It has been shown that Darcy's relation is a solution of the Laplace equation and thus is analagous to other natural phenomena such as heat flow. Theis, using the analogy of heat flow by conduction, developed an expression for determining the transient or time-dependent groundwater flow through a homogeneous, isotropic medium. The resulting equation Was also derived by Jacob using hydrologic considerations alone.' The individual terms in the equation are described in Table I. It is important to understand the assumptions upon which this equation is based. 1) The medium through which the fluid flows is infinite in areal extent, homogeneous and isotropic. 2) The well into which the fluid discharges completely penetrates the medium. 3) The characteristics of the medium remain constant at all times. 4) The initial pressure surface is horizontal. 5) The confining media are impervious and horizontal. 6) Fluid is removed from storage instantaneously by a decline in pressure. 7) The diameter of the discharge well is infinitesimal with respect to the drainage radius of the medium.

Jan 1, 1962

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Jan 1, 1923

By Herbert H. Kellogg, Hugo Vasquez- Rosas

Recently the long-chain primary amines have been used extensively for the flotation of silicate minerals. The use of amines to float sulphide minerals has been investigated by several authorsl-5-l8 but most of this work has been done with the short-chain (less than six carbon atoms) primary amine compounds or the more expensive secondary, tertiary and quaternary amines. Perhaps the fact that the long-chain amines are good collectors for the common gangue minerals has led investigators to omit them from consideration as collectors for the selective flotation of metallic sulphides. The work reported in this paper was designed to investigate the use of a typical long-chain amine salt, laurylamine hydro-chloride, as a collector for the flotation of galena-sphalerite ores. The results show that laurylamine hydrochloride (LAmHCl), when used in small amounts, is a good collector for the selective flotation of sphalerite and galena from the common gangue minerals. The differential flotation of sphalerite from galena was not accomplished but the amine flotation of sphalerite after the standard xanthate flotation of galena is possible. The experimental work reported herein is not complete enough to be able to say whether amine flotation of lead-zinc ores would prove superior to xanthate flotation, or whether the method is even applicable to a more complex ore than the one used for this work. However, the apparent reagent costs for the flotation operations described in this paper seem to be less than for xanthate flotation. This fact alone should be sufficient to encourage the millman to investigate the use of these amine reagents, especially as these reagents are available on a commercial scale at a reasonable price. This paper has as its secondary purposes to illustrate how contact-angle measurements have aided in this investigation, and to bring forward some evidence concerning the mechanism of the collecting action of primary amines. Contact-angle Tests The contact-angle measurements were made by the method described by del Giudice6 and used in recent work by Taggart and his collaborators.7-9 The mineral specimens for the contact-angle tests were carefully chosen, to avoid cracks and inclusions of other minerals. All specimens were mounted in "transoptic" plastic mounts and the surfaces were cleaned by polishing with levigated alumina on a cloth-coverkd glass polishing wheel. Distilled water was used on the lap during the polishing and at all subsequent steps in the contact-angle tests. The mounted mineral specimens were handled with glass forceps and special care was exercised to prevent exposure of the clean surface to air or any other source of contamination.

Jan 1, 1947

By Herbert H. Kellogg, Hugo Vasquez- Rosas

Recently the long-chain primary amines have been used extensively for the flotation of silicate minerals. The use of amines to float sulphide minerals has been investigated by several authorsl-5-l8 but most of this work has been done with the short-chain (less than six carbon atoms) primary amine compounds or the more expensive secondary, tertiary and quaternary amines. Perhaps the fact that the long-chain amines are good collectors for the common gangue minerals has led investigators to omit them from consideration as collectors for the selective flotation of metallic sulphides. The work reported in this paper was designed to investigate the use of a typical long-chain amine salt, laurylamine hydro-chloride, as a collector for the flotation of galena-sphalerite ores. The results show that laurylamine hydrochloride (LAmHCl), when used in small amounts, is a good collector for the selective flotation of sphalerite and galena from the common gangue minerals. The differential flotation of sphalerite from galena was not accomplished but the amine flotation of sphalerite after the standard xanthate flotation of galena is possible. The experimental work reported herein is not complete enough to be able to say whether amine flotation of lead-zinc ores would prove superior to xanthate flotation, or whether the method is even applicable to a more complex ore than the one used for this work. However, the apparent reagent costs for the flotation operations described in this paper seem to be less than for xanthate flotation. This fact alone should be sufficient to encourage the millman to investigate the use of these amine reagents, especially as these reagents are available on a commercial scale at a reasonable price. This paper has as its secondary purposes to illustrate how contact-angle measurements have aided in this investigation, and to bring forward some evidence concerning the mechanism of the collecting action of primary amines. Contact-angle Tests The contact-angle measurements were made by the method described by del Giudice6 and used in recent work by Taggart and his collaborators.7-9 The mineral specimens for the contact-angle tests were carefully chosen, to avoid cracks and inclusions of other minerals. All specimens were mounted in "transoptic" plastic mounts and the surfaces were cleaned by polishing with levigated alumina on a cloth-coverkd glass polishing wheel. Distilled water was used on the lap during the polishing and at all subsequent steps in the contact-angle tests. The mounted mineral specimens were handled with glass forceps and special care was exercised to prevent exposure of the clean surface to air or any other source of contamination.

