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Institute of Metals Division Iron and Steel Division Extractive Metallurgy Division J C Kinnear, Jr, President A W Thornton, Past President W R Hibbard, Jr, Vice-President R W Shearman, Secretary-Treasurer AIME, 29 West 39th Street New York 18, N Y Board of Directors J B Austin, D L Clark, H B Emerick, T D Jones, H H Kellogg, C T Marshall, E E Schumacher, C S Smith, J D Sullivan

Jan 1, 1957

By H. R. Brannon, J. S. Osoba

The introduction of the scintillation counter into field use for gamma-ray well logging has provided a new tool with special utility for the deternzination of natural radioactivity of sediments. Previous subsurface gamma-ray measurements have indicated only the total amount of radioactivity of the sediments. With the scintillation counter, the relative amounts of the elements which emit gamma radiation can be determined. Sediments logged included 35 zones in wells located in the Teras Gulf Coast, East Texas, and West Teras. Although the data obtained from measurements made to date are not sufficient to evaluate the possibilities of spectral logging, it appears likely that spectral measurements will yield information of geologic value. INTRODUCTION Although variations in the natural radioactivity of sediments were recognized as early as 1909,1 the appli- cation of such variations to borehole logging was not made until almost 30 years later. A group of Russian workers in the early 1930's were successful in making crude measurements of natural gamma activity in an oil well borehole. The first practical gamma-ray logging system was developed by Howell and Frosch2 in 1939. Induced radioactivity, or neutron, logging appeared soon after the introduction of gamma-ray logging. After early work had demonstrated the potentialities of radioactivity logging, development of sensitive and stable logging equipment for field use followed, so that neutron and natural gamma logs are now run routinely and have proved to be extremely valuable in characterizing subsurface formations. Even though tremendous strides have been made in developing radioactivity logging, it is apparent that the ultimate in the method of logging has not been reached, for, until very recently1 in none of the commercially available logging systems has advantage been taken of the fact that gamma radiation is composed of a spectrum of rays, each ray having a distinct and characteristic energy. An individual gamma ray originates in a single element and has energy determined by the element. The inten- sity of radiation, or number of rays emitted from unit volume in unit time, is determined by the concentration of the element. If it were possible to sort out these gamma rays and assign them to their parent elements, thereby essentially analyzing for the elements, a wealth of new information descriptive of formation material and fluid content would be at hand. For example, if in natural gamma logging, the gammas due to potassium and to the thorium and uranium series were measured individually, data would thus be available on the concentrations of each of the three elements, adding materially to the information content of the log. In contrast, conventional gamma logs measure only a quantity proportional to the combined concentrations of uranium, thorium, and potassium. The naturally radioactive elements occur in sediments in concentrations dependent on source material of the sediment, and through their chemical characteristics, on conditions of deposition,' so that the individual concentrations may be diagnostic for particular formations. These concentrations, particularly if measured in situ, could lead to a powerful tool for correlation and for reflecting environmental conditions under which sedimentation took place. As a correlation tool, individual uranium, thorium, and potassium measurements

Jan 1, 1957

By E. G. Leonardon

THE object of this paper is to describe briefly the practical results obtained in several problems of civil engineering by resistivity measurements of the underground. It is intended for the mining engineer, as well as for the construction engineer; the stratigraphical problems discussed are general and frequently are encountered in mining exploration. Resistivity measurements have been used in mining and oil exploration for a number of years.1 Their introduction in the field of civil engineering, on the contrary, is rather recent. It was applied for the first time in the spring of 1928 near Littleton, N. H., in the survey of two dam sites for the New England Power Assn .2 Since then, the geophysical firm with which the author is connected has had an opportunity to develop this field of activity, and more than 20 investigations at dam and tunnel sites have been carried out in the United States and Canada. A part of this work has been verified by underground or drilling exploration. This paper deals with but a few of the results, which we are permitted to make public now. The theoretical and technical sides of the processes employed will not be discussed; they have already been described in various technical. .publications. A few general points will be mentioned, to make clear the practical examples given.

Jan 1, 1931

By R. V. Ramani, Robert Stefanko

The more stringent ventilation requirements of the 1969 Act have created a greater need for improved network analyses. More air is required at the last open crosscut (9000 cfm) and for the first time a minimum quantity is specified for the face (3000 cfm). Severe restrictions are placed on both belt and track haulage, and the intake air cannot contain more than 2 mg per cu m of respirable dust, to be reduced to 1 mg later. Larger tonnage and longer life mines are the trend today, necessitating multiple fans and shafts. Yet relatively little engineering goes into designing the mine ventilation system. In this paper a ventilation system is designed for a typical Pittsburgh block system, manual calculations are made and then checked by a computer solution. The computer is the ideal tool to try out proposed changes on paper to insure that the entire mine is properly ventilated and no costly adjustments need be made by dumping air. While it is theoretically possible to solve complex ventilation network problems by hand, it is not practical to do so because of the tremendous man-hours required and the many opportunities for errors. Thus the digital computer is indispensible to the ventilation engineer and newer improved ventilation programs are being developed to more realistically model mine ventilation networks. Suggested ventilation changes to comply with the new regulations are also critically evaluated.

