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By Charles W. Huggins

Electron diffraction and electron microscopy were used to determine the unit cell parameters of garnierite [(Ni,Mg)3 Si2O5 (OH)4] and to examine its crystal habit. Bundles of ribbons, many less than 200 A. in cross section, make up the bulk specimen of the garnierite Electron diffraction revealed the unit cell to be monoclinic. Unit cell parameters were: a, 5.33 A,; b, 9.23 A.; c, 14.96 A.; and ß, 94°441.

Jan 1, 1961

By M. E. Wadsworth, C. H. Pitt

Nickel corrosion in sulfuric acid solutions at elevated temperatures and oxygen wer-pressures was imestigated. Weight loss was 1inear with time and varied directly with oxygen concentration. Independent variation of the possible active species in solution indicated that the undissociated sulfuric acid molecule plays an important part in the corrosion mechanism. The rate determining step was considered to be the adsorption of oxygen on a site containing adsorbed H2SO4. THE tendency for a metal to go into solution depends on a number of factors some of which are: 1) the position of the metal in the electrochemical series; 2) the type and concentration of corroding species in solution; 3) the concentration of oxygen in solution; 4) the type of film formed at the liquid-metal interface; and 5) the physical state of the metal. The corrosion of a metal in an aqueous solution may be considered to be a heterogeneous reaction that occurs at the liquid-metal interface. The reaction is generally considered to occur as a result of electrochemical potential differences within the system. Little work has been published in the literature concerning the corrosion of pure nickel. A great deal has been publistled dealing with the experimental and theoretical aspects of the over-all corrosion process. Evans,1 Uhlig,' and recently Todt 3 and Tomashoff,4 have published books which review the results of experiments which have been conducted on corrosion, and have developed some of the basic ideas of the more widely accepted theories of corrosion. Friend5 states that. nickel does not readily discharge hydrogen from any of the common nonoxidiz-ing acids and that a supply of some oxidizing agent is necessary for appreciable rates of corrosion. He further notes that at temperatures between atmospheric and close to boiling, corrosion rates tend to vary with concentration, temperature, and aeration in acid concentrations up to 25 pct. Whitman and Russel6 studied the effect of dissolved oxygen on a number of metals in acid solutions and found that oxygen accelerates the rate of corrosion of nickel in sulfuric acid. Flowers and Kelley7 in studying the action of dissolved CO, on electroplated nickel postulated that nickel dissolves as NiHCO3 in the presence of CO, and air. It was found that oxygen was necessary for corrosion to take place and that the rate increased with increasing amounts of oxygen in solution. Flowers and Kelley attributed the oxygen effect to cathodic depolarization. MacGillavry, Rosenbaum, and wensson' determined metal solution potentials of nickel in various electrolytes. They found that nickel has no tendency to corrode in alkaline solutions in the presence or absence of air. In acid solutions in the presence of air, metal solution potential increases in the order of 1/2 v were observed. This increase was attributed to probable chemisorption of oxygen on the nickel surface and the corrosion mechanism suggested was the interaction of H+ ions with the nickel oxide formed at the surface. Delahay9 observed the reduction of oxygen on various metals. A polarograph was used to measure the course of the reaction. With some metals hydrogen peroxide was produced as an intermediate compound. However, nickel was not considered to be a hdrogen peroxide producer. Van Rysselberghe 10,11 and associates attributed the accelerating effect of carbon dioxide on the corrosion process to the presence of percarbonic acid produced in solution reacting with the hydrogen peroxide. The percarbonic acid can be reduced at less negative potentials than hydrogen peroxide and as a result accelerates the reaction. EXPERIMENTAL Since a complete description of the apparatus used can be obtained elsewhere,12'13 no attempt will be made here to describe the equipment other than to note that it consisted essentially of an autoclave unit from which samples could be withdrawn periodically without disturbing the interior state of the autoclave. A titanium autoclave liner was used to protect the autoclave from the solution.

