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By Raymond C. Boettner

The present work had for its purpose: 1) the identification of crack nucleation sites in AISI 4340, quenched to martensite and tempered over a range of 'temperatures; and 2) the comparison of fatigue processes in AISI 4340 with processes observed previously in pure metals From constant def1ection-bending fatigue tests, martensite boundaries were identified as the favored crack nucleation sites in quenched and tempered AISI 4340. It, also, was concluded that the fatigue processes operating- in this lous-alloy steel were similar to Processes observed in pure tnetals. ALTHOUGH much engineering data has been accumulated on the fatigue properties of quenched and tempered martensitic steels,' fatigue as a process is not as well understood in martensite as it is in pure metals.' Important features of the fatigue process, such as the identity of the nucleation sites, have not been determined in the commercially important high-strength low-alloy structural steels. The present work had for its purpose: 1) the identification of crack nucleation sites in a low-alloy steel, i.e., AISI 4340, which had been quenched to martensite and tempered over a range of temperatures; and 2) the comparison of fatigue processes in the AISI 4340 with processes observed previously in pure metals. This comparison of the fatigue processes in the different tempers was restricted to the high-strain low-cycle part of the S-N curve. Under these test conditions, previous work on a number of metals has shown that a large number of cracks are nucleated in less than 30 pct of the fatigue life.3 Furthermore, crack nucleation sites are not restricted to inclusions but are also associated with intrinsic structural characteristics of the metal. MATERIAL A 20-lb ingot of vacuum-melted AISI 4340 (for composition see Table I) was hot-rolled to 1-in.-diam rod and then cold-rolled to a 1-in.-wide strip, 0.08 in. thick. Fatigue specimens, see insert of Fig. 1, were machined from the strip with the long dimension parallel to the rolling direction. m this orientation, the stringers of 1 to 2 p inclusions present in the sheet lay parallel to the stress axis in the specimens. The specimens were austenitited at 2050°F in order to obtain a large prior austenite grain size, i.e., 2 mm, which facilitated the subsequent identification of the prior austenite boundaries. A helium atmosphere was used to minimize decarburization. After austenitiza-tion at 2050°F, the specimens were transferred to a 1450°F furnace so that specimen distortion was held to a minimum in the subsequent oil quench. Previous work4 indicated that refrigeration in liquid nitrogen prior to tempering reduced the percentage of retained austenite in the quenched specimens to less than 5 pct. Tempering was carried out in air over the temperature interval of 200°to 800°F to produce a range of mechanical properties, Table I. The preparation of the fatigue specimen was completed by grinding about 0.005 in. from each surface and electropolishing in a chrome trioxide-acetic acid solution for 30 min. Examination of etched cross sections of specimens prepared in this fashion showed the foregoing specimen preparation to be adequate for the removal of the decarburized layer present after the heat treatment. Transmission electron microscopy showed that the as-quenched microstructure of this alloy consisted of a mixture of martensite plates containing either a high density of dislocations or microtwins. Previous work5'6 indicated that in the course of oil quenching autotem-pering resulted in the formation of E carbide on the martensite and microtwin boundaries. Tempering for 2 hr at temperatures up to about 400°F resulted in further precipitation of the E carbide. Finally, at about 400°F, cementite began to replace the E carbide on the martensite and microtwin boundaries in addition to forming a Widmanstatten structure within the plate matrix. EXPERIMENTAL S-N curves were obtained using electropolished specimens cycled at 1800 cpm as cantilever beams in fully reversed bending at selected constant deflections. The deflections were translated into surface strains by means of a calibration curve obtained through the use of strain gages. An argon atmosphere was used to minimize environmental effects. To investigate the development of fatigue slip bands, the specimens of the different tempers were unidirec-tionally bent to a surface strain of 0.005 to 0.007, photographed to record the location and appearance of slip bands so introduced, and then cycled to failure

Jan 1, 1968

By J. F. Radavich

Many heats of steel of low carbon value have been known to produce brittle pieces of steel. The brittleness is believed to be due to the impurities located within the grain boundaries. Such brittle steels have been examined with an optical microscope to ascertain the nature and the amount of the impurities present at the grain boundaries. Due to the relatively low resolving power of the optical microscope, the impurities are not visible in fine detail. The writer obtained some sheet steel and proceeded to determine the location of the impurities and to show the application of the electron microscope to the study of grain boundaries. One sample was known to be capable of becoming embrittled, whereas another sample was believed to be much less susceptible to embrittlement. Treatment of Specimens The specimens were embrittled by annealing above the A3 point under mildly oxidizing conditions. One piece of ingot iron could not withstand a 90" bend, whereas another piece of ingot iron was not affected and could withstand a 90" bend. The brittle piece was then annealed at a high temperature in a hydrogen atmosphere. The annealed ingot iron was termed cured and could withstand a 90" bend very easily. The three specimens examined will be designated as brittle, good. and cured in the discussion that follows. Procedure The sizes of the specimens were as follows: one piece of brittle ingot iron-3/8 by 35 in.; one piece of good ingot iron-96 by 1/8 in.; one piece of cured ingot iron-36 by 54 in. The specimens were too small to be polished by hand and therefore were mounted in bakelite. The polishing procedure was carried out in the conventional manner with the use of 1/0 through 3/0 papers, and the final polish was done with alumina on a billiard cloth. The specimens were then etched in a 4 pct solution of picral in alcohol, and then they were examined through an optical microscope. An area was chosen that showed distinct grain boundaries, and an effort was made to keep near this area when pulling the replicas REPLICA TECHNIQIJE The replica technique used in the preparation of the replicas for examination under the electron microscope is described in Electron Metallography.' It consists essentially of the following steps: 1. Obtaining a suitably etched specimen. 2. Applying a swab of ethylene di-chloride on the surface. 3. Applying a formvar solution on the surface. 4. Placing a screen on any desired spot. 5. Breathing on the fornivar layer. 6. Applying scotch tape on the screen and film. 7. Pulling the film and the screen up with the Scotch tape. 8. Separating the screen from the Scotch tape. This replica technique is very similar to the one described by Harker and Shaefer. However, with the added step, the percentage of replicas removed is very much higher regardless of the length of the time from the etching of the specimen to the actual pulling of the replica. The replicas were then shadow cast with manganese at a filament height to replica distance ratio of 1 1/2:7. This produced a very high contrast replica for use in the electron microscope. One of the dificulties encountered with this study was the restricted area of the specimen. The width of the specimens was the same as that of the 200 mesh nickel supporting screen. In order to increase the effective area, the screens were cut down as shown in Fig 1. The arrow indicates the direction in which the replica was pulled. This operation made it possible to obtain a large percentage of good replicas. Fig 3 shows an electron micrograph of a brittle piece of ingot iron and a grain boundary that was polished mechanically. The surface is very rough probably due to the incomplete removal of the flowed layer by the picral etchant. The grain boundary does show evidence of impurities. It was decided to electropolish the specimens to obtain a much smoother surface than the one obtained by mechanical polishing. ELECTROPOLISHING The specimens were cut in half to expose the metal on the back side. The exposed metal had sufficient area to make good electrical contact and electropolishing was carried out easily. The conditions for electropolishing were 0.9 amp, 35 volts, and 25 sec. in an electrolyte composed of 850 cc of ethyl alcohol, 100 cc distilled water, and 50 cc of perchloric acid. The polished specimens were then etched in the 4 pct picral solution for a shorter time than was necessary for