Jan 1, 1947

By Henry M. Howe

1. The purpose of the National Research Council as organized for war purposes is twofold, to stimulate those outside its own personnel to conduct researches of importance for winning the war and to carry on such researches through its personnel to a limited extent. How this is done is explained in Section 10. "Research" is used here in a very broad sense, including, for instance, inventing and developing mechanical and physical devices. The need of this work arises from the inevitable concentration of most of the governmental war agencies on the production and transportation of war materials of the types now adopted, as distinguished from devising new kinds of instrumentalities, such as armor, guns, aircraft, and apparatus for detecting, locating, observing, signaling, transporting, and many other military purposes. But it is important that we should devise new agencies. The war came near being won by an invention, the submarine, and its course has been affected greatly by two other inventions, tanks and aircraft. In spite of our numerical superiority victory may well be snatched from us by an invention, if we allow Germany to outstrip us in inventing. Hence the importance of the Council's work in mobilizing and organizing the services of the patriotic civilian experts throughout the country, so as to bring their powers to bear on important war problems and on inventing war devices, as an adjunct to the development work of the regular governmental bodies. 2. Status of the Council.—Though President Wilson's request caused the Council to be created in 1916 by the National Academy of Sciences under its congressional charter; though his executive order of May 11, 1918, directs the heads of "Governmental departments immediately concerned" to "continue to co-operate with it in every way that may be required;" and though the Government has contributed largely to its financial support; it is not a department of the Government but an independent research body, aiming to evolve the necessary mechanism for the novel work of systematic stimulation and guidance of research. Thus the Government, which instigated the creation of the Council, recognizes and collaborates with it, and in part supports it. The Council acts moreover as the Department of Science and Research of the Council of National Defense.

Jan 1, 1919

By Herbert H. Kellogg

RECENTLY the long-chain primary amines have been used extensively for the flotation of silicate minerals. The use of amines to float sulphide minerals has been investigated by several authors1-5,18 but most of this work has been done with the short-chain (less than six carbon atoms) primary amine compounds or the more expensive secondary, tertiary and quaternary amines. Perhaps the fact that the long-chain amines are good collectors for the common gangue minerals has led investigators to omit them from consideration as collectors for the selective flotation of metallic sulphides. The work reported in this paper was designed to investigate the use of a typical long-chain amine salt, lauryl amine hydrochloride, as a collector for the flotation of galena-sphalerite ores. The results show that lauryl amine hydrochloride (LAmHCI), when used in small amounts, is a good collector for the selective flotation of sphalerite and galena from the common gangue minerals. The differential flotation of sphalerite from galena was not accomplished but the amine flotation of sphalerite after the standard xanthate flotation of galena is possible. The experimental work reported herein is not complete enough to be able to say whether amine flotation of lead-zinc ores would prove superior to xanthate flotation, or whether the method is even applicable to a more complex ore than the one used for this work. However, the apparent reagent costs for the flotation operations described in this paper seem to be less than for xanthate flotation. This fact alone should be sufficient to encourage the millman to investigate the use of these amine reagents, especially as these reagents are available on a commercial scale at a reasonable price. This paper has as its secondary purposes to illustrate how contact-angle measurements have aided in this investigation, and to bring forward some evidence concerning the mechanism of the collecting action of primary amines. CONTACT-ANGLE TESTS The contact-angle measurements were made by the method described by del Giudice6 and used in recent work by Taggart and his collaborators.7-9 The mineral specimens for the contact-angle tests were carefully chosen, to avoid cracks and inclusions of other minerals. All specimens were mounted in "transoptic" plastic mounts and the surfaces were cleaned by polishing with levigated alumina on a cloth-covered glass polishing wheel. Distilled water was used on the lap during the polishing and at all subsequent steps in the contact-angle tests. The mounted mineral specimens were handled with glass forceps and special care was exercised to prevent exposure of the dean surface to air or any other source of contamination.