Jan 1, 1961

By Nicholas J. Grant, Rolf Nordheim, Thomas B. King

Constant-load creep-rupture tests were conducted in an argon atmosphere at temperatures of 1600 to 2200°F on two heats of iron containing about 0.06 and 0.09 pct P in solid solution. The tests were conducted in the as-cast condition. Stresses were selected to give strain rates approaching those encountered in the hot working of steel, and within the limits of the creep-rupture test apparatus, namely. from about 0.001 to 50 pct per sec. FOR generations, rolling and forging practices have been developed largely by empirical methods, based on prior experience. While largely successful, difficulties are frequently encountered when new or different alloy compositions are tried for the first time. There is need to know the relationships which exist among temperature, strain rate, composition, and other variables on the deformation and fracture characteristics of steels. It has been shown for aluminum and several high-temperature alloys that the deformation and fracture characteristics follow rather well-defined laws and patterns which are closely related to the effects of strain rate, temperature, and composition.1"3 As the melting temperature of aluminum or its alloys was approached, it was possible to study the interplay of work-hardening factors and recovery or recrystal-lization, the latter resulting in improved ductility and increased resistance to intercrystalline fracture. In particular, the effects of composition are very poorly known. Within the meaning of "composition" should be included impurity elements, such as sulfur, phosphorous, lead, copper, and many others, as well as those elements which are added for alloying purposes in iron. The role of multiphase structures, in contrast to solid solutions, should also be studied in much greater detail. high strain rate creep-rupture tests would provide information regarding the deformation and fracture characteristics of metals at hot-working temperatures. It was also desired to establish the stresses which are necessary to accomplish the desired deformation, and to relate these to the strain rate and temperature. Secondly, it was the purpose of this particular study to determine the effects of phosphorus, within solid solution limits, on the deformation and fracture characteristics of iron at hot-working temperatures. EXPERIMENTAL PROCEDURE Two phosphorus levels were selected, one corresponding to the upper limit normally found for commercial steels, and one substantially higher than this, but within the region of solid solubility at the test temperatures chosen for this investigation. Twenty-pound heats were prepared by induction melting electrolytic iron in air in a magnesia lined furnace. After deoxidation with about 0.2 pct Al, ferro-phosphorus was added, and the heats were then poured into prefired silica molds. The purpose of using silica molds was to obtain a slow cooling rate during solidification to produce a relatively coarse grain size, producing a structure subject to some segregation and therefore more nearly characteristic of ingot structures. The major part of the casting assembly provided a large shrinkage head in order to produce sound castings and to promote slow cooling of the specimens. The primary austenitic grain size varied from ASTM No. 2 to No. 00. The composition of the heats, including a low phorphorus melt, used for comparison purposes, is shown in Table I. It will be noted that the oxygen content of the phosphorus containing heats is relatively high, in spite of the deoxidation practice, a condition which is difficult to control in small melts. Creep-rupture tests were nevertheless undertaken when it was noted that this quantity of oxygen did not appear to give results any different from those from a heat containing 0.01 pct 0, low phosphorus and comparable carbon Content;4 see Table 11.