Jan 1, 1950

By G. W. Thomas

A mathematical tnodel of forward combustion in an oil reservoir is treated in this paper. The model describes a radial system having a vertical section of essentially infinite thickness, all of which is permeable to gas flow. Combustion, however, is presumed initiated over a limited thickness of the total vertical section. In the interval supporting cotnbustion, the mechanisms of radial conduction, convection and heat generation are taken into account. Above and below the burning interval, heat transport in the radial direction is by cottduction and convection. Vertical heat losses from the ignited interval are accounted for by conduction alone. A general solution is presented for the temperature distribution caused by radial movement of the combustion front. The results show that no feedback of heat occurs into the ignited interval when convection and conduction are acting in the bounding media. Peak temperatures are also 5 to 10 per cent higher than in the case where heat transport in the bounding media is by conduction alone. We arbitrarily define vertical coverage to be that fraction of the total ignited interval which is at 600F above atnbient, or greater, at any given time. The radial distance at which the vertical coverage becomes zero is the propagation range of the combustion front. It was found that an increase in vertical coverage results when the oxygen concentration, fuel concentration or gas-injection rate is increased. Moreover, the combustion front can be propagated 10 to 15 per cent further than in the case where only conduction is acting above and below the ignited interval. INTRODUCTION In the theoretical treatment of forward combustion in a radial system, one of the problems encountered is the determination of the transient temperature distributions caused by an expanding cylindrical heat source. Bailey and Larkin' and Ramey' simultaneously presented analytical solutions to the problem assuming heat transport by conduction alone. In a subsequent publication, Bailey and Larkin3 included the effects of both conduction and convection while treating linear and radial models. In this latter work, however, vertical heat losses were largely neglected. Selig and Couch' dealt with a radial model in which both conduction and convection were acting. Only a limiting case involving vertical heat losses was considered, however. Namely, temperatures on the boundary of the bed of interest were set equal to zero. Solutions thus obtained were representative of a system having a maximum vertical heat flux. Chu5 recently treated a more general case in which a permeable bed was considered bounded by impermeable media. Conduction and convection took place within the bed, and only conduction outside of the bed. The effects of vertical heat losses were included in his study. Solutions were obtained by numerical techniques. This paper is an extension of the theoretical work of other authors pertaining to forward combustion in a radial system. In particular, a mathematical model of the process is treated in which heat generation occurs over a small vertical interval of a larger permeable section. In the interval supporting heat generation, and above and below this interval, the mechanisms of radial conduction and convection are also presumed acting. Heat losses from the ignited interval are accounted for by vertical conduction. An analytical solution for the temperature distribution caused by radial movement of the burning front is presented. The effects of certain process variables are indicated and comparisons with Chu's results are made. THEORY To render the mechanism of forward combustion tractable to mathematical treatment, we idealize the problem to the extent of assuming continuous reservoir media possessing homogeneous and isotropic properties. The following additional assumptions are implicit in this analysis. 1. The thermal parameters, i.e., heat capacities, thermal conductivities and thermal diffusivities are invariant with temperature and pressure. Moreover, the bounding media possess the same thermal properties as the bed of interest. 2. The temperatures of the porous media and its contained fluids at any point and at any time are equal. 3. The reaction rate between the oxidant gas and the fuel is infinite. This assumption implies that the incoming oxygen concentration instantaneously goes to zero within an infinitesimal distance, i.e., the width of the combustion zone is negligible. 4. The rate of gas injection is constant and corresponds to the average rate throughout the lifetime of the project. 5. The fuel concentration is constant throughout the volume of rock swept out by the burning zone. 6. There is complete burnoff of fuel. This assumption demands that the rate of propagation of the burning front equals the rate of fuel burnoff. In a radial system, with a

By V. F. Zackay, W. A. Goering

ALLOYS of iron and aluminum up to 35 wt pct aluminum are single-phase solid solutions, and are of potentially wide applicability.1-3 In spite of early and continued interest1-4 little progress has been made until recently in the preparation and evaluation of sound alloys containing more than 6 wt pct aluminum. Vacuum-melting techniques for the production of ductile Fe-A1 alloys have been described recently.1-7 A. procedure for air melting these alloys is presented here. Low-carbon iron is induction melted without a slag in a rammed magnesia crucible. At the beginning of melt-down, aluminum pig (99.95 pct Al), charged in a clay-graphite bottom-pouring crucible is placed in a pot furnace at 1800°F. The primary deoxidation of the molten iron after melt-down is effected by the addition of 0.1 pct aluminum and 0.5 pct manganese. (Hilty and Crafts" have reported a significant increase in the deoxidation efficiency of the aluminum and manganese combination over that of the aluminum alone.) A more drastic deoxidation designed to reduce the oxyen content to the lowest possible level is accomplished by plunging metallic calcium to the bottom of the melt. This is done by wiring small cubes of the metal to a steel rod. A circular shield larger than the diameter of the crucible opening is attached to the rod so that any spa'ttering of the molten metal will not endanger the operator. Since the temperature of the molten metal is above the boiling point of calcium, the bath is vigclrously purged by calcium vapor. It is believed that the calcium-vapor treatment permits a homogeneous distribution of calcium in the melt. Owing to the vigor of the reaction the temperature of the molten metal should be kept below 2900°F prior to the calcium addition. A total of 0.05 pct calcium is added in two stages in this manner. The second calcium deoxidation is made just before charging the molten aluminum into the iron, in order that an excess of calcium be present for the remainder of the melt. The aluminum, which has been removed from the holding furnace, is then hydrogen degassed by bubbling chlorine through a quartz tube immersed in the molten aluminum. The hydrogen-chlorine reaction is an exothermic one preventing the solidification of the aluminum during the 5-min chlorination. Approximately 0.1 pct calcium, based on the amount of aluminum, is then added to the aluminum. A further excess of calcium is introduced into the melt in this manner. The oxide dross is removed, fluorspar is added to the molten iron, and the molten aluminum is poured through the fluorspar slag. The fluorspar should be dried thoroughly prior to its use, as any water present will react with the aluminum. Aluminum oxide formed during the pouring operation reacts with the fluorspar slag to form gaseous aluminum fluoride and calcium oxide. A forced-draft ventilating system is required for this operation as aluminum fluoride is toxic. As soon as the molten aluminum has been added, vigorous manual stirring of the melt is required because the slag-aluminum oxide reaction is highly exothermic and tends to take place near the top of the melt. The combination of high temperature and the slagging action of the fluorspar quickly erodes the crucible at the slag line if the aluminum is not stirred uniformly into the melt. It has been found that at least 4 min of manual stirring combined with induction stirring are necessary to ensure homogeneity. The power is shut off 1 min prior to pouring to allow metal and slag to separate. As much slag as possible is removed from the melt, which is then poured directly into cast-iron molds. A mold wash of aluminum oxide is used to prevent ingot sticking. For slab ingots which are to be rolled into sheet, a carbon-tetrachloride vapor atmosphere or a chlorinated-pitch mold wash is desirable, as the aluminum oxide formed in the pouring operation is subsequently removed by the chlorine in the presence of carbon." As in vacuum melting, a pouring temperature of about 2900°F is recommended. Adequate hot-topping is important as iron-aluminum ingots are subject to very deep piping. Ingots are removed from the molds and buried in vermiculite, where they are allowed to cool slowly to room temperature. The ingots are radiographed,