Jan 1, 1973

By L. Adler

Some estimate of the geologic pressures existine at the site of a proposed underground opening is essential for its economic design and construction. Regardless of the size of such an opening, drill hole, or mine stope, these primitive stresses need evaluation; at present a number of techniques are available for this purpose. However, a new method of analysind stresses is proposed in this paper. Some estimate of the geologic pressures existing at the site of a proposed underground opening is essential for its economic design and construction. Regardless of the size of such an opening, drill hole or mine stope, these primitive stresses need evaluation. At present a number of techniques are available for this purpose, and another one is to be proposed. These may be grouped into three general methods: 1) precedent, 2) instrumentation, and 3) theoretical analysis. The first two are covered in the literature where their advantages, as well as limitations, are discussed.'9' Generally a theoretical approach combines structural geology with engineering mechanics. The former deals with the geodynamic causes of residual stresses (stresses not related to overburden weight) and presents interesting, but controversial, views.'" A general and useful conclusion, however, can be drawn - vertical residual stresses are much less prevalent than horizontal. However, if for some reason, the values and effects of horizontal pressures were better known to engineers the following analysis

Jan 1, 1962

By Oberlin Smith

The experiments described in this paper are very incomplete and only preliminary to those I hope to make in the future. Having had a good deal of experience in cutting, forming and drawing sheet-metals, and feeling a great interest in the commercially new and wonderful metal, aluminum, I applied to my friend, Mr. A. E. Hunt, for some specimens in sheet-form, that I might, from time to time, test its working-properties in presses with which we happened to be experimenting at the works of the Ferracute Machine Company. The chances for such trials being accidental only, and the time having been limited to the last few weeks, no crucial experiments have been tried, and no exact data have been obtained for a rigid comparison with other metals. The results of what little we have done, however, are shown in the articles exhibited in connection with the reading of this paper, which comprise various cups, plates, boxes, bells and cartridge-cup and shells. For the latter I am indebted to my friend, Mr. Hobbs, of the Union Metallic Cartridge Co., who, at my request, ran several pieces of sheet-aluminum through the dies with which he was making brass cartridges. The specimens are rougher than they would be had the metal not been a little too thin for the particular dies which he happened to be running.

Jan 1, 1890

By A. Berghezan, E. Bull Simonsen

A simple and general method is described for melting and zone refining refractory metals by induction heating on a specially shaped water-cooled copper crucible. The crucible is the essential part of the apparatus and is placed horizontally. It consists of either a copper plate, or a flattened tube, or of several parallel small diameter tubes all water cooled. The charge lies on the crucible, or whenever possible, is suspended above it. This assembly goes into a transparent quartz tube and the whole is passed through the coil of a radio frequency generator. Vaarious atmospheres can be used. No contamination is detected from the copper crucible. purification is obtained both by selective evaporation of impurities and by zone refining. METHODS of melting and refining relatively large ingots of all reactive and refractory metals as well as some semiconductor materials have been developed in this laboratory during the past several years using induction heating and cold crucibles. These methods are simple and permit the use of a variety of starting materials in preparing ingots of suitable shapes. Among these methods, two are of particular interest. One deals only with the problem of melting without contamination. In this method the induction coil has a specially designed shape and acts simultaneously as heating element and crucible. The second goes one step further, being designed for both melting and further purification of the refractory metals. The aim of this paper is to describe the second method which is of more general interest and of greater applicability to metallurgical problems. A) THE PRINCIPLE OF THE MELTING AND PURIFICATION METHOD As originally proposed by one of us1 the method consists of heating a charge of any refractory metal or semiconductor material to the melting point on a water-cooled copper crucible by passing both the charge and the crucible through the induction coil of a radiofrequency generator. Although both are subjected to the same induction field, one achieves the melting of a refractory metal on a copper crucible even when the refractory metal has a melting point of more than 2000°C above that of the crucible. This seemingly "odd" method works effectively for the following reasons. Because of its high electrical and thermal conductivity as compared with the material being melted, copper can be used as the crucible and kept at a low temperature while the material is heated by induction to its melting point. With water Silver and other highly conducting materials can also be used. If a nonconducting material is contemplated, e.g. SiO or a high polymer, a very thin wall should provide efficient cooling. cooling through ducts in the crucible its temperature can be kept between 40" to 70°C; thus its electrical resistivity is kept low, while the resistivity of the charge increases rapidly as its temperature is increased. B) APPARATUS The crucible is the essential part of the apparatus. It has been designed in various shapes depending on the atmosphere used, whether vacuum or an inert gas or hydrogen. In all crucible designs an effort was made to reduce its volume to "nothing but the cooling water" in order to avoid shielding the ingot from the induction field. In practice it is either a