Jan 1, 1961

By R. B. Porter, R. P. Porter, R. A. Lothrop

Changes became necessary in dredging methods employed in Idaho through passage of the Dredge Mining Protective Act (1954). Among other provisions, the law requires dredge operators to construct settling ponds of sufficient capacity and character to reasonably clarify the water used in the mining process before such water is discharged into the stream. Porter Bros. Corp., a placer mining company with many years operating experience in Oregon and Montana, became interested in strategic mineral placers in Idaho in 1950 when it was learned that prospectors had discovered a radioactive mineral deposit in Bear Valley Creek, 95 miles northeast of Boise. The company acquired mining leases and proceeded with exploration and development work on the property. After extensive research had resulted in the determination of successful separation processes, contracts were negotiated with the federal government and deliveries of columbium-tantalum and uranium concentrates commenced in 1956. The mining operations are located in a primitive area of Idaho among salmon spawning grounds and crystal-clear mountain trout streams. To avoid involvement in a very controversial issue, it appeared advisable for the company to develop water treatment procedures exceeding those requirements stated in the Idaho Dredge Mining Protective Act. Operation: The company operates one 6 cu ft continuous bucketline dredge and one 4 1/4 cu ft continuous bucketline dredge on the property. The dredges are jig-equipped, with feed being screened to 3 in. by trommels. The screening and gravity concentration methods satisfactorily separate the heavy minerals from companion clays, sand, and gravel. However, this separation of the heavy minerals requires water from the dredge pond with a minimum content of silt and colloids; therefore, water for dilution is added continuously to the dredge pond to suppress solids buildup. Discharge of this highly turbid water to maintain the proper pond level would ultimately result in an excessive silt load in Bear Valley Creek. To prohibit the turbid pond water from flowing directly into Bear Valley Creek, it was necessary to isolate the dredging area. Main by-pass canals were constructed along each side of the dredge pond and numerous secondary canals were dug for diverting seepage and snow runoff. One by-pass canal, extending more than two miles along the west side of the valley, diverts the main stream as well as tributaries entering from the west; a canal east of the dredge area diverts streams entering from that direction. At the beginning of operations in 1956, the dredge pond effluent was filtered through tailings and settled by use of coagulents in a series of lagoons. The filtrate was then discharged directly into the stream. Although this procedure gave satisfactory results in conformance with the state law, ice buildup and lagoon freezing hindered the efficiency of the process during periods of low temperature. For this reason, testing began in 1956 on a water treatment process that would operate efficiently under the extreme weather conditions encountered in Bear Valley. Development of Water Treatment System: Porter Bros. Corp. established the following requirements for effective continuous treatment of dredge pond effluent to the stream which, at low flow conditions, effluent to the stream which, at low flow conditions, would not result in a turbidity exceeding 25 ppm in the stream, 2) produce a sludge sufficiently dense to minimize disposal area requirements, 3) be semi-portable to follow dredge movements, 4) be capable of operating at low temperatures, and 5) be capable of handling a variety of capacities and turbidities.

Jan 1, 1961

The development of Mount Isa Mines Limited power supply is traced through the history of the mine operations. As would be expected, growth of the power supply system follows closely the increase in mine output, although it will be seen that total kWh. produced per ton milled shows a considerable reduction in later years when the mine output showed a more rapid rate of increase. That this reduction is not more marked is possibly due to the increased community and Shire Council power usage per head of population.INTRODUCTIONThe geographical position of Mount lsa, far from any large regional power supply Authority, dictated the policy that the Company be responsible for the production and suppiy of all power required for the plant operation. The Company also, in November 1937, accepted responsibility for the supply of a part of the power requirements of the township of Mount Isa. The history of power supply to the Mine may be divided into several phases.1. The supply Of lighting and power during the first plant construction period 1929-1931.2. The construction of the first section of the Mines Power Station, comprising Nos. 1 and 2 turbo alternators and boilers.3. The addition of No. 3 turbo alternator and boiler.4. The addition of No. 4 turbo alternator and boiler.5. The addition of No. 5 boiler.6. The addition of a. 2 turbo blowers for air supply to the Copper Smelter converters; b. 1 turbo blower for air supply to the L.ead Smelter; c. 2 turbo compressors for compressed air supply to the Mine and surface plant.

Jan 1, 1961

By L. A. Stewart

This is one of a series of reports prepared by the Federal Bureau of Mines on mining methods, performance, and costs at individual mines in the United States. The primary purpose of these papers is to promote development and conservation of our mineral resources by disseminating technological information on methods, practices, and results that may be applied to the engineering analysis and solution of mining problems. This report discusses the highly selective mining methods of the Jaquays Mining Corp. at the Regal asbestos mine, 45 road miles northeast of Globe, Ariz. The milling method at the Globe plant is discussed briefly, and the extraction ratios of the various grades of fiber are tabulated. The proposed flowsheet of a new mill under construction is shown.

Jan 1, 1961

By T. W. Wloder

During recent studies concerning the effects that various surface treatments, surface imperfections, locked-in residual stresses and metallurgical and geometrical notches have upon the mechanical behaviour of metals and, in particular, upon their tension-bending characteristics under impact loads, it became apparent that specially developed methods and samples would be of great assistance in determining the desired data. This paper describes and discusses a number of different types of double-notched tension-bending impact samples which have been considered and examined for this purpose. The types most suitable for exploratory investigations are proposed for application in the study of the _behaviour of metals, their welds, and, in particular, their surfaces, when subjected to various notch-severities, surface imperfections, strain rates, temperatures, and constrained states of stress (i.e. the relations of the three principal stresses). It is expected that the proposed double-notched tension-bending samples and the proposed test methods will also contribute toward further understanding of the cold brittle behaviour and the notch-sensitivities of metals. The possibilities of introducing the so-called impact notch-sensitivity index and relative impact notch sensitivity of metals are discussed. Data obtained on double-