Jan 1, 1959

By S. G. Cupschalk, J. J. Wert, R. A. Buchanan

The uniaxial deformation of thermally ordered and disordered polycrystalline Cu3Pt was studied by means of the X-ray line - broadening analysis according to Warren and Averbach and the extension of this analysis to ordered fcc materials by Mikkola and Cohen. Because of the heat treatment history, extinction had a pronounced effect on the X-ray spectra of ordered and disordered C%Pt at small plastic strains. After an appropriate correction for extinction, the long-range order in thermally ordered ChPt was found to decrease at a slow constant rate with plastic strain. Furthermore, the antiphase domain probability increased at a constant rate to 17.5 pct strain. The effective particle size behavior indicated that the stacking fault energy is lower in ordered than in disordered Cu3Pt. Analysis of the stress-strain curves shouled that ordered Cuzt has a slightly lower yield Point but a much higher work-hardening rate than disordered Cu3Pt. THE presence of long-range order in a solid-solution alloy has a marked effect on its mechanical properties. While this effect has been known qualitatively for many years, it was not until recently that detailed investigations have been performed to determine the exact role long-range order plays in this strengthening mechanism. The development of an advanced, quantitative. X-ray diffraction analysis by Warren and Averbachl and the extension of this analysis to the L1, type super lattice by Mikkola and cohen2 have greatly accelerated research in this field. The research reported in this paper consisted of two primary phases. The first phase was to determine the effect of long-range order on the tensile properties of polycrystalline Cu3Pt. This objective was accomplished by comparing the stress-strain behavior of thermally ordered CusPt to that of thermally disordered CusPt. The second phase of the research was to determine the difference between the atomic arrangements in thermally ordered and thermally disordered Cu3Pt as a function of uniaxial deformation and thereby gain a deeper insight into the mechanism by which long-range order affects the tensile properties. This second objective was accomplished by applying the Warren-Averbach method of peak profile analysis to the X-ray diffraction patterns obtained from ordered and disordered Cu3Pt after given amounts of uniaxial deformation. EXPERIMENTAL PROCEDURE The Cu3Pt was prepared by vacuum melting and casting. After a homogenization anneal, the ingot was cold-rolled to sheet form. Two tensile specimens with gage sections of 2.50 by 0.500 by 0.115 in. were carefully machined from the sheet. The specimens were polished with a final step of 600-grit paper to insure smooth diffracting surfaces. Finally, one specimen was heat-treated to yield an average grain diameter of 0.016 mm and an initial degree of long-range order, S, of 0.825. The other specimen was water-quenched from above the critical temperature, 645"C, to yield an average grain diameter of 0.017 mm and zero long-range order. The heat treatment history of each specimen is shown in Table I. The tensile tests were performed utilizing a Research Incorporated Model 900.95 Materials Testing System. This unit employs a closed-loop feedback system which maintains a constant strain rate through an extensometer clipped to the gage section of the tensile specimen. A strain rate of 1.32 i0.02 x 10"4 sec-' was employed in testing both specimens. In the X-ray diffraction analysis, a General Electric XRD-5 diffractometer equipped with a pulse-height analyzer set for 90 pct efficiency was employed. The goniometer speed selected was 0.2 deg, 20, per min. Filtered Cu radiation was used for all peaks and all peaks were chart-recorded. Because of nonuni-form grain size. it was necessary to spin the specimens during X-ray analysis in order to obtain reproducible integrated intensities. The spinning rate was 2000 i100 rpm. The application of the Warren-Averbach method of peak broadening analysis to a diffraction pattern is very time consuming if done manually. In this research, the calculations involved were performed with the aid of a computer program by wagner.3 As reported by Wagner, the program is written in Fortran TV computer language. It was modified to Fortran I1 so as to be handled by the IBM 7072 computer at Van-derbilt University. In the X-ray diffraction analysis of uniaxially deformed Cu3Pt, the 100, 200. 400. 111, and 222 reflections were recorded from the initially ordered sample after 'plastic strains of 3.0, 6.0, 9.0, 12.0,