Jan 1, 1945

By F. W. Jessen, C. A. Johnson

The effect of treatment with ferrochrome lignosul-fonate on both sodium and calcium bentonites has been examined. In the early stages of treatment it appears that some base exchange of iron and chromium for sodium may occur with the sodium bentonite. Such exchange appears specific for exchange of sodium ions when the calcium ion concentration represents 40-5.5 per cent of the total exchangeable cations, and when additions of lignosulfonate are less than 1 lb per bbl. Adsorption appears entirely physical above 1 lb per bbl treatment level for all concentrations of calcium studied. Gel strength and plastic viscosity of both calcium and sodium bentonite systems were reduced with treatments of ferrochrome lignosulfonate up to 2 Ib per bbl, the greatest reduction occurring within a range of calcium concentration of 40-5.5 per cent of the total exchange capacity of the clay. INTRODUCTION The problem of control of viscosity and gel strength of drilling fluids by the action of thinners or dispersants has been studied by many investigators.1-7 In addition, much work has been done on formation of gel structure in clay suspensions. However, gel formation and structure still are incompletely understood, and the use of the various dispersing chemicals is based, to a large extent, on data almost entirely empirical in nature. In recent years the lignosulfonates have become increasingly important in the treatment and control of drilling fluids. More specifically, ferrochrome lignosulfonate has found rather wide acceptance, particularly in calcium systems.5-7 Lignosulfonates are refined lignin products made from spent sulfite liquor from which the fermentable sugars have been removed.15 The exact structure of lignin is not known; however, it is believed to be a phenolic propane type polymer which may exist as a branched chain or cross linked structure. The molecular weights of lignosulfonates probably range from 300 to 100,000 or more.15 A better understanding of the mechanism of adsorption of dispersants is essential before improvement and development of characteristics of drilling fluids and drilling fluid control is possible. This investigation was undertaken to determine the action of ferrochrome lignosulfonate on sodium and calcium montmOrillonite' LABORATORY INVESTIGATION A Stormer viscosimeter and Fann V-G meter were used to measure viscosity and gel strength. A Zeiss spectrophotometer was used for analysis of Fe and Cr and the flame attachment was employed in the analysis of Na, Ca and Mg. A General Electric X-ray diffraction unit utilizing Copper Ka radiation and a Ni-filter was utilized in the X-ray studies. PROCEDURE Two systems were studied. Predominately sodium clay, obtained from Wyoming, and a predominately calcium clay from Texas were used. These particular samples were chosen because of the extensive work of characterization completed by Mungan. Ionic base exchange capacity determined by flame photometry and total exchange capacity by the Kjehldahl method were obtained experimentally. A 7-per cent suspension of the sodium clay and a 20-per cent suspension of the calcium clay in distilled water were prepared by mixing with a high-speed mixer. The suspensions were allowed to stand for two weeks for complete hydration. Calcium chloride was added to portions of the sodium and calcium cla suspensions to obtain suspensions varying in Ca++ concentration as shown in Table I. A series of treatments was run with 500-ml portions of the original suspensions using a ferrochrome lignosulfonate. Treatment was carried out in the same way with each of the suspensions of varying Ca concentration. Viscosity and gel strength were measured and a filtrate obtained at each treatment level. Ten ml of filtrate were diluted to 50 ml, and aliquot portions of the 50 ml were taken for the Na, Ca, and Mg analysis by the flame photometer. The pH of these filtrates ranged from 7 to 7.3. Standard