Jan 1, 1961

By S. J. Aresco

The Bureau of Mines has been active in promoting the purchase of coal for Government use under specifications that define the requirements in terms of heating value of the coal, expressed in British thermal units, and the composition as shown by proximate analyses. To these, when required, are added the ash-softening temperature, the free-swelling index, and the Hardgrove grindability index. Under most of these specification contracts the bidders guarantee the quality of the coal, and that guaranteed by the successful bidder becomes the standard of his contract. The deliveries are sampled in accordance with instructions5/ issued by the Bureau of Mines; the samples are analyzed in the Bureau laboratory to determine whether the coal is of the quality guaranteed by the contractor and, if it is not, a price adjustment is made. Analyses of the delivered coal and tipple samples (samples collected at mine tipples as coal is being loaded into railroad cars or trucks) provide valuable data for use in evaluating future bids. In addition, the continuous sampling of coal as delivered is a check on the practical results obtained in burning the coal.

Jan 1, 1961

By S. E. Bronisz, J. O. Brittain

Experiments have been carried out to study the effect of an applied stress on strain aging in steel. It was found that the stress-induced strain aging reaction proceeds rapidly in the temperature range of 0° to 60°C. The variation of stress-induced strain aging with plastic strain, aging time, and temperatures is reported. The activation energy for the stress-induced strain aging was found to be 10,000 cal per mol for the steel used in this investigation. VARIOUS observations1-5 have been made of the influence of an applied stress upon the yielding of iron and steel. However, there have been only cursory studies of the effect of an applied tensile stress upon strain aging in iron and steel1,2 The following represents the results of a preliminary study of strain aging as influenced by the application of an external tensile load during the aging process. For the most part, previous experimental work on strain aging can be classified into two parts. First, the experimental technique involved a direct determination of mechanical properties of a suitable specimen that has been plastically deformed to a constant strain and aged generally at a temperature of the order of 200°C, with the aging times varying from about 1/10 to 2 hr.6-8 The second classification of strain aging experiments involves an indirect determination of strain aging by means of physical property such as electrical resistivity or internal friction as a function of the aging time at a constant temperature and strain.9-12 The latter results have

Jan 1, 1961

By H. J. Oberson, J. H. Brown

Comminution devices such as rod or ball mills are characteristically nonselective in their operation in that all material fed to a mill is ground to some extent. This is unfortunate when the object of comminution is liberation, for not only is energy expended in breaking pure gangue particles wasted, but, since gangue is frequently the predominant phase, the opportunity for such loss is great. Ideally, in this application a comminuting device should develop fracture only in locked particles. In the present investigation an attempt was made to use the large density difference which may exist between minerals to prevent comminution of one while grinding the other. EXPERIMENTAL MATERIALS AND EQUIPMENT The two minerals used in this work were -8-mesh galena and -8+ 20-mesh quartz. All tests were made on 2000-g charges containing 50 pct by weight of each mineral. Heavy media suspensions consisted of -100-mesh ferrosilicon in water. For grinding, a laboratory mill 10 in. diam by 12 in. long was filled to about 30 pct of its volume with either a ball or a rod charge. The balls ranged in size from 3/8 to 1 1/8 in. in diam; the rods ranged from 5/8 to 1 1/4 in. diam by 11 in. long. EXPERIMENTAL PROCEDURE In all tests employing heavy media, the ground pulps were treated as follows: 1) After recovering the ground charge from the mill but before drying, the pulp was wet screened on 200 mesh. 2) After drying the + 200-mesh product from step 1, the ferrosilicon was removed magnetically. 3) The nonmagnetic quartz and galena product from step 2 was sized on 10-mesh through 200-mesh screens. 4) The mineralogical composition of each screen fraction was determined by measuring its specific gravity. The specific gravity was related to the weight of galena in the fraction through the relationship