Jan 1, 1970

By R. C. Himes, K. Zanio, J. B. Wagner, J. W. Moody, J. F. Miller, W. Johnson

The recent research with which this paper deals has been concerned with the preparation of pure PbTe crystals suitable for control of radiative processes and othe.v electronic applications. The research has been directed toward the developrnent of methods for the preparation of puve, homogeneous, loul-ca,wier-density PbTe crystals suitable for use in the fabrication of optically pumped and electrically pumped diode lasers. Steps in the preparation of the crystals include 1) purification of the starting materials, 2) synthesis and purification of the PbTe, 3) growoth of PbTe crystals, and 4) adjustt~zertt of composition of the crystals This Paper describes the general preparation procedure employed and discusses some investigntiotzs of purification processes. THE as-received lead and tellurium are nominally 99.999 to 99.9999 pct pure. Assays furnished by the suppliers, obtained by emission spectrographic analysis, show only the presence of about 2 ppm Mg in the tellurium. Such analyses are not very informative, however, since they give no information on the concentrations of normally gaseous impurity elements such as oxygen. Both the lead and the tellurium in the as-received state usually contain appreciable concentrations of oxygen—primarily in the form of oxides on the surfaces of the material. To reduce the oxygen content, the lead is held in the molten state in hydrogen at -700°C for several hours. For this treatment, the lead is contained in a graphite boat which is rf-heated, and the hydrogen is passed through a liquid-nitrogen trap prior to use. Tellurium is subjected to multiple distillation in hydrogen to remove oxygen and other foreign impurities. If, in conducting the distillation, approximately the last 10 pct of the charge at each "stage" is left as the discard cut, purification of the tellurium proceeds as indicated in Fig. 1.l Tellurium used in this work has been distilled two or three times to reduce carrier concentration to about 10" per cu cm. The PbTe is prepared from the purified elements by reacting them in the molten state in sealed, evacuated, or hydrogen-filled silica ampoules. The charge is usually held above the melting point of PbTe (923°C) at 1000 C for 24 hr to ensure that it has been homogenized. Two methods have been employed for the growth of the required single crystals of PbTe: growth from the melt, which will be discussed first, and growth from the vapor phase. Large single crystals of p-type PbTe can be grown readily from the melt by the Bridgman method. For this method of crystal growth, the PbTe is synthesized in situ from proper proportions of the purified elements. Growth (dropping) rates in the range 1.3 to 6.5 mm per hr are employed. Material near the maximum melting composition (about 50.012 at. pct Te) is utilized to avoid composition change on freezing, and thus to obtain crystals of nearly uniform composition. Crystals prepared by use of procedures described up to this point were sufficiently pure and perfect that they could be used for the preparation of laser crystals in studies at Lincoln Laboratory.2-5 ADJUSTMENT OF COMPOSITION Good n-type crystals of PbTe cannot readily be grown from the melt. Further, growth from the melt of crystals of any compositions (n or p type) other than those near the maximum melting composition is difficult because of the large composition changes that must occur on freezing.'" However, melt-grown crystals can rapidly be brought to other desired compositions by isothermal equilibration through the vapor phase with a two-phase Pb-Te stock material, essentially as described by Brebrick and Allgaier.1 The work to be discussed has been concerned with the preparation of n-type crystals; thus, the two-phase stock which was employed contained excess lead, and all ensuing discussion is of the preparation and properties of n-type crystals. The equilibration was designed to the shift composition to the lead-rich limit of stability at the selected temperature. Initial treatment of the crystals at high temperature was employed to minimize the total time required for the equilibration. Final adjustments of the composition and state of the crystals were made by use of low-temperature heat treatment at temperatures in the range 200" to

Jan 1, 1968

By W. M. Wojcik, R. F. Kowal

Oxygen and sulfur distributions in commercial, 5-ton ingots of killed, medium carbon steel are described. Oxygen distribution is found to vary with deoxidation practice. Irregular distribution of oxygen within ingots makes necessary special precautions in sampling of rolled products for analysis of oxygen. Oxygen distribution is discussed in terms of recently published solidification concepts which had been successfully applied to simpler cases of segregation. These concepts have been found inadequate to explain observed oxygen distributions. Convective movements of the liquid metal, as determined by tracer elements, are shown to be capable of accounting for the observed distributions of oxygen. IN an effort to explore the origin of surface and subsurface imperfections in pierced steel products, a study of oxygen and sulfur segregation was made on ingots cast in open-top and hot-top molds. The results of our previous investigations1"3 have indicated the importance of the location and amount of oxide inclusions in an ingot. Inclusions close to the surface of the ingot have been found to contribute greatly to the formation of imperfections in the surface of finished products. This study of the effects of deoxidation and casting practice on segregation and the resulting oxygen distribution in ingots was initiated to determine the parameters controlling the location of inclusions in an ingot. Segregation of solute elements during solidification of low-melting binary alloys has been studied in the past.1, 5 Formation and growth of inclusions in iron melts have been studied under specific conditions."- In spite of these and other recent studies,10-12 segregation during solidification of commercial, killed steel ingots is not well understood. Consideration of solidification rates, of segregation during solidification of the chill, dendritic, and central zones, and of material balances for the segregated elements has indicated that a simplified theoretical solidification model is not adequate. However, the observed high oxygen contents in localized volumes of the dendritic zone can be rationalized if additional effects of convection currents in the ingots, precipitation, and rapid growth of new phases are considered. EXPERIMENTAL PROCEDURE Steelmaking and Processing. A group of nine killed. medium carbon steel heats having compositions listed in Table I have been studied. The deoxidation and mold practices used were varied to give a wide range of steel oxygen contents. The amounts of aluminum added to the ladle and the ingot casting practices (hot top and open top) were the main variables. The steel was made by a duplex practice in 160-ton tilting basic open-hearth furnaces. All nine heats were top-cast into 24 by 24 in. big end down, fluted molds, to a height between 60 and 76 in., using both open tops and exothermic hot tops. The deoxidation practice and the tapping and teeming details for each heat and ingot studied are given in Tables II and III, respectively. Hot-top practice is indicated by the letter H following the heat designation. Furnace and ladle temperatures were measured by standard disposable-tip, Pt/10 pet PtRh thermocouples. Teeming-stream temperatures were obtained as described by Samways et al.,13 by immersing a Pt/10 pet PtRh thermocouple, covered by a silica sheath, into the teeming stream under the nozzle. The output of this thermocouple was recorded with Leeds & Northrup Speedomax potentiometer. Calibration of the latter thermocouples was based on the freezing point of a pure iron/oxygen alloy (2795°F). The accumulated errors of measurements were within ±10°F. The thermocouple measurements were supplemented in this investigation by continuous recording of a ratioing, two-color pyrometer (Shawmeter), protected from smoke by a blast of clean air within the sighting tube, and calibrated to read with better than ±10°F accuracy. Following teeming of three heats, P, R, and T, tracer elements were added to the steel in the molds to obtain a record of the progress of solidification. As soon as the teeming stream was shut off, a 0.010-in.-thick steel can containing a mixture of crushed standard ferro-titanium and ferro-vanadium (0.05 pet of each alloy element) was plunged into the middle of the steel pool to a depth of 6 in. In about 30 sec no indication of the can or its contents remained. The surface of the open-top ingots solidified in 20 to 30 sec. A study of liquid metal movement and the precipitation of oxides was facilitated materially by use of the tracer technique as titanium has a low distribution coefficient between solid and liquid steel while vanadium has a high distribution coefficient.