The Molycorp operation at Mountain Pass, California, is unique in that it is the only place in the world where bastnasite is mined. The orebody is a metamorphic carbonatite; the mineral of importance is bastnasite, a fluocarbonate containing principally cerium, lanthanum, neodymium, and praseodymium, with small amounts of samarium, gadolinium, and europium. In addition, appreciable quantities of barite, calcite, and strontianite are present. Molycorp had mined and processed the bastnasite ore since the early 1950s at a rate of about 100 tpd by a unique hot flotation process in a plant originally used for cyanidation of gold ore. The concentrate was primarily used in high quality glass polishing, lighter flints, ceramics, and in specialty steel making. Then in the early 1960s, Molycorp and the Colorado School of Mines Research Foundation developed a solvent extraction process to recover europium from the bulk rare earth concentrates. In 1965 a new SX plant was constructed to produce this material for use as a red phosphor in color television tubes. Because of the demand for this material, a new 500 tpd concentrator was designed and constructed in 9 ½ months. Then, because of a sharply increased demand for europium, the plant was expanded to 1200 tpd only four months after completion of the original construction. The crushing section of the new plant was designed similarly to those portable units used in road construction and arrived on the site in ten major pieces. Foundations were concrete piers; and after their completion, the entire crushing plant composed of primary and secondary crushers, conveyors, and a screen was erected in fourteen days by a crew of ten men assisted by a mobile crane. Pit-run ore is loaded into 35-ton trucks by a 7 yd (5.4 cu m) loader, trans- ported to .the crushing plant, and dumped into the 65 -ton concrete pocket. A 42 in. by 20 ft (1.07 m by 6. 1 m) apron feeder feeds ore to the 30 in. by 42 in. (760 rnrn by 1070 mm) single toggle jaw crusher. Crushed ore is trans- ferred by a scissors conveyor to a 5 ft by 14 ft (1.52 m by 4. 27 m) double- deck screen which produces a final ¾ in. (19 rnrn) product with the oversize being treated in a 4 ¼ ft (1. 3 m) standard cone crusher. Cone crusher product is returned to the first scissors conveyor to join the primary crusher product. Dust collection is by a wet scrubber, and an operator's control room is located to overlook the primary. The entire crushing is in the open, and a 30-ton mobile crane is used for maintenance. Molycorp’s two-stage crushing plant is an excellent example of functional design for a small mining and milling operation.

Jan 1, 1978

By Rossiter Raymond

JOHN BIRKINBINE was born Nov. 16, 1844, at Reading, Pa., the eldest son of H. P. M. Birkinbine, widely known as a hydraulic engineer. The family removed subsequently to Philadelphia, where, as a young man he established with his father the office now continued by his sons, after more than 60 years. His education was received at public schools, the Friends' High School in Philadelphia, the Hill School at Pottstown, Pa., and the Polytechnic College of Pennsylvania, where his studies were interrupted in 1863-4 by service in the Union Army, which included participation in the battles at and around Gettysburg. Later, he devoted two years to work in a machine shop; and subsequently he became associated with the late P. L. Weimer, under the firm. name of Weimer & Birkinbine, operating the Weimer Machine Works at Lebanon, Pa. Much of his work was in mining, metallurgy, and blast-furnace construction. As manager for the South Mountain Mining & Iron Co. he carried on experiments with various fuels for iron-ore smelting while maintaining the furnace in constant operation. The carefully recorded results obtained were widely published, and are referred to in text-books by other metallurgists as most complete. From his Philadelphia office he was sent to nearly every State, and to Canada and Mexico, for examinations, reports, constructions or improvements in iron-ore mines, blast furnaces, iron works, water supplies, hydraulic development, irrigation projects, etc., and his engineering knowledge was requisitioned by several European corporations. A number of business trips were made to Mexico, beginning with a visit to the Cerro de Mercado at Durango, before railroads were established in that portion of Mexico, to make a critical examination and report on this "Iron Mountain." Later visits covered other localities and engineering problems, familiarizing him with the major part of the iron industry in Mexico. The late disturbed political conditions in that Republic have retarded the probable enlargement, modernization, and improvement of much of the iron and steel industry of Mexico, upon which he investigated and reported for various capitalists on both continents. One interesting subject included in these reports was a proposed electric furnace, to be operated by energy from water power.

Jan 7, 1915

One of the newest and most modern surface mining operations in the East is gathering steam at Mapco Inc.'s Martiki mine in anticipation of yielding 2.7 million tons (3 million st) of coal annually.

Jan 10, 1977

By R. E. Hucko

Introduction The principal thrust of the US Department of Energy (DOE) coal preparation R&D program is to develop technology to reduce ash and sulfur content of US coals to levels where the resultant product can be formulated into a high quality solid or slurry fuel that could replace oil or natural gas in both new and retrofit applications. The coal preparation program is implemented by the Pittsburgh Energy Technology Center (PETC) and is conducted both in house and by a cross section of industrial organizations, universities, and national laboratories. Research is subdivided into three areas - coal characterization, beneficiation, and ancillary unit operations.