Jan 1, 1961

By N. H. Coates

As part of a joint program of the U.S. Atomic Energy Commission and the Federal Bureau of Mines for using nuclear energy to supply process heat, the Bureau designed and constructed a pilot-scale simulated nuclear reactor system. Although workable components were developed,5 the simulated nuclear reactor could not be operated continuously at its design conditions of 2,500°F. and 250 p.s.i.g. because the refractory materials used for insulation deteriorated. Replacement of these materials with porous carbon permitted sustained operation at design conditions, and a 1,000-hour demonstration run was completed successfully. No serious operating difficulties developed during the test. Leakage of helium after 1,000 hours was only 3 to 4 std. c.f.h. Inspection after the run revealed no damage to any of the components. Including earlier runs during previous research5 the system has been operated about 4,000 hours, of which 1,120 hours have been at 2,500° F. or higher. The helium-recycle compressor performed satisfactorily with no main¬tenance whatever for 2,445 hours, with about 2,000 hours at 900° to 1,000° F.

Jan 1, 1961

By H. M. Otte

Certain choices for the shear elements of the inhomogeneous distortion in the phenomenological theory of martensite formation are examined for their agreement with crystallographic and X-ray data of iron alloys. The assumption that the shear elements must represent slip or twinning systems characteristic of bcc metals is found to covey all observations, even when a small uniform dilatation is taken into consideration. In bct martensite, (011) becomes a possible twinning or faulting plane, in addition to {112), and qualitatively similar X-ray line broadening is to be expected from both. The basic concept inherent in the current theoriesl-4 of the formation of martensite is that the interface between the parent (austenitic) and product (martensitic) phase is an invariant strain plane (i.e., one that is undistorted and unrotated). Experimental evidence that the interface is of such a nature is available in certain transformations2'5'6 but for the transformation in iron alloys direct observation has not proved enlightening. Internal strains resulting from the formation of the small martensite platelets within the parent austenite matrix7 make it difficult to produce the desired evidence. Indirect evidence, however, such as the continuity of scratches in passing from untrans-formed to a transformed region, strongly indicates that the habit plane in iron alloys is an invariant strain interface. The scatter in habit planes in a given specimen8 would suggest that internal stresses have a slight but definite influence. On the other hand, composition changes which affect the lattice parameter can alter the habit plane appreciably, and by an amount greater than the scatter.' The success of the theories depends on the choice made for the "inhomogeneous distortion" or "complementary shear'' in the analysis and also on the choice for the parameter 6 representing a small uniform dilatation. In the approach developed by Wechsler, Lieberman, and Read'," it is implicitly assumed that 6 is unity. In the case of iron alloys, all observations cannot be explained without varying either the inhomogeneous distortion or 6 . Bowles and Mackenzie3 considered only the effect of varying d. They found it difficult to reconcile the wide scatter of habit planes with the theory and were forced to the conclusion that it may also be necessary to consider variations or different choices of the inhomogeneous distortion. Wechsler and Read" considered a limited number of possible choices for the inhomogeneous distortion, but no variation in 6, though this could easily have been introduced if so desired. It is the purpose of the

Jan 1, 1961

By J. S. Browning

The physical properties and specific gravity ranges of various liquids and salt solutions used for laboratory sink-float separations of rocks or minerals are presented. The test equipment and techniques employed by the Bureau of Mines in making sink-and-float separations of particles as coarse as 3 inches to as fine as 400 mesh are described. Also discussed are methods of recovering and reclaiming the liquids or salts from the minerals and wash solutions, as well as the hazards encountered and precautions to be followed while working with the materials. The laboratory use of various liquids for separating minerals of different specific gravities has been recognized for many years. During this time, laboratory sink-float procedures have proven their utility as a rapid and moderately accurate means for determining the mineral content of ores, test products, and plant products in certain nonmetallic concentrating operations, such as those producing mica, spodumene, kyanite, and so forth. These procedures also have been used as analytical tools for determining the mineral content and associations of other metallic and nonmetallic ores.

Jan 1, 1961

By J. H. Field

Synthesis of hydrocarbons by the Fischer-Tropsch reaction in a hot-gas- recycle system was demonstrated to be technically feasible. This project was undertaken, by the Bureau of Mines, to determine if the system was operable and to ascertain the optimum conditions for the production of gasoline. Carbon steel turnings packed with a void volume from 88 to 90 pct. were satisfactory catalysts, but steel catalysts with greater void volume, either turnings or steel wool, were not as active. Good temperature control with a pressure drop of less than 0.5 pounds per square inch (p.s,i,) per foot of catalyst bed of turnings was obtained by operating with a recycle to fresh feed ratio of 20 and by splitting the total gas flaw and injecting portions into the reactor at different entry ports.