Jan 1, 1965

By K. Tanaka, J. D. Mote, J. E. Dorn

It) an attempt to ulLcoce.lP the operative strain-rate-contl-olliy: dislocation nieclzanistns, specially oviented sizgle clystals of the intel-nzediate 1zexagonal phase containing Ag plus 33 at. pct A1 were tested in tension over a wide range of temperatures. Slip was observed to take place by the {0001} <1120> {l100} mechani fracture took place across the(i100) plane and winning occurred by the (i01Z) ?lechanisn. Basal slip exhibited a strong yield point over the -alzge from 77 to 450°K, the upper ,esolved shear st]-ess having the exceptionally high value of 10,500 psi over this entire ?-a?zge of tenzpei,atuves. The critical 9-esolved shear stress for prismatic slip decreased f7-om 48,000 psi at 4.3"K to 23,000 psi at 170°K (Region 1) follozcirg zt:lzich it decl>eased sloz&ly to 21,500 psi at 475°K (Res&apos;on II); from 475" to 575°K (Regioz III), the c7-itical esolced shear stress dec&apos;-eased precipitously to 2000 psi; and from 575" to 750°K (Region IV) it decreased less afi&apos;dly to a low value of about 500 psi. Pvistintic slip in Region I was pobably controlled by the tliel-nally activated riecharzisui of nucleation and g,-ozcth of kinks in dislocations lying in Peierls potential troughs. In Region II for prismatic slip the critical 1-esolved shear stress was slzocn to be deteemined by sh0l.t-range 01-dering, Overall the forgiorz fo basal slip, 7.c.lre1-e a Strong yield-point phenorlienu ia7as observed, the critical vesolved slzea?-stress was shoztn to be determined by n conibirzation 0-f Szizuki locking and short-range-order Izavderzizg, The precipitous decrease in the critical resolved shear stress with increase in ter,/pe7-atrir-e over Region HI was tentatively ascribed to a decrease in the degree of slort-)ange 07-del;iqq (0)- clusteing) and also the effect of fluctuations the degree of o?der, It is at pgreser2t zrtzce)taitz as to 1t1hethe1- these or other possi1)le effects are also ,esponsible. fo- the data obsel-ved 172 Region IV. 1NTEREST in inter metallic compounds stems not only from their role in dispersion hardening of polyphase alloy ystems but equally from their potentialities for high strength, hardness, and stability not only at atmospheric temperatures but especially at elevated temperatures. As summarized in a re- cent symposium of the Electrochemical Society on "Mechanical Properties of Inter metallic Compound", most of the experimental evidence regarding the mechanical behavior of intermetallic compounds centers about the effect of temperature on the hardness and ductility of polycrystalline specimens. The available data reveal that the plastic behavior of intermetallic compounds might be rationalized in terms of the usual dislocation mechanisms appropriate to a solid solutions providing the additional complexities arising from crystal structure, long-range ordering, short-range ordering, and defect lattices are taken into consideration. It is apparent, however, in terms of the history on a solid solutions, that a complete detailed mechanistic rationalization of dislocation processes may not be possible until the deformation processes are studied in single crystals of intermetallic compounds. The present paper contains a preliminary report on the plastic behavior of single crystals of the hexagonal Ag-A1 intermetallic phase over a wide range of temperatures. The results confirm the thesis that single crystal data provide a most effective method of identifying operative dislocation mechanisms in intermetallic compounds. EXPERIMENTAL TECHNIQUES Several factors prompted the selection of the hexagonal Ag-A1 intermetallic phase for this preliminar investigation on the plastic properties of single crystals of intermetallic compounds: 1) This phase has a wide solubility range5 which would permit future investigations on the effect of composition and axial ratios on slip mechanisms. 2) Although it undoubtedly exhibits short-range ordering (or clustering) this intermetallic phase is free from complexities arising from long-range ordering.6 3) Since the atomic radii of aluminum and silver are practically identical, the possible complications due to Cottrell locking are minimized. 4)Whereas the dislocations on the basal planes are expected to dissociate into Shockley partials and are thus susceptible to Suzuki locking, those on the prismatic planes probably remain complete. 5) The axial ratio, being 1.61, is almost ideal, suggesting that short-range ordering may be almost spherically symmetrical. The present investigation was conducted exclusively with the hexagonal Ag-A1 alloy containing 33 at. pct Al. Preliminary investigations revealed that this alloy undergoes basal slip by the (0001)

Jan 1, 1962

By Voyle R. McFarland, Robert A. Burmeister, David A. Stevenson

The distribution of lead between phases in the Ag-Sb-Te system was studied using microautoradio -graphy. Two compositions were investigated, both containing an intermediate phase Known as silver antimony telluride as the major phase, and one containing AgzTe and the other SbzTes as the minor phase. For both compositions, two thermal treatments were used: nonequilibrium solidification from the melt and long equilibration anneals of the as-solidified structure. For each composition, lead was segregated in the minor phase of the as-solidified structure, but was distributed in the matrix after anneal. The electrical resistivity and carrier type were insensitive to the distribution of lead in the two-phase structure. ThERE has been considerable interest in the Ag-Sb-Te system because of its thermoelectric properties. The major interest has been in compositions on the vertical section between AgzTe and SbzTes, particularly the 50 mole pct SbzTes composition AgSbTez (compositions are conveniently expressed as mole percent SbzTes along the AgzTe-SbzTes section). One of the major problems in the proper evaluation and utilization of this material is the inability to control the electrical properties through impurity additions: all alloys prepared to date have been p-type, even with the addition of large amounts of impurities. It has been shown Wit all the compositions previously studied contain an intermediate phase of the NaCl st&apos;ructure as a major phase (denoted by b) and a second phase, either AgzTe or SbzTe3, as a minor phase.&apos;-3 One explanation for the unusual electrical behavior of this material is that the impurity additions have a higher solubility in the second phase than in the matrix; the impurity would segregate to the second phase, leaving the bulk matrix essentially free of impurity.4 In order to investigate this mechanism with a specific impurity element, the distribution of lead between the two phases was determined using autoradiography. Lead 210 was chosen because of the suitability of its 0.029 mev 0 particle for autoradiography and also because of the interest in lead as an impurity in this system.5&apos;6 EXPERIMENTAL PROCEDURE Two compositions were taken from the vertical section between AgzTe and SbzTes, 50 mole pet SbzTes (Viz. AgSbTez) and 75 mole pct SbzTes, in which AgzTe and SbzTes appear, respectively, as the minor phase. Lead containing radioactive lead (pb210) was added to the above compositions to provide a concentration of 0.1 wt pct Pb. The material was placed in a graphite crucible in a quartz tube which was then evacuated and sealed. The samples were melted and solidified by cooling at a rate of 8°C per min and then removed and prepared for microa~toradiography. After autoradiographic examination of these samples, they were again encapsulated and annealed in an isothermal bath at 300°C for a number of days and prepared for examination. An alternate method of preparation employed a zone-melting furnace; the molten zone traversed the sample at a rate of 1.2 cm per hr and the solid was maintained at a temperature of 500°C both before and after solidification. This treatment had the same effect as solidification at a slow rate followed by an anneal for several hours at 500°C. In order to obtain the best resolution, thin sections of the alloy were prepared by hand lapping to a thickness of approximately 20 p. Other samples were prepared for examination by lapping a flat surface on the bulk sample. The resolution, although somewhat better in the former procedure, was adequate in both instances and the majority of the samples were treated in the latter fashion. A piece of autoradiographic film (Kodak Experimental SP 764 Autoradiographic Permeable Base Safety Stripping Film) was stripped from its backing, care being taken to avoid fogging due to static-electrical discharge. A small amount of water was placed on the sample, the film applied emulsion side down on the surface of the sample, and the sample and the film dipped into water in order to assure smooth contact. After drying, the film was exposed for 2 to 5 days, the period of time selected to give the best resolution. The film was developed on the specimen and fixed and washed in place. Two major factors must be considered in establishing the reliability of an autoradiograph: the in-