Jan 1, 1985

By Elwood Haynes

As in organic nature certain animal and vegetable forms have undergone modifications, and thus, as it were, fitted themselves to live in a new environment, so it has been found possible in certain instances to form new metallic combinations which are practically immune to the natural conditions that exist on the earth at the present time. A few of the metals, such as gold, silver, and the metals of the platinum group, are found native, but the commoner heavy metals are nearly always found in the form of oxides or sulphides. For a number of years I have made experiments with a view to finding certain metallic combinations or alloys which would not only resist oxidation and other harmful influences, but would also possess valuable physical properties, which would render them fit for special service. The first decisive step made in this direction was the discovery of an alloy of nickel and chromium in 1898. The properties of this alloy have already been described in a previous paper.' Immediately following the discovery of the nickel-chromium alloy, I produced an alloy of cobalt and chromium, which has likewise been described in the reference given, but the range of proportion between the cobalt and chromium is so great, and the combination is modified to such a marked degree by the introduction of other substances, that I have felt justified in reading another paper on this subject, describing more fully my researches in this particular direction. As early as 1907 and 1908,I made alloys or combinations of cobalt, chromium, and tungsten; cobalt, chromium, and molyb-

Jan 1, 1913

By John M. Logan, John Handin

Quasi-dynamic triaxial compression tests have been done for the first time at confining pressures to 7 kb. The intermediate strain-rate apparatus employs a gas loading cylinder which allows axial strain rates up to 102/sec on a sample 2 cm in diameter and 4 cm long. Samples can be deformed at confining pressures to 7 kb. Strain gages bonded to the loading piston and to the jacketed specimen allow internal measurements of load and sample strains respectively. Westerly granite has been deformed at confining pressures to 7 kb, room temperature, and axial strain rates of 10-2 to 1/sec. An increase of ultimate strength with confining pressure was found as expected. The ultimate strength was also found to vary directly with increasing strain rate; the rate of rise increases with confining pressure. Brittle deformation has dominated the sample behavior. Solenhofen limestone has been deformed at confining pressures to 3 kb, room temperature, and axial strain rates of 10- to 10/sec. The brittle-ductile transition was found to take place at about 1.5 kb confining pressure at a strain rate of 10/sec.

Jan 1, 1971

By Anthony Tuke

Members of the Society of Mining Engineers may well regard it as rather unusual that a paper on this subject is being presented by someone whose first taste of mining came at the age of 60 or so - someone who last heard of cathodes and anodes in 1938. On the other hand, the title does refer to the financing of a mine and at least I can claim to have spent all my business life since the war until 1981 in the world of banking, though this inevitably means that I have been used to looking at these and other problems through what you might regard as the wrong end of the telescope. The lending of money, and more particularly the provision of finance for commerce and industry, is the central job of a banker and I have been involved in this in various ways over many years, but regrettably only very marginally in the world of mining. As you will see from what follows, the rather specialised form of finance which RTZ required was, to my regret, not provided by the British banking community since the great majority of the finance came from American banks and, to a lesser extent, from German banks. I am most indebted to Mr. Roy Wright for a great deal of the nuts and bolts in this paper. He was one of the three central figures in the growth and expansion of RTZ during the 1950's and 1960's and was right at the centre of the negotiations with bankers, with governments and with many others. The going, as you will see, was far from easy. The essential basis for the financing of each of the RTZ group's mining projects was a firm long-term sales contract for sufficient of the output of the particular mine to produce the cash flow necessary to service the loans. Wherever possible, loans were raised in the same currency as the sales contracts were made. Each sales contract was designed to give the customer the product he wanted with a long-term assurance of supply and at the same time to give the bankers the protection they required. Thus the marketing concept and the financing concept for a particular mine formed one overall plan, and talks with the customers and the bankers were conducted in parallel until a satisfactory marketing/financial package was agreed in principle. Preliminary talks were begun soon after the discovery of a potentially viable orebody. As confidence about a discovery increased, customers were persuaded to enter into contingent sales contracts before the very detailed and costly business of the economic and technical feasibility study of the mine was launched; such a study might cost 10% or more of the estimated total capital cost. At the same time provisional understandings were reached with the bankers. The contingent sales contracts usually gave a period of grace of eighteen months to two years, during which time the decision whether or not to continue with the mine had to be made. This decision rested mainly on the result of the feasibility study and also on coming to a firm agreement with the bankers. If all went well and the mine went ahead, then the contingent sales contracts became firm, but they fell away if the decision was negative. The Company was fortunate that during the whole period when its major mines were being developed, world trade was increasing rapidly and Japan was becoming a dominant industrial power. The Japanese supported many of the mines, including Hamersley Iron Ore, Lornex Copper, Bougainville Copper to name a few, with the basic long-term sales contracts that enabled their development. The Germans supported Palabora and to a lesser extent Bougainville. The mines were financed as individual projects generally with a loan/equity ratio of about 65/35, without legal recourse to RTZ for the loans. RTZ was, however, responsible for providing any capital overruns required to bring the mines into commercial operations. Nevertheless, the RTZ management regarded itself as morally responsible to the lenders because, Palabora aside, the sales contracts had either a fixed selling price (like Hamersley), an indexed price (like the Elliot Lake Uranium Mines and Mary Kathleen), or a floor price (as in Lornex, Bougainville and Rossing). Thus the Company believed that any financial failure would have been due to poor management or technical