Jan 1, 1961

By A. E. Bibb, F. W. Kunz

A platelet form of zirconium hydride was found in zirconium and ZY-1 wt pct U single crystals containing hydvogen in the range of 50 to 100 ppm. The habit planes for the hydride plateletg in the zirconium crystals were found to be {1012}, {1121}, and (1122) while the habit planes in the ZY-1 wt pct U crystals were {1121), {1123}, and (1.231). With the exception of the {1231} plane, these have been identified as the twin planes in zirconium. The different effect of hydridc on the mechanical puoperlies of zirconium at high and low strain rates has been explained in terms of the defornzation mechanism and the habit planes of the hydride. ZIRCONIUM and zirconium-base alloys are considered for many nuclear reactor applications, where the pick-up of hydrogen is a distinct possibility, if not an unavoidable occurrence. An excellent example of this is the absorption of hydrogen by zirconium and its alloys during aqueous corrosion, where as much as 30 pct of the hydrogen produced by the corrosion reaction is picked up by the metal. Under the proper conditions, the absorbed hydrogen would precipitate as zirconium hydride and consequently alter the mechanical and physical properties of the zirconium-base alloys. The knowledge obtained from a study of the crystallographic aspects of the hydride precipitation is necessary for the interpretation of the observed changes in the mechanical and physical properties. The deleterious effect of hydrogen on zirconium-base materials is not always observed in normal slow tensile loadings at or above room temperature, but becomes immediately obvious under impact loading, where the energy absorbed decreases with increasing hydrogen content,' and in notched specimens where triaxial loadings are attained.2 This effect is of serious consequence in the applications of Zr where shock loads or high strain rates are experienced. The purpose of this investigation was to determine the crystallographic planes of the Zr and Zr-1 wt pct U matrices upon which zirconium hydride will precipitate and to correlate these with the observed mechanical property data. PROCEDURE Crystal Growth—Single crystals of Zr and Zr-1 wt pct U alloy were used in this investigation. The Zr crystals were made from sponge that had a typical analysis as shown in Table I. Large grains were grown in this material by rapid cooling an arc-melted charge in a button furnace. This operation undoubtedly lowered the volatile impurity concentration below those listed in Table I. Back-reflection Laue patterns of these large grains showed the presence of considerable substructure and lattice distortion within each grain. It was found that an 18-day anneal in an argon atmosphere at 840°C (a high a heat-treatment) followed by furnace cooling, resulted in the further growth of the large grains and removed the detectable substructure ana lattice distortion. Equiaxed crystals with a cube edge of approximately 1/4 in. were produced in this manner. Large crystals of Zircaloy-2 (1.5 wt pct Sn, 0.15 wt pct Fe, 0.1 wt pct Cr, 0.05 wt pct Ni) also were produced by this technique but the large amount of substructure formed could not be removed by annealing. The Zr-1 wt pct U solid solution crystals were produced from an alloy rod consisting of Westing-house-Foote hafnium-free crystal bar zirconium and depleted uranium. The chemical analysis of the alloy is also given in Table I. Three-inch sections were cut from an 0.120-in.-diameter alloy rod and tapered to a fine point on each end. The samples were sealed in evacuated Vycor tubes, homogenized for 5 hr at 1000°C in the ß-phase field, and slowly lowered in a gradient furnace into the a phase (800°C), annealed for 60 hr at this temperature to produce grain growth and furnace cooled. This technique produced large grains approximately 1/2 to 3/4 in. long over the entire cross section of the rod, which were free of observable substructure. Metallographic examination up to X1000 did not show the existence of any second phase in these grains. Crystal Orientation—All crystals were abraded on fine emery paper to produce two flat surfaces 90 deg to each other. The crystals were analyzed by the standard Back-Reflection Laue technique to obtain the crystal orientation with respect to the abraded surfaces. The Back-Reflection Laue Photograms of all crystals used were clear and sharp indicating that the crystals were free from any substructure that could be detected by these means. Hydriding—Only samples containing four to five grains were used for hydriding. Samples that exhibited fine grained patches were discarded. The samples were hydrided using the following technique. After etching in 48 vol. pct HNO3, 48 vol. pct H2O, and 4 vol. pct HF (48 pct) solution, the specimens