Jan 1, 1964

By W. Allen

FOR the past six years gravity surveys have been used for underground prospecting in the copper mines at Bisbee, Ariz. The primary purpose of the surveys has been to reduce the diamond drilling and crosscutting necessary for exploration. Since many of the orebodies are small, and geologic control is not always apparent, any information that will direct the drilling and crosscutting is highly desirable. Because of extensive development and exploration work in the copper mines at Bisbee, it has been possible to cover more than 630,000 ft of crosscuts on 30 levels with the gravity surveys. In the process the gravity procedures have been refined to a high degree. Density Contrast: For a gravity survey to be successful, a sufficient density contrast must exist between the geologic feature sought and surrounding host rocks. Most mineralized areas will provide this contrast if fairly massive bodies are present. In the Bisbee area the entire sequence of formations, except for alluvium, appears to have specific gravities ranging from 2.65 to 2.70. These values have been determined by means of a large number of cut samples and diamond drill cores. As a further check, vertical gravity differences have been used where nonmineralized sections are known to occur.&apos; The only known major gravity disturbances result from mineralization that has increased the density and the voids that have decreased density. The voids are caused by mining operations and by underground water movement that has developed several areas of caverns. Equipment: While not absolutely essential, a small rugged gravity meter, such as the Worden meter, is highly desirable. A tall tripod, about the height of a transit tripod, permits instrument set-ups in deep water and in locations where fallen timber and muck piles make it impossible to use a short tripod. An additional advantage of a tall tripod is that it places the meter in the center of the crosscut, reducing the error caused by the crosscut void. Size and weight are important, since the only satisfactory means of operating the meter underground is to carry it by hand. A backpack can be used in rare instances but is usually a hindrance because of the close station spacing. The operator&apos;s ability to move through tight clearances will improve survey coverage, as it is then possible to move through raises and caved areas and to pass mine cars and machinery with a minimum of trouble. Station Control: Gravity stations are normally located every 100 ft along the crosscuts, at each intersection, and in the face of all stub crosscuts. In areas of high gravity relief, or where small anomalies might be expected, stations may be located at 25 or 50-ft intervals. When possible, the stations should be offset to avoid effects of raises or other voids. The gravity stations on a level are tied to one or more base stations, which are usually located at the shaft or near the portal of an adit. The base stations may be part of a gravity control net that extends to each level in the mine as well as to the surface. Such a net extending throughout the potential area of the surveys is highly desirable, as it is then possible to compare all gravity stations on a uniform basis. The stations that are part of the base net should be carefully established by multiple readings and, if necessary, by a least squares adjustment of the loops. In some instances where levels do not have a shaft station, or where access may be blocked by caving, it may be necessary to establish secondary bases at the top and bottom of the raises that are between levels. Under fair conditions 70 to 90 gravity stations can be located and run in 6 hr by a two-man crew. The best field procedures depend on conditions. Reduction of Field Data: Most of the time required to produce a final gravity map is consumed in processing the data. Each meter reading must be corrected for a minimum of five factors that affect the gravity value in addition to the density contrast being sought. These factors are 1) instrumental drift, 2) station elevation, 3) topography, 4) latitude, and 5) regional gravity gradient. Mine openings, such as stopes and raises, will affect the value. However, it is seldom practical to make corrections for these voids. Usually a rotation is made on the field note on the station, and any

Jan 1, 1957

By David S. Bolin

INTRODUCTION This paper is directed toward those companies or individuals who may be considering the possibility of tin exploration or development projects in South America. Although tin deposits are known in many countries of Latin-America including Argentina, Peru, and Mexico, the majority of the deposits are located in Bolivia and Brazil. These two countries also account for virtually all the current production. Many factors affect the economic decisions related to mining and exploration projects in this region including the following: 1) Types of deposits 2) Anticipated size and grade of deposits 3) Deposit geometry and ore distribution as it affects the selection of a mining method 4) Metallurgical amenability 5) Governmental policies 6) Taxation 7) Anticipated capital and operating costs 8) Marketing costs This discussion will be directed toward each of these points. The majority of the presentation will be concentrated on Bolivia as this country is the principal producer in the region, however, the potential for further tin development in Brazil is excellent. Due to the remote and previously almost inaccessible location of the stanniferous districts of Brazil, little is known with respect to size and type of non-alluvial deposits which may exist in this vast country. TYPES OF DEPOSITS Two major types of deposits are currently being exploited in Bolivia; alluvial, and hard rock or lode deposits. Bolivia produces substantial tin from both types of deposit whereas virtually all Brazilian production to date has been from alluvial sources. Alluvial Deposits Brazil: The alluvial tin deposits of Brazil are located in river channels and flood plains adjacent to low mountain ranges. The terrain containing the tin placers is flat, marshy, and generally jungle covered. The major controls of alluvial cassiterite concentration are the ancient and present stream channels. The average tin concentration in the placers varies from 500 grams to approximately 1.0 kilograms per cubic meter. Tin reserves in the Rondonia field of Brazil have been estimated at 600,000 tons of fine tin. A bucketwheel suction dredge went into production in the Rondonia district in 1979, and four others have since been ordered. Several other gravel pump, and hand mining operations are also in production in this field. In addition to the Rondonia district, tin occurrences are known from Xingu, in Para state, and in the state of Minas Gerais. Bolivia: The alluvial deposits of Bolivia are somewhat more complex due to the variable geomorphology and abrupt topography. Conventional placer accumulations of cassiterite are found in many stream channels and intermontane basins surrounding the major lode tin producing regions. In addition to stream and valley placers, a group of deposits locally referred to as "Pallacos" or "Llamperas" which consist of colluvium, landslide debris and glacial moraine material, contain substantial tin reserves in some areas. The stream channel and intermontane basins contain the only deposits which are presently being exploited by mechanized methods. One dredge is working the stream channel below Cerro Rico de Potosi and another is operating in an intermontane basin southeast of the city of Oruro. Both of these dredges are operated by private companies. The average grade for these operations varies from 250 to 500 grams per cubic meter. The largest of the intermontane basin placers known at present is the Centenario deposit located adjacent to the Catavi lode deposit. This deposit contains approximately 170 million cubic meters of material with an average grade of about 150 grams per cubic meter. The "Pallacos" deposits are found on the slopes of mineralized areas and in glacial moraine. The mineralized material is generally completely unsorted, with tin and sometimes tungsten values distributed erratically throughout the entire mass. Most of these deposits are worked by small leasors or cooperatives; however, at least one mechanized washing plant is in operation southeast of Oruro. The size of these deposits may reach up to several million cubic yards. Grades are very erratic, but may range from 200 to 500 grams per cubic yard. In addition to the formal mining operations, virtually every drainage surrounding the major mines is being worked by independent&apos; miners utilizing hand mining and jig or pan concentration. The aggregate production from these operations is substantial. The