Jan 1, 1962

By David L. Holt

It is well-established that hydrostatic pressure distribution is hardly achieved during uniaxial compaction of powders. All the previous investigations1-4 give consistent results and this variation is attributed to the die-wall friction. The conclusions are based on measurements of the density of very small portions of the compact. Although the analysis of the density or the strain distribution in the compact is very helpful in obtaining information about the stress distribution within a powder compact, it does not describe the problem from a more fundamental point of view. The densification in metal powder compacts takes place chiefly by plastic deformation (ignoring particle rearrangement) at the points of contact of the powder particles. The onset of yielding and subsequent growth of the contact areas (for spherical powders) take place fixed by a constant stress equal to three times the yield stress in tension or compression,5-7 assuming little or no work hardening. Therefore, by deforming spherical powders in the die and measuring the contact areas on each particle, the load at each contact point can be determined. In the present investigation, this was done by hot-pressing uniform spheres of lead, K-Monel, and sapphire. The details of the experiment have been described elsewhere.' The spheres were studied for the size and the number of contact points on each particle using a specially designed goniometer. It was found that the deformed faces that were approximately normal to the direction of pressing were about 2.2 times larger than those parallel to the direction of pressing. Fig. 1 shows the typical deformed sphere. A detailed study showed that the mean value of the contact areas on each sphere was within 5 pct for all the spheres in the die (ignoring those touching the die walls and the top and bottom of the die).' The spheres touching the die walls and the top and bottom of the die were found to have larger contact areas (8 to 10 pct) which indicates higher pressures in these regions of the compact and thus higher compact densities in these regions. These results show that density distribution calculated from such an experiment will give results consistent with the previous investigators. It is concluded, therefore, that the pressure distribution in the die is better understood by studying contact areas on each particle. 'R. Kamm, M. A. Steinberg, and J. Wulff: Trans. TMS-AIME, 1947, vol. 171, p. 439. 'Pol Duwez and Leo Zwell: I. Metals, 1949, vol. 1, p. 137. 'G. C. Kucynski and I. Zaplatynskyj: Trans. TMS-AIIME, 1956, vol. 206, p. 215. 'R. P. Seelig and J. Wulff: Trans. TMS-AIME, 1946, vol. 166, p. 492. 'H. Hencky: Z. Angew. Math. Mech., 1923, vol. 3, p. 241. "J. Ishlinsky: I. Appl. Math. Mech. USSR, 1944, vol. 8, p. 233. 'D. Tabor: Proc. Roy. Soc. (London), Ser. A, 1948, vol. 192, p. 247. 'Ashok K. Kakar and A. C. D. Chaklader: 1. Appl. Phys., 1967, vol. 38, p. 3223. Superplasticity in 60Zn-40Al David L. Holt THE occurrence of superplasticity in Al-Zn alloys is of interest because of its possible industrial exploitation.' The eutectoid composition (78Zn-22A1) has been the most extensively studied;'-= neck resistant flow and high strain rate sensitivity of flow stress (characteristic of superplasticity) are associated with a micron-size grain conferred on the alloy by an homo-genization and quench.5'6 Compositions away from the eutectoid have received comparatively little attention, especially from the viewpoint of relating the structural

Jan 1, 1969

By R. L. Smith, I. G. Greenfield

The binary system Ga-Sb has been investigated by thermal, X-ray, and metallo-graphic methods. 'The intermetallic compound GaSb melts at 705.9OC and forms a eutectic with antimony at 11.8 atomic pct Ga. This eutectic melts at 589.8OC. A eutectic appears to be formed at 29.8°C but is too close to the composition of pure gallium to be detected. IN the course of an investigation of the semiconducting properties of the intermetallic compound, GaSb, the phase equilibrium between gallium and antimony has been investigated. Recently, the phase diagram of similar systems, such as In-Sb,' In-AS,' and Bi-As3 have been determined. These diagrams have the same general appearance in that an intermetallic compound is formed at 50 atomic pct and a eutectic is formed on both sides of the intermetallic compound. Jenny,& who has been investigating the semiconducting properties of intermetallic compounds, has concluded from thermal data of several alloys that the phase diagram of the Ga-Sb system resembles those mentioned previously. This paper represents a more detailed study of the Ga-Sb equilibrium. Experimental Procedure The gallium that was used to prepare the alloys was obtained from A. D. Mackay Inc. and the Aluminum Co. of America; the latter reported the purity as 99.95 pct. The antimony was obtained from Bradley Mining Corp. who specified a purity of 99.997 pct. Since the intermetallic compound of GaSb was prepared primarily to be used for further studies of the semiconducting properties, additional purification by a standard zone-melting technique under an atmosphere of hydrogen was performed. Hall-effect measurements on this material indicated an impurity content of less than 3 ppm.5 The antimony also was purified by zone melting and used in conjunction with the compound GaSb to make the necessary alloys for the determinations of the antimony-rich side of the phase diagram. The antimony-rich alloys were chill cast in Vycor tubes which were evacuated to a pressure of less than one micron. Since these alloys expand on freezing, precautions were taken to prevent oxidation of the ingot in the event the tube fractured. To insure homogeneity, the brittle alloys were ground and then placed in the furnace for the thermal-arrest determinations. Since the cost of gallium is high, the experimental procedure was complicated somewhat because of the necessarily limited sizes of the melts. In order to economize, the gallium-rich side of the diagram was determined by using a 35 g ingot of pure gallium initially and adding increasing amounts of antimony in order to obtain additional alloys. The furnace used in the determination of the cooling curves is illustrated in Fig. 1. A 2¼ in. quartz tube, sealed at one end, was fitted with a brass flange which was attached with DeKhotinsky cement. The brass collar was water cooled to prevent the cement from softening. An "0" ring was used to provide a seal between the brass collar and the furnace cover. Nichrome ribbon was wound around a 2 ½ in. asbestos-covered copper core which was used to reduce the thermal gradient in the furnace. The insulation consisted of alternate layers of asbestos and aluminum foil surrounded by sil-o-cel refractory and