Jan 1, 1961

By R. E. Ogilvie, N. L. Peterson

Intevdiffusion and intrinsic diffusiorz coefficients were determined in the uranium-niobium system from diffusion couples analyzed with an electron microbeam probe. A Previously unveported intermediate phase, designated in this report as the delta phase, was found to exist along the mobium-rich side of the miscibility gap. Its composition width was determined from the concentration gradients in the diffusion couples. The presence of this phase was also confirmed by microhardness analysis and metallographic observations. THE excellent corrosion resistant properties, high-temperature strength and reasonable nuclear properties of niobium have prompted its use as an alloying element with uranium and as a possible cladding material for reactor fuel elements. Hence the formation and growth of intermetallic phases as well as diffusion data for the uranium-niobium system are of considerable practical importance to metallurgists and nuclear engineers. Diffusion zones may exhibit varying degrees of complexity dependi.ng upon the mutual solubility of the metals involved, and the intermediate phases which may form. In the simplest case where the metals exhibit a calmplete range of solid solubility, a single phase region is produced. Generally, however, the metals may react to produce a multiphase diffusion zone containing several layers of intermetallic phases. A number of investigatorsl-6 have analyzed the concentration gradients present in diffusion couples in order to investigate phase equilibria and solu- bility limits. If diffusion is the rate-controlling process in establishing a concentration gradient, the compositions at the interfaces of the intermediate phases will represent the equilibrium values expected from the phase diagram at the temperature at which diffusion has taken place. No published information is available at this time on diffusion in the uranium-niobium system. A number of investigators7-" have contributed information to the construction of the uranium-niobium phase diagram from other than diffusion techniques. There is good agreement on the high uranium side of the phase diagram, but the high niobium side of the miscibility gap still remains somewhat in doubt. The phase diagram as determined by B. A. Rogers, et al.7 is shown in Fig. 1. The present work was aimed at obtaining fundamental information about the solubility limits of the miscibility gap and diffusion in the uranium-niobium system. A Kirkendall effect, which might be expected on the basis of the rather large difference in melting points between uranium (1132°C) and niobium (2415" C), was also investigated. The concentration gradients were measured by an electron microbeam probe technique, similar to that used by Castaing,l2 Adda and philibert,13, l4 and Macres.4

Jan 1, 1961

By B. H. Bergstram, C. L. Sollenberger

When glass spheres are crushed by slow compression loading, the outer lune-shaped fragments resulting from the fracture consistently fly outward at high velocity. About 45 pct of the strain energy fed into the sphere-platen system reappears in the form of the kinetic energy possessed by these fragments. These measurements were obtained from high-speed photographs. This kinetic energy can be utilized for addtional comminution if the fragments are allowed to impact against a suitable structure. Comminution theory has advanced considerably in recent years by the study of this unit operation under laboratory conditions. Some of the parameters have been isolated, but the experimental measurements of the pertinent quantities, such as energy, particle size, etc., are still only made prior to and after the conclusion of a fracture sequence. The catastrophic fracture process itself has not been adequately studied from a comminution point of view. It has recently been suggested by Gilvarry that the fragments which result from the free crushing of a single glass sphere by slow compression contain a considerable amount of kinetic energy after fracture. This kinetic energy, if properly directed, possibly can be partially utilized to cause additional fracture. In this paper a hypothesis will be presented which suggests that this kinetic energy is necessarily present and that its dissipation is the process by which a large part of the thermal energy imparted to the crushed product is generated. Evidence supporting the existence of kinetic energy and its utilization for secondary fracture will also be presented. THEORETICAL A previous paper4 has shown that the load-deformation curve of a system composed of an elastic sphere gripped by a pair of parallel platens, can be predicted by a consideration of the theories of Hertz as summarized by Timoshenko.' The deformation A, of one half of the system is given by which states that the deformation is a function of the mutually applied load, P, the radius of the sphere, R; and the respective physical properties of Poisson's ratio, v, and Young's modulus of elasticity, Y. The shape of experimental load-deformation curves conform to this relationship. The energy input to the sphere-platen system, can be predicted from the integral of the load acting through the appropriate distance, dA. Since dA can be evaluated in terms of P from the derivative of Eq. 1, this integral can be integrated between limits of 0 and P. The test sphere, however, is loaded at not one but at two points of contact, i.e., at both ends of a diameter, and hence the total energy input, E, is twice the energy input at each end, or The energy input to the system calculated from this equation corresponds to the energy computed from the measured area under the load-deformation curve. Timoshenko, considering the impact of two perfectly elastic spheres, has shown that the inter-penetration distance A is given by - m f (D (^ * ^t w as modified for the special case where one sphere is of infinite radius, i.e., its surface is a plane; where M is the mass of the finite sphere of radius R, and V is the velocity of approach at the start of an impact and also equals the final velocity of separation for perfectly elastic bodies. Because A is also a function of the load and the elastic properties, as shown in Eq. 1, the velocity, V, can also be calculated in terms of the elastic properties and maximum load, P, or