Jan 1, 1982

By Chas. A. R. Lambly

In the extreme northeast corner of the State of Washington, on the Canadian border, lies the Metaline mining district. This district is old in history, but young in production. Geology The Metaline district is a zinc-lead area of the replacement type in dolomite and limestone. The ore bodies of the Josephine horizon are in many ways similar to the ore bodies of the famous Tri-State zinc fields. The beds are faulted and folded and have varying low dips in varying directions, and underlie large areas of the district. History Production started in 1927 on a very limited basis. The property is now mining and milling 700 tons per day. The mine is opened by adit tunnels and a vertical shaft. As the ore horizons gained depth, it was necessary to sink inclines to follow the ore horizon (see Fig 1). From 1927 to date, approximately 600,000 ft of diamond drill was put down This work indicated that suficient tonnage existed to justify a redesigning of the whole operation, surface and underground. After four years of general study, the following program was planned: 1. A new mine entrance, which would be an incline, that could follow the ore body down at whatever pitch was necessary. The incline will be equipped with conveyors for the moving of ore and waste to the surface and with tractor-type locomotives for man and supply transportation. 2. The new incline also required a new type of mining which was developed and is now in use. It is called contour mining and will be described in a future paper. 3. The new incline exit would necessitate the moving of the mill and mine shops across the Pend Oreille River. This part of the program is now underway. The Incline The sinking of the incline was to start as soon as World War II ended and was as follows: The first leg of the incline was to be sunk from the surface 1600 ft on a 17" slope. The collar and first level at elevation 2180 ft, the second level at elevation 2000 ft, the third level at elevation 1875 ft, and the fourth level at elevation 1700 feet. From the 1700 ft elevation the incline was to flatten out to 12" for 400 ft to give the necessary depth for the ore pockets below the 1700 ft level and the necessary clearance for future sinking (see Fig 1 and 2). Due to lack of manpower in 1946, the program was changed and was as follows: A drift was driven from the old mine workings on the 1700 ft elevation in an easterly direction. At 1300 ft the drift was turned N 50" E and at this point a raise was driven 180 ft on a 50" slope. This raise intersected the Josephine horizon and commercial ore was encountered. At the 2000 ft mark, a main raise was driven, 245 ft on a 50" slope, and the 1875 ft elevation was cut. Exploration drifts were started on this level and production followed on a limited basis. The main drift at the 2500 ft point was turned N 35" E and ran parallel to and 10 ft east of and under the proposed incline line. At the proposed intersection of the drift and incline on the 1700 ft elevation, it was planned to raise the incline to intersect the 245 ft raise and to continue on to the surface, a distance of 1600 ft. When this proposed intersection point was reached, a heavy flow of water, approximately 800 gpm, was encountered and all work on the main drift face was stopped. This water flow flooded the main pump station in the old mine and the two lower levels with approximately 20,000,000 gal of water. The water was controlled and finally drained from the cave areas and lower levels after six months of pumping. After the heavy flow of water was encountered in the main heading, it was decided that the incline would have to be started from the surface, as originally planned, so that too much time would not be lost. The surface overburden had to be removed, a total of 6000 yards. A temporary dry house for 6 men was built. An 8 in. churn drill hole was intersected in the first raise driven from the 1700 foot elevation tunnel. Air and water lines were placed in this hole, and air and water were delivered to the collar of the incline from the mine working. The incline started down at 15 ft wide and 7 ft high through the Leadbetter slates. After sinking 4 sets, it was