Jan 1, 1956

By R. A. Swalin, L. A. Neimark

The research work presented in this paper had initially a two-fold goal. First, further data concerning the low-temperature recovery of cold work was desired. Recovery phenomena have been extensively studied in face-centered-cubic metals but at the time of initiation of this research, no investigation concerning the low-temperature recovery in body-centered-cubic metals had been made. During the course of the investigation a paper by Martin on the recovery of point defects in molybdenum appeared.&apos; Comparison of our results on tungsten with Martin&apos;s results on molybdenum will be made. Secondly, knowledge concerning the influence of a particular type of impurity addition on the recovery kinetics was desired. It has been known for a long time that extremely small amounts of certain impurity additions exert a profound influence on the recrystallization behavior and the resulting microstructure of tungsten. Small amounts of potassium silicate and aluminum chloride added prior to the reduction of tungsten oxide to the metal have been found by Smithells to raise the recrystallization temperature markedly,2 and yield an ultimate microstructure in which grains several millimeters long are produced in fine wires of say 10 mil diam. If the impurities are added singly, ordinary secondary recrystallization results with none of the spectacular properties of the wire to which special additions were made. Swalin and Geisler3 and Rieck4 have studied the recrystallization behavior of such doped wire in some detail. The former workers found that small amounts of these impurities raised the recrystallization temperature over 400°C and electron microscopic examination revealed no obvious inclusions in the microstructures. In fact. chemical analysis showed that there was <0.001 pct K, <0.002 pct Al, trace of Si, and <0.0003 pct 0 in the wire studied. The possibility that the role of the special impurities is to keep the structure open by void formation and that submicroscopic porosity acts as the inhibiting agent has been discussed.2&apos;3 Meijering and Rieck5 have suggested that the impurities are strung out as second-phase particles in a direction parallel to the drawing direction. It was thought that a kinetic study of recovery could perhaps elucidate the role of the impurities to some extent. When a metal is deformed by cold work three basic types of defects are thought to be introduced into the crystal lattice, namely, interstitials, vacancies, and dislocations. Van Bueren6 has proposed that recovery of cold-worked metal is a four-stage process, each step being the result of the annealing of a primary defect or a combination of defects and having a unique activation energy. The steps in order of increasing activation energy are attributed to a) the diffusion of interstitials recombining with vacancies, b) diffusion of vacancy pairs, c) the diffusion of single vacancies, and d) climb of dislocations. In metals with relatively low- or medium-range melting points the temperatures for recovery are low enough so that the first three steps may occur during room-temperature deformation. For tungsten, because of the high melting point and subsequently high recovery temperature, it was calculated, using Nowick&apos;s approach7 that this recovery would occur in the temperature range 200" to 600°C. It is also known that recovery of X-ray line broadening, presumably due to dislocation climb, occurs at about 600°C.8 EXPERIMENTAL METHOD Two types of cold-rolled 10-mil-diam tungsten wire were used in the investigation; a) pure tungsten, (called undoped) and b) G. E. No. 218 wire (called

Jan 1, 1961

By F. H. Buttner, E. R. Funk, H. Udin

Gold wires, 5 mil in diam, are found to creep viscously up to approximately 5.5x106 dynes per sq cm around 1300°K. Beyond this point, an additional slip mechanism appears. The average coefficient in the viscous range at these temperatures is 18.9 ± 7x10 12 poises. This observation and other visual observations made during the experiments agree with Herring&apos;s predictions. EARLY creep studies by Chalmers on single crystals of tin produced some of the first experimental evidence to suggest that metals deform viscously under very light stresses. That is to say, over a small initial stress range up to 150 g per sq mm, the single crystals of tin elongated at a rate proportional to the stress. The proportionality constant between strain rate and stress is by definition the coefficient of viscosity. Chalmers named this range of proportionality the microcreep range. One of the first theoretical attempts to explain the microcreep phenomenon was given by Kauzman,&apos; who applied Eyring&apos;sQ eneral statistical mechanical theory of shear rates to creep data then available. From the rate theory, he deduced the general hyperbolic sine law for shear rate on the assumption that the distortion of the reaction path due to stress is negligible and that the system is an infinite continuum. In order to fit the available data to the equation, it was necessary to assume that creep occurs by shear of rather large blocks of material, rather than by an atomistic shear process as in diffusion. The size of the shear units was shown to increase with increasing temperatures and lower stress, or lower strain rates. In applying the hyperbolic sine law equation to the microcreep data of tin, it was shown by Kauzman that the unit shear blocks became quite small, which suggested to him that microcreep might be a self-diffusion process. Making this an assumption, Kauz- man reworked the rate theory and arrived at an equation where the shear rate is proportional to the stress. In the form of viscosity coefficient, the equation is: o- _ \LkT V = 2qAlA where u is the stress; S, the shear rate; X, the distance in shear direction moved by flow units relative to one another in the unit process; L, the distance between layers of units of flow; T, the absolute temperature; k, Boltzmann&apos;s constant; qAL, a constant proportional to the size of flow units; and kT A, the diffusion coefficient = ------kTe-Q/RT = K X2 h Kauzman applied the expression to molten lead with a fair degree of success, the calculated viscosity being low by a factor of four. For solid lead the result is 5000 times too high. Taking q = 1, and X = dA = L = 21 = nearest neighbor distance, Udin, Shaler and Wulff8 found the equation low by a factor of lo7 for solid copper. On the basis of the discrepancy in lead, Kauzman indicated that microcreep is probably not a simple diffusion process of molecular shear units, but one involving preferential diffusion paths, or even that diffusion in solids does not involve shear at all. Cottrell and Jaswon4 treat the microcreep phenomenon on the basis of slow moving dislocations and apply it to Chalmers&apos; data on tin with fair success. Nabarro Suggested a microcreep model in which mass movement in the direction of pull is effected by the diffusion of holes. The tension on the crystal effectively creates a greater hole concentration at regions near the crystal surfaces perpendicular to