Jan 1, 1985

By D. R. Miller

Internal friction and elastic modulus variations in electrorefined titanium, iodide refined titanium, and alloys of the latter material with oxygen, nitrogen, aluminum, and zirconium were investigated. No oxygen peak was detected with electrorefined titanium but, provided precautions were taken to prevent increases in background damping, an oxygen peak at about 410°C could be resolved with each of the other materials. An additional partially resolved peak was observed at 500°C in a Ti-N alloy. An anomaly in the variation of rigidity modulus with temperature was observed. Possible mechanisms for the formation of any oxygen peak have been discussed. PRATT, Bratina, and Chalmersl investigated the internal friction of commercial purity titanium and alloys of this material containing 1.5, 3.5, and 4.5 at. pct O. With commercial titanium the internal friction curve consisted of two components, a background which increased steadily with temperature and a peak at about 600" C which was due to grain boundary relaxation. In the Ti-O alloys, however, an additional internal friction peak was observed at 430" to 450°C and, since this peak increased in height as the oxygen content was increased, it was thought to be associated with the presence of oxygen. The diffusion of oxygen in titanium at temperatures between 300" and 500° C is believed to have marked effects in its tensile properties2'3 and the present internal friction measurements were undertaken to obtain further information on this diffusion, using material of higher purity than that of Pratt et d. and an apparatus of very much greater sensitivity. In the course of the investigation a number of important limitations on the work of Pratt et al. were revealed and results have been obtained which emphasize the need for ensuring that in this type of experiment, internal friction is independent of strain amplitude and that the values obtained are reproducible. 1) MATERIALS AND APPARATUS The basis material from which the majority of the specimens was prepared was iodide-refined titanium, the major impurities in which were oxygen and nitrogen—the metallic impurities being present at concentrations less than 0.001 at. pct. The hardness of this material after arc melting, forging, and swaging to rods 1/4 in. diameter was Dph = 110. Specimens 10 in. long and 0.020 in. (0.51 mm) diameter were prepared from these rods by further swaging and wire drawing and were finally annealed in vacuo (5 x 10-6 mmHg) for 24 hr at 800°C. The oxygen alloys were prepared from iodide-