Jan 1, 1961

By Greaves M. C, Amos M. D

A study was made of the instrumentation and technique of atomic absorption spectroscopy developed by Walsh of the Commonwealth Scientific and Industrial Research Organisation (C.S.I.R.O.), Australia.The method was evaluated for the determination of silver in lead sulphide concentrate. The precision of the procedure developed is equal to that of the uncorrected fire assay method and the accuracy is greater.Brief mention is made of the use of this technique for the determination of silver and other elements in ores and concentrator products.INTRODUCTIONThe fire assay method, although accepted on a world-wide basis as the umpire method for the determination of silver in ores and concentrates, is freely recognized as yielding results which are lower than actual due to unavoidable losses.King (1934) investigated the influence of the cupelshape, size and material on silver losses during cupellation. Using 100 mg silver prills he recorded silver losses ranging between l. and 10 per cent under extreme conditions and averaging approximately 2 percent under conditions which might be considered normal. Guerin (1957) made a detailed study, under carefully controlled conditions in a furnace similar to that described by Esdaile (1952), of the effect of temperature on silver losses during cupellation. He concluded that if cupellation were carried out at 840°C., then the amount of lead retained by the silver prill was insignificant and that the silver losses were governed by the equation: Y = 0·055 XO.74where X = the final weight of the silver priIl (mg)and Y = the silver lost (mg)

Jan 1, 1961

By Perry G. Cotter

The borides of the transition metals in Groups IV and VI exhibit, in addition to a certain degree of hardness, considerable resistance to heat and oxidation. They have high melting points (1,850°-3,060° C.) and low coefftcients of thermal expansion and can be bonded with other materials and hot-pressed to desired shape (cermets). Suggested uses for the borides include use in rockets and jet engines, as thermocouple protection tubes, as containers for molten metals in die casting, as flame-plated coatings on less refractory compositions to prevent erosion by hot gases, and as control rods and neutron shielding material in nuclear engineering, The Federal Bureau of Mines investigation of zirconium diboride started in 1950 at the Boulder City Nev,, Metallurgy Research Laboratory, Its purpose was to reduce the cost of raw materials for the production of zirconium diboride.

Jan 1, 1961

In general, the metallurgical industry has so far been slower than the chemical industry to adopt ion exchange materials for industrial processes. The atomic energy industry presents a marked exception to this general situation, and the literature shows a rapidly increasing use of ion exchange techniques for the recovery of atomic energy metals on scales ranging from the ultra micro up to that of the largest mining operations. In many cases, the processes used would be equally applicable to more common metals and it is hoped that this review will be of interest to metallurgists outside the specialised atomic energy field. The review is intended to describe developments of ion exchange processes made during the last three years. Earlier studies have been summarised by Kunin and Preuss (1956) and Roland (1957). In order to restrict the number of references discussed, purely analytical procedures have been omitted and only those processes which have been conducted on a reasonably large scale or which, from their nature, areclearly capable of being upscaled, have been considered. The paper is divided into five main sections concerning respectively:Water treatment and effluent disposal.Metal recovery and purification.New ion exchange materials.New ion exchange equipment.Membrane cells.WATER TREATMENT AND EFFLUENT DISPOSALA high proportion of atomic reactors, and particularly those of American design, are cooled by water which is...

Jan 1, 1961