Jan 1, 1953

By G. L. Kehl, Emilo Jaraiz F., J. S. Brett

The transformation of eutectoid beryllium bronze has been quantitatively investigated at 550° and 592°C, the temperature region where the products of p decomposition are a fine lamellar eutectoid and a coarse lamellar aggregate which replaces the fine eutectoid with prolonged annealing. Metallographic evidence indicates that the coarse lamellar aggregate forms preferentially in the most densely lamellated regions of the fine eutectoid and favors the hypothesis that the development of the coarse lamellar aggregate in the fine eutectoid is due to the occurence of a cellular segregation reaction. WHEN eutectoid beryllium bronze (Cu-94 pct, Be-6 pct) is isothermally transformed at high temperatures in the and y region after quenching from the fl field, the principal initial decomposition process is G one of growth of approximately spherical nodules composed of a number of lamellar colonies of the a and y phases. After the initial reaction has proceeded substantially or completely, depending on the transformation temperature, a second reaction occurs wherein the fine lamellar eutectoid is replaced by a coarser lamellar aggregate composed of the same oand yphases.&apos; This reaction is not simply a spheroidization of the initial fine eutectoid but the nucleation and growth of a coarser, structurally different, and more stable distribution of the @and yphases. Fig. 1 illustrates the replacement of the initial fine lamellar structure by a coarse lamellar aggregate. The a phase is the dark mottled constituent; the light constituent the y phase. The phase diagram for the copper-rich end of the Cu-Be system2 is shown in Fig. 2. The a phase has the face-centered cubic structure characteristic of copper-rich solid solutions. The B phase is a disordered body-centered cubic structure, while the y phase is body-centered cubic, ordered (CsC1, B2 type). A. viswanathanS investigating Debye patterns of Cu-6 pct Be discovered that a transitory phase appeared on very rapid quenching from the /3 region which was absent when the quenching velocity was moderate. The phase could be assigned a body-centtred cubic structure with a lattice parameter of 2.876. Tempering at 100°C for 2 hr after quenching resulted in complete disappearance of the phase. The work of Fillnow and Mack&apos; is the only previously published study of the isothermal transformation of eutectoid beryllium bronze. Their study elucidated the nature of decomposition at various subcritical temperatures in an exploratory fashion. The purpose of the research reported in this paper was principally to obtain quantitative information on the isothermal decomposition of the fl phase and to clarify the relationships existing between the fine lamellar eutectoid and the coarse lamellar aggregate. EXPERIMENTAL PROCEDURE The material used in this investigation was an almost eutectoid Cu-Be alloy bar furnished by D.J. Mack. The alloy had been melted under a protective carbon cover and centrigugally cast into a graphite mold preheated to 490 "C. Segregation was minimized by violent agitation during melting and pouring. The analysis of the casting was 93.85 pct Cu, 5.60 pet Be with traces of Si, Mg, Mn, Co, and Al. To determine the minimum soaking time necessary to insure specimen homogeneity, a number of specimens were held in the P region at 788OC for times fron 1 min to 12 hr and isothermally transformed at 550°C. Specimens betatized less than 12 min exhibited partial transformation at times shorter