Jan 1, 1962

By W. C. Hagel, J. H. Westbrook

Usittg a sectioning technique with Agl10 as the tracer, the diffusion of silver in silver-excess (45.8 at. pct Mg), near-stoichiometric (49.8 at. pct Mg), and magnesium-excess (52.0 at. pct Mg) cylinders of CsCl-type AgMg was determined from 500" to 700°C. Diffusion coefficients conform to the expression D = Do exp (-q/RT) where the respective Do values are 1.53, 0.280, and 0.134 sq cm sec-I and the Q values are 41.3, 40.6, and 38.0 kcal g-atom-'. Lnttice-parameter and density measurements were performed on a more numerous assortment and wider range of compositions. Substitutional defects were found on both sides of stoichiometry. Activation energies for other rate processes in these alloys show related trends with changing composition, although silver may not be the rate-detemining species. KNOWLEDGE of diffusion coefficients is necessary for a quantitative understanding of the many rate processes (e.g., grain growth, precipitation, sintering, oxidation, or mechanical deformation) occurring in solids. Although these data are available for most metals and common alloys, they are quite limited for intermetallic compounds—a group of materials whose unique physical and mechanical properties are presently attracting great interest. From a fundamental viewpoint, diffusion in intermetallic compounds also offers several engaging aspects owing to: their ordering, the possibility of introducing large, stable concentrations of lattice defects, and the variety of bonding types and crystal structures which can be found. In the case of CsC1-type compounds, some previous work has been directed at examining the role of vacancy defects by changing their concentration compositionally. The diffusion of Co60 was measured in 0 NiAl1- and in P COA., Except for the results of Smoluchowski and Burgess, isothermal diffusion coefficients were found to pass through a minimum at the stoichiometric composi- they decreased sharply on what was reported by Bradley and co-wrkers' to be the vacancy-rich (aluminum excess) side of stoichiometry. This investigation of the diffusion of Agl110 in AgMg was undertaken both as an adjunct to a concurrent study of its deformation behavior and for the purpose of obtaining information on the influence of lattice defects and temperature on diffusion in another CsC1-type intermetallic compound. Bcc AgMg remains ordered up to and melts congruently at 820°C. Solubility limits at 300°C are about 41 at. pct Mg and 53 at. pct Mg. It is one of the Hume-Rothery electron compounds with a 3/2 electron-atom ratio. Previous investigations of its properties include hardress,' tenile,'-' electrical reistivity, and thermodyna-mic1',14 studies. Indications of a high bonding strength may be found in the large heat of mixing1' and in the 6-pct vol contraction on compound formaticp, as calculated using atomic radii of l.40 and l.55a for Ag and Mg. EXPERIMENTAL PROCEDURE Alloys were prepared by the induction melting of selected fine silver (99.95) and low-iron magnesium (99.95) in magnesia crucibles under 1 atm of A. Supplied by the Handy and Harmon and Dow Chemical Cos., respectivelv. Melts were poured under argon into graphite molds providing 1 1/8-in.-diarn. by 4-in.-long ingots. These were homogenized in evacuated and argon-filled fused-silica capsules by heating for 16 hr at 750'. Three 1 in.-diam. by 3/4-in.-long cylinders were machined from the mid-portion of each ingot for diffusion measurements. Three alloys, analyzing 45.8, 49.8, and 52.0 at. pct Mg were taken as representing the extremes of interest, with 49.8 at. pct Mg being very close to the stoichiometric composition of 50.0 at. pct Mg.

Jan 1, 1962

By L. W. Bahney

Frequently in using a thermo-electric pyrorneter for measuring the temperature of a furnace, a hole is drilled at the back or side of the furnace, through which is introduced the tube containing the thermo-couple. At times the couple is left almost where it drops, for the reason that it soon becomes too hot to be handled easily, and the space at the back or side of the furnace may be so small and uncomfortably hot that an easy and accurate adjustment is nearly impossible. In order to overcome this clumsy and unscientific method of using the thermo-electric pyrorneter, I designed an adjustable stand, to hold the clay or quartz tube inclosing the platinum and platinum-rhodium leads that constitute the couple of the Le Chate-lier thermo-electric pyrometer. This stand also allows an easy and rapid adjustment of position to varying heights and angles, as may be desired for special reading, This stand is illustrated in Fig. 1. The couple in the tube might be of better service if the tube were held a little higher above the charge in a roasting-dish, changing the height and angle if desired. The stand, made of 1.5-in. water-pipe and mounted on casters, is heavy enough so it cannot be tipped over easily. It is adjusted to any position, and has a universal clamp which holds the clay or quartz protecting-tube. To avoid disturbing the wires of the couple at the cold junction each time the tube is moved, the cooling-bottle sets in a wire basket so placed that it moves forward or back with the couple. To overcome the necessity of leveling and adjusting a galvanometer at each furnace, a switch-board is used to connect