Jan 1, 1950

By W. F. Chiao, R. B. Gordon

Tile sharp-yield point found in magnesium crystals in the solulion-treated and aged condition is studied by dislocation internal-friction experiments. The results show that the sharp yield is not file to the sudden release of pinned dislocations hut is movc likely due to the rapid multiplication of an initially small number of dislocations. Recovery or the dislocation internal friction after deformation is also studied. This yecovery results from the re-pinning of dislocations by a solute, presumably nitrogen, which moves with a relatively small activation energy. SHARP-yield points, when they occur, are a striking feature of the stress-strain curve generated during a tensile test. Although commonly associated with steel, sharp yielding has been found in a variety of metallic and nonmetallic crystalline materials. In particular, sharp-yield points have been found in zinc"&apos; and cadmium3 containing nitrogen. With this background, Geiselman and Guy4 investigated the tensile properties of magnesium single crystals containing nitrogen to see if sharp yielding also occurs in this system. They found that sharp yields did indeed occur in solution-treated and aged specimens tested at elevated temperature but were not able to give conclusive proof that the sharp yield was caused by nitrogen, a yield drop being observed even in their purest crystals. Sharp-yield points have also been found in various polycrystalline magnesium alloys.7&apos;8 In the study of the sharp-yield phenomenon it is desired to observe the behavior of dislocations in the earliest stages of the deformation process. Internal-friction experiments are useful for this purpose because dislocation damping is sensitive to the mobility of free-dislocation segments. At low strain amplitudes the damping, A, due to the the forced vibration of dislocation segments of average length L is ? =KAL4 [1] where A is the dislocation density and K, if the applied frequency is well below the resonant frequency of the dislocation segments? is a constant for the sample under observation.5 Dislocation damping, because of the fourth-power dependence on L, is particularly sensitive to the creation of free-dislocation segments during deformation. Since sharp yielding is associated with the sudden release of pinned-dislocation segments, marked changes in the dislocation damping are expected at the yield point.6 The use of the dislocation-damping observations to help elucidate the incompletely understood mechanism of yielding in magnesium is the primary objective of the experiments reported here. PROCEDURE Many investigations have shown that very marked and rapid changes occur in the dislocation damping of of a deformed material as soon as the straining is stopped.5 It was quite essential, then, for the purpose of this investigation, to make the damping measurements during the deformation of the samples. This can only be accomplished through the use of the ultrasonic-pulse method. In this method traveling sound-wave pulses are used and, in contrast to resonating-bar methods, only the sample ends are set in vibration. Thus, the sample can be gripped along its sides in the tensile-test machine without disturbing the damping measurements. In the pulse method, the decrease in the amplitude of a sound pulse is measured as it travels back and forth through the sample. If A is the amplitude after traversing a distance x and A. is the initial amplitude, A=Aoe-ax [2] and a is called the attenuation. It is commonly measured either in units of cm-I or as db per µ sec. The observed attenuation in a metal sample is due to a number of causes. These include scattering by grain boundaries and impurity particles, thermo-elastic damping, diffraction effects, stress-induced ordering of solute atoms, and dislocation damping. The total observed attenuation in a given sample usually cannot be resolved into these various components, but changes in a due solely to changes in dislocation damping can be accurately determined, provided the experiment is arranged so that all other sources of damping are held constant. It is desired to reduce the extraneous sources of attenuation to a minimum and for this reason the experiments are done on single crystals of high purity. Magnesium crystals offer the further advantage that, when properly oriented, only a single set of slip planes is active during deformation. Crystal Preparation. The method of sample preparation is similar to that of Geiselman and Guy.4 The starting material was high-purity, sublimed magnesium rod supplied by the Dow Chemical Co. Melting under Dow 310 flux was used to reduce the nitrogen content of the starting material: the fluxing was done under an argon atmosphere and the

Jan 1, 1965

By H. C. Rogers

A phenomenological study of the failure of polycry stalline ductile metals at room temperature was carried out using light and electron microscopy. Tensile fractures as well as sections of partially fractured bars of OFHC copper in particular were examined. The initiation and growth of the central crack in the neck of a tensile specimen occurs by void formation. After the formation of the central crack the f&apos;racture may be completed in either of two ways: by further void formation or by an "allernating slip" mechanism. The first leads to a "cup-cone" failure; the second, to a "double-cup" failure. In the past decade or decade and a half there has been a great deal of emphasis on the solution of the problem of the brittle fracture of metals, particularly those which normally exhibit considerable ductility such as steel. Since the problem of the fracture of metals after large plastic strains has less immediate commercial or defense significance, there has been considerably less effort expended in describing the details of the phenomenology and determining the mechanism of this type of fracture. The present research was undertaken to increase our knowledge in this area. The problem of ductile fracture has not been neglected completely, however. Ludwik1 first found by sectioning a necked but unbroken tensile specimen of aluminum that fracture began with a large internal crack which appeared to have started in the center of the neck. Examination of the fracture indicated that the crack had propagated radially with increasing deformation until a point was reached at which the path of the fracture suddenly left this transverse plane and proceeded at approximately 45 deg to the stress axis until the surface was reached. This gives rise to the commonly observed cup-cone tensile fracture. When MacGregor2 was attempting to demonstrate the linearity of the true stress-true strain curve from necking until fracture, he found that copper was anomalous in that the stress dropped off markedly from the straight line value before fracture occurred. Radiography indicated that in the copper an internal crack was formed long before the final fracture, the stress decreasing during the growth of this crack. One of the most significant advances in the understanding of ductile fracture was the result of work by Parker, Flanigan, and Davis.3 By the use of etch-pit orientations they were able to demonstrate conclusively that the fracture surface at the bottom of the cup, although on a gross scale normal to the tensile axis, did not consist of cleavage facets as had been previously supposed by many investigators. Recently, Forscher4 has shown evidence of porosity near the tensile fracture of hydrogenated zirconium which he attributes to hydride decomposition. The workers at the Titanium Metallurgical Laboratory5 have also shown evidence of porosity in a number of the commonly used metals after heavy deformation. Many metals have relatively low ductility during creep tests at high temperature. The fractures are intercrystalline, resulting from the nucleation and growth of grain boundary voids. The work in this area has been recently reviewed by Davies and Dennison.6 It is possible that some of the observations and conclusions may have a bearing on the present study? especially since at least two studies7,&apos; have been extended down to room temperature and below using magnesium alloys. However, since magnesium does exhibit low-temperature cleavage, these results may not be pertinent to the present one. The use of the electron microscope as an aid to the study of fractures has been extensively exploited by Crussard and coworkers.9 The examination of direct carbon replicas of the fractures of a large number of metals and alloys showed that the bulk of the fracture surface was covered with cup-like indentations of the order of 1 to 2 µ in size. These frequently had a directionality by which Crussard claims to be able to tell the direction of the crack propagation. With this rather disconnected background of information, this investigation was undertaken in the hope of presenting a unified picture of the initiation and propagation of a fracture in a ductile metal. To this end all of the techniques previously used were employed simultaneously so that there might be a good correlation of the data obtained by different techniques. EXPERIMENTAL PROCEDURE The metal which was chosen as the starting material for this investigation was OFHC copper. Of the dozen or so materials considered, it best fulfilled the requirements of commercial availability in large sizes, good ductility, relatively high melting point compared with room temperature and

Jan 1, 1961

By G. H. Wilson

INTRODUCED in 1946 to serve a need in power-plant operation, closed-circuit TV has been used by well over 200 organizations in approximately 25 different industries. Known as industrial television, or simply ITV, it can be described as a private system wherein the television signal is restricted in distribution, usually by confinement within coaxial cable that directly connects the TV camera to one or several monitors, Figs. 1, 2. The picture is continuous and transmission is instantaneous, permitting an observer to see an operation that may be too distant, too inaccessible, or too dangerous to be viewed directly. Destructive testing or the machining of high explosives can now be conducted hundreds of feet away by personnel who still have close control through the eyes of the TV camera. It is also possible for one man to control operations formerly requiring the co-ordinated efforts of several workers. For example, at a large midwestern cement plant conveyance of limestone from primary crusher to raw mill and loading into five storage bins once necessitated the work of two men, one having little to do but prevent spilling of material by manually moving the tripper on the belt conveyor as occasion required