Jan 1, 1961

By A. G. Jordan, W. Jeitschko, Paul A. Beck

The occurrence qf the V phase structure /Zr,Co,Ge, type) in ternary syste7ns (titanium, zivconium, niobium, lanta1urn) -(nickel, cobalt, iron)-(silicon, germanium) was incestigated. Nine V silicides and four V gertrlanides were found and their lattice constants are reporled. The lattice constants of twenty-one preri-ously identified E phases (TiNiSi type) are given. The average atomic volumes of these phases are discussed in relation to similar binary phases. ThE occurrence of a phase Ti4Ni4Si7 was first reported by Westbrook. DiCerbo, and peat&apos; who gave it the name "V phase". They also reported the existence of an E phase TiNiSi. Subsequently a systematic study was undertaken in this laboratory to explore the occurrence of E&apos; and V phases3 in related ternary systems. In the meantime the crystal structure of the E phase TiNiSi 4 and of the V phase Zr4CO4Ge 75,6 was determined. In the present paper the details of the V phase investigation and the lattice constants of the E and V phases are presented. V PHASES Alloy specimens of approximately 10 to 15 g were prepared by arc melting under argon (99.996 pct Ar) atmosphere. The starting materials were all of purity higher than 99.9 pct, with the exception of cobalt. which contained 0.14 pct Fe as the only major impurity. The weight losses were in all cases less than 2 pct, in most cases less than 1 pct. The samples were encapsulated in fused silica tubes with sufficient argon to yield about 1 atm pressure at the annealing temperature. After the homogenization anneal. Table I. the specimens were water-quenched. A representative portion of each specimen was then examined metallographically (etchant: 20 pct HNO,. 10 pct HF. 25 pct glycerine, 45 pct H20). Only minor amounts of second- and third-phase particles were observed in the specimens listed in Table I, with the exception of alloys Zr4Fe4Si7 and Ta,Fe,Si,. which contained an estimated 10 pct by volume of foreign phases. X-ray powder photographs were taken with a Seeman-Bohlin type focusing camera and Fe-KO radiation. Of the thirty possible combinations of elements in the ternary systems (titanium, zirconium. vanadium. niobium. tantalum)-(iron. cobalt, nickel)-(silicon. germanium) thirteen V phases could be identified. In the remaining seventeen ternary systems and also in the systems Cr-Ni-Si and (M0.W)-(Ni.Co)-Si no V phase was found at the composition 4:4:7 after annealing at temperatures between 900" and 1200&apos;C. For the determination of the lattice constants of the V phases Debye-Scherrer photographs were taken using the asymmetric film arrangement and CrKcr radiation (ka1, = 2.28962A). Using the positional parameters, as determined6 for Zr,Co,Ge,. Table 11. intensity calculations were carried out for each of the V phases with the aid of a computer program.: Thus unequivocal indexing of the diffraction patterns was greatly facilitated. The lattice constants. Table I. were then computed by a least-squares fit of the high-angle lines with f (0) = cos2 Q as extrapolation function. Only few. if any. very weak impurity lines were observed, with the exception of the three iron alloys Zr,Fe,Si7. Zr4Fe,Ge7. and Ta,Fe,Si7. The agreement

Jan 1, 1970

By R. F. Rolsten

The preparation of pure metals by the thermal decomposition of volatile halides was developed byde boer&apos; and van Arkel.2 This has proved to be a useful technique for the refining of columbium,the mechanical and physical properties of which are seriously altered by such interstitial contaminants as oxygen, nitrogen, hydrogen, and carbon. The conventional deposition surface of a resis-tively heated metal filament was replaced, Fig. I, with an indirectly heated clear quartz surface. The impure columbium (feed) was contained in the annular space between the Vycor deposition bulb and the perforated molybdenum retaining cylinder. The head assembly was attached to the deposition bulb by fusing the Vycor at "A". This unit was then connected to a vacuum system composed of a three-turn glass coil to eliminate fracture due to vibration or expansion, a McLeod gage, a cold trap, a two-stage mercury diffusion pump, and a mechanical pump. The entire system was cold outgassed, and the 10 to 20 g of iodine in the auxiliary bulb (reservoir) was held in dry ice to prevent excessive loss of iodine. The columbium was hot outgassed at 800" to 825oC with the pressure maintained at l0-5 to 10-6 mm Hg for 48 hr and cooled under vacuum to 200° to 240oC. Iodine was sublimed from the reservoir and collected in the deposition bulb. The feed material temperature was adjusted to give the desired iodide vapor pressure and the finger temperature of 1000" C was independently attained and measured with a platinum-platinum 10 pct Rh thermocouple located in the center of the nichrome wire helical heating element, "F." The system was attended until temperature equilibrium was established, whence it operated without attention. This is a definite ad- vantage over the conventional "hot-wire" technique which required either constant attention or automatic control. In operation, the iodine vapor originally introduced into the vessel reacted with the crude metal to form a columbium iodide. This iodide vapor diffused to the hot deposition surface where it thermally decomposed, depositing columbium and releasing iodine. This liberated iodine then diffused back to the crude columbium where iodide was formed again. Thus, by repetition of this process, the iodine carried pure columbium from the crude material to the filament, where it deposited. The success of the "iodide" process in producing ductile metals depends on preventing the transfer of oxygen, nitrogen, hydrogen, and carbon from the feed material to the deposit. In many cases relatively minor quantities of these interstitial contaminants impair the ductility of metals. The material produced by the iodide process has such exceptional ductility that it is frequently and mistakenly assumed that iodide metal is always of very high purity. This assumption is not necessarily true since a number of metallic impurities can also be transferred. In the present investigation, the temperature of the feed material was adjusted to iodinate selectively and the deposition temperature adjusted to decompose the iodides selectively. By this technique, some metals present in the feed material were prevented from codepositing with the columbium. It is quite important to have the feed material symmetrically located around the deposition surface in order to obtain a uniform deposit at the maximum rate. For example, Runnalls and pidgeon3 observed that, when the base of a titanium filament was about 1 cm from the feed material, deposition was rapid on that section close to the feed, but that the rate decreased with distance from the feed so that a

Jan 1, 1960

By John Birkinbine

An unusually large number of crystals of magnetite obtained in the exploitation of a deposit of magnetic iron-ore of remarkable purity, encouraged the preparation of this paper, and its presentation at this time, that the matter might go on record in the Transactions. To make this record more complete, a preliminary statement is offered concerning the district and locality in which the ore is found. To the northeastern portion of the State of New York the United States is indebted for a large percentage of the iron-ore which has assisted in developing the resources and industries of the nation. As early as 1804, iron-ore was mined between Lake Champlain and the Adirondack mountains, and this district has since been an important and continuous contributor to our iron-ore supply. The production of the Lake Champlain district for the last, eleven years is as follows: Years. Gross tons. 1879,...........420,341 1880,...........531,000 1881,...........637,000 1882,...........675,000 1883,...........500,000 1884,...........504,894 1885,...........379,077 1886,...........588,752 1887,...........768,852 1888,...........789,419 1889,...........750,230 Approximate total,.....6,644,565