Jan 1, 1910

By R. K. Ham, M. L. Wayman

TD-Nickel has been broken in tension and in fatigue at voom temperature. Rod specimens failed in tension by necking, with axial cracks attributed to voids elongated in the extrusion direction. Fatigue specimens failed in shear. Thin-film electron microscopy showed that the subgrain structure of TD-Nickel was very stable, and that particle-matrix detachment was very difficult, in tension and fatigue. TD-Nickel softened slightly during fatigue but had a high fatigue ratio (0.5at 10' cycles). Fractography suggested that Stage I fatigue crack propagation is greatly extended in TD-Nickel. Td-NICKEL* is a dispersion of 2 pct by volume of thoria (ThO2) in nickel, produced by powder-metallurgical methods including compaction, sintering, and extrusion. The spherical thoria particles, which may have a mean diameter of a few hundred angstroms, are dispersed with a mean planar spacing of a few thousand angstroms. By a combination of cold working and annealing, a subgrain or cell structure of dislocations intimately associated with the dispersion can be produced.' This gives the material useful tensile properties which are extremely resistant to exposure to high temperatures.'-= At the same time, the material shows considerable ductility.3'4 At the beginning of the present work, it was considered of great interest to investigate the mechanical stability of TD-Nickel under conditions of fatigue. On the one hand, materials which derive strength from a cold-worked structure are unstable in that they are susceptible to fatigue softening: in addition, the presence of discontinuities such as the particle-matrix interfaces might be expected to assist in the initiation and propagation of fatigue cracks, in that they may provide local concentrations of internal stress and sites for the initiation of voids." On the other hand, the substantial ductility of TD-Nickel suggests that if it obeys Coffin's relation8 (or the more refined form proposed by Manson9) it should have good fatigue resistance. The initial purpose of this investigation was to assess the importance of these factors. Also, relatively little fundamental work has been done on the mechanism of fatigue in dispersion-strengthened materials. Work on overaged A1-4 pct CU10-12 revealed a very large Bauschinger effect indicative of internal stresses at the particles, and very great fatigue hardening1' presumably due to the multiple slip stimulated by these internal stresses, followed by softening which was initially due to softening in the matrix, but later might have arisen from cracking at the particle-matrix interfaces. The study of overaged Al-4 pct Cu could not settle this latter point by the electron microscopy of thin films, since the dispersion is too coarse. A previous study of the fatigue of internally oxidized copper13 was complicated by inter granular failure, attributed to oxide particles at grain bouhdaries; internal oxidation of single crystals, however, improved their fatigue properties.'3 Investigations of SAP (sintered aluminum powder) are complicated by the complex particle shapes, and the possibility of continuous internal oxide films.14 It was hoped to avoid these difficulties with TD-Nickel, which had the further advantages that it was commercially available and suitable for study by the thin-film technique. 1) MATERIALS AND EXPERIMENTAL PROCEDURE TD-Nickel was purchased from the Driver-Harris Co. as 3/9-in.-diam rod which had been extruded, swaged, and "stress-relieved" (normally at 1010°C for 1 hr). Continuous-radius fatigue specimens with a minimum diameter of -0.1 in. were ground to shape and electropolished in 40 pct phosphoric, 35 pct sul-furic, 25 pct water at 25oC, with a stainless-steel cathode, at -6 v. Fatigue tests were carried out at room temperature with a Sonntag SF-1-U machine operating in push-pull at 1800 cycles per min, and in an Instron TT-C-L modified for reversed stressing at 26 cycles per min as described elsewhere.10 Round tensile specimens were ground with 0.85-in. gage lengths of 0.135 in, diam, electropolished, and tested in a Tinius Olsen hydraulic machine. The surfaces of fatigue specimens were examined with a Reichert metallograph. Discs for electron microscopy with a Siemens Elmiskop I were spark-cut 0.01 in. thick with a modified Servomet 11 employing a tool of moving molybdenum wire, cleaned in 50 pct acetic, 30 pct nitric, 10 pct phosphoric, and 10pctsul-furic at 85oC, and thinned by the window method in the electropolishing solution at -20°C and -6 v. Two-stage replicas (parlodion, then Pt-50 pct C self-shadowed at 40 deg) were taken from fatigue fracture surfaces for electron microscopy. Plane sections parallel to the specimen axis and containing the direction of fatigue crack propagation were polished, etched with Carapella's reagent, and examined optically. Transmission Laue X-ray photographs of as-received material electropolished to a point were used to determine preferred orientation. 2) RESULTS 2.1) The Structure of As-Received Material. Grains -1 µ diam and elongated 20 to 30 u in the direction of the rod axis were observed, With' elongated "intergran-ular" voids (-4 p diam and -90 µ long and identified as such using longitudinal and transverse sections and

Jan 1, 1968