Jan 1, 1890

By AIME AIME

ALTHOUGH the retiring Chairman of the Industrial Minerals Division, Charles Henry Behre, Jr., does not say "you all" he is a product of the deep South, since he was born at Atlanta, on March 16, 1896. At the Boy Scout age he moved to New Orleans, where his father owned an ice plant, which seems an intelligent business for that climate. Intelligence evidently runs in the family, for Charlie, as his friends call him, has one sister who is a professor of zoology and another who is a concert pianist. Charlie has no explanation of why, when he reached college age, he decided to go to the University of Wisconsin, other than something more than an ordinary boyish interest in science, and the reputation which Wisconsin then enjoyed. At Madison he fell under the influence of Eliot Blackwelder, chose paleontology as his objective, and transferred, at the end of his sophomore year, to the University of Chicago, where the paleontological panorama seemed more extensive. He took his B.S. there in 1918, and graduated into the U. S. Army, where he eventually became a Sergeant in the Medical Corps.

Jan 1, 1945

By Stephen Royce

[PAGE Ground Movement Adjacent to a Caving Block in the Climax Molybdenum Mine (TP 2000 by JOHN W. VANDERWILT, Min. Tech., May 1946. Discussion by STEPHEN ROYCE and the Studies of the Design of Shaped Explosive Charges and Their Effect in Breaking Concrete Blocks (TP 2157 by GEORGE B. CLARK, Min. Tech. May 1947. Discussion by PHILIP B. BUCKY, V. H. CLARK, E. D. GARDNER, M. H. HAWKINS, H. L. WALKER, and the author) 2 See TP 2377, Min. Tech., May 1948 for discussion of San Manuel ProsPect (TP 2255 by H. J. STEELE and G. R. RUBLY, Min. Tech., Sept. 1947. Discussion by L. KENNETH WILSON, ELDRED D. WILSON and the authors)] Ground Movement Adjacent to a Caving Block in the Climax Molybdenum Mine STEPHEN ROYCE•-It is interesting to note from B, Fig 2, how closely the subsidence limits approximate to the 60° angle of draw, which is so commonly found to rule in large scale rock subsidence. The tension cracks shown at B are commonly found in the initial stages of subsidence movement and spread like a halo about subsidence limits as movement extends. These tension cracks usually grow into escarpments later on. Apparently from the illustrations and description given, a system of vertical fractures is the predominating weakness in the wall rock at Climax, and therefore both tension cracks and escarpments are prevailingly vertical in attitude. The illustrations in Mr. Vanderwilt&apos;s article seem to conform to the general rule that yield by subsidence is heralded by tension cracks which foreshadow the appearance of the subsidence scarps which are both described in the paper and shown in Fig 2. The difference between the B side and the A side of Fig 2 is apparently caused mainly by the vertical fracturing which controls subsidence at Climax as compared to the relatively homogeneous rock formation at A upon which the original figure in Peele&apos;s Handbook was based. The draw at B is exactly 60°, while the draw at A is a little flatter. The influence of the vertical fractures explains the difference. The surprising feature is the relatively small deviation from the general 60° draw line, which is about the average of rock subsidence experience. The influence of local fracture systems, faults and bedding in controlling subsidence all the way from extremely low angles of draw to vertical is rather fully discussed in the Peele&apos;s Handbook article referred to. The more illustrations of subsidence there are published the better will be our knowledge. The general principles are pretty well established. The wide local differences reflect the effect of local conditions. This paper is a very valuable contribution to the subject, and for the benefit of the mining industry, it is to be hoped that there will be many more such clear and concise presentations. Particularly block caving is apt to be of greatly increasing importance in the future of a mining industry that must meet high labor costs. More examples of block caving from small scale to large scale operations like those at Climax will serve a vital need. JOHN W. VANDERWILT (author&apos;s reply)-I would like to thank Mr. Royce for his discussion; however, in his comments the meaning of subsidence, draw and tension cracks is not entirely clear. As used in my discussion of subsidence at Climax, subsidence refers to movements involving appreciable downward displacement. Tension cracks indicate only

Jan 1, 1947

By J. A. B. Forster

W. G. WOOLF*—The paper has a wealth of data that take careful, detailed study. As has been indicated the highlights can be only touched in the paper. The design and the arrangement of the rabble teeth as well as some of the other details of operation show a very careful study and a scientific approach to the problem which in most plants using hearth roasters are matters of trial and error with empirical conclusions and, perhaps too often, just arbitrary supervisory preferences which may be erroneous. Here the problem has been approached from a scientific angle which think well merits careful study. The ability to treat the tonnages they get through these furnaces think is made easier by reason of the high sulphide sulphur in the resulting calcines which the balance of the plant—the leaching and so on—can cope with. As indicated by Mr. Weldon in his dis- cussion earlier this morning, in most zinc plants an attempt is made to have as low a sulphide sulphur content in the roaster calcine as possible. But in the operation of the Risdon plants, they are able to cope with sulphide sulphur content up to 5 pct which is far beyond the amount of sulphide sulphur that can be handled elsewhere. I think the autogenous roasting is made easier because driving out the last percentages of sulphide sulphur brings on the necessity for extraneous heat, and that is further exemplified because even at Risdon the author shows the desirability of using some oil to better the operation, particularly for uniformity of roasting results and to obtain more regularity of furnace operation. A. A. CENTER*—Regarding the hard crusts in the beds of the furnace and autogenous roasting, the paper speaks of the former being due, at least to a considerable extent, to lead sulphide in the crusts. I wonder if the author has considered the hard crusts as being due in large part to zinc sulphate. While I was developing large zinc operations we ran into hard crusts which had to be dug up. I took several lumps which were so hard they showed the marks of the rabble teeth very plainly and kept them in my office for some weeks. A visitor came along one day, and as he was having similar troubles, I told him what we were doing about ours. I started to pick up one of these lumps and to my amazement the thing crumbled in my hands whereas originally it had been so hard it wore the rabbles down very rapidly in the furnace. I sent the sample to the laboratory and found that it analyzed very high in water-soluble zinc and sulphate-sulphur. The crumbling of the lumps was evidently due to the anhydrous zinc sulphate gradually taking on moisture from the air and forming crystalline zinc sulphate seven parts water. The increase in volume would, of course, result in disintegration of the lumps. As to getting a high tonnage in the autogenous roast, that is partly because of finishing at about 5 pct sulphide sulphur. It is a real job to get down to, say, ½ pct sulphide sulphur, which is what is usually desired, and still put through a good tonnage.

Jan 1, 1950

By D. H. Thompson, A. W. Tracy

E. A. ANDERSON*—At the outset, I note that you are using a humid atmosphere containing ammonia but that you make no reference to the variable of carbon dioxide content. Edmunds in his work in this laboratory found very marked effects on the rate of failure due to variations in carbon dioxide in the environment. This point is, of course, strongly related to the overall corrosion rate problem since the role of the carbon dioxide seems to be to permit the formation of hygrogroscopic salts which give a controlled moisture film on the specimen surface, which in turn seems to support the intergranular penetration more consistently than would otherwise occur. (2) Your results with various copper binary systems are very striking. It is curious, however, that the time-to-failure minima all occur at percentages of the alloying element which are considerably below the solubility limits as given in the conventional equilibrium diagrams. If your theory regarding the presence of these impurities in some concentration in the grain boundaries is correct, then either the existing diagrams are not accurate in the room temperature region, or there is a difference in solubility in the grain boundaries as compared -with the grains. A study along these lines might be very revealing. (3) The undesirable effect of silicon in copper calls to mind our own observations on the influence of silicon on the stress corrosion cracking resistance of alpha brass. In this case, silicon was found to have a very marked beneficial effect, particularly when a heat treatment capable of producing a grain boundary constituent was used. I should appreciate it if in the discussion of your paper this point should arise, you would attempt to clarify the difference between the copper-silicon binaries and the copper-zinc-sili-con ternary alloys. D. H. THOMPSON and A. W. TRACY (authors&apos; reply)—(1) We have no data on the constancy of the carbon dioxide content of the air used for the test atmosphere but have believed that the normal carbon dioxide content of the air was as constant as could be obtained by using Edmunds&apos; method of removing carbon dioxide from the air and then adding a measured quantity. In any event, the test atmosphere was the same for all specimens in a test run. We agree with Mr. Anderson that the carbon dioxide content is important in the formation of a hygroscopic film on specimens. (2) We can imagine that there could be a concentration of solute atoms at the grain boundaries which would be so small that present methods would not detect it even if it exceeded the solubility limit of the alloy. There could be somewhat greater solubility at the grain boundaries for an interstitial solute. There is a possibility that phosphorus dissolves in this way but we believe that none of the other solutes studied does. In our present studies we hope to find out something about conditions at the grain boundaries of some of the systems mentioned in the paper. (3) Mr. Anderson points out that silicon brass, which has had a high temperature heat treatment followed by a quench. is highly resistant to stress-corrosion cracking. Although the test conditions used by Anderson* et al were different from our test conditions, it is noted that the silicon brasses which had not had the special heat treatment were less resistant to stress-corrosion cracking than copper containing approximately equal amounts of silicon. G. R. GOHN†—Nonferrous metallurgists and particularly, materials engineers, have been accustomed to thinking

Jan 1, 1950

By T. Sterry Hunt

I HAVE lately had occasion to examine sulphuretted ores of bismuth&apos; both from Tudor, Ontario, and Latete, New Brunswick. The former consisted chiefly of bismuth-glance, carbonated at the outcrop, and within associated with some metallic bismuth, iron-pyrites and graphite, in a quartz gangue. In the second locality, where it appears to be present in considerable quantity, the veinstone is also quartz, but the associates of the bismuth-glance are chalcopyrite and galena. The treatment of such mixed ores in the furnace for the extraction of the bismuth could yield only a very impure product, and in view of the high price of the metal I tried with success a wet method for the treatment of the ore, which is based on well-known chemical reactions, and may, in some cases, be advantageously used. The pulverized ore is dissolved by heat in commercial nitric acid, and the remaining gangue washed by displacement, first with a little strong acid (which is used to attack a fresh portion of ore) and then with a moderate quantity of water, which is added to the first solution. This, if the excess of acid be considerable, may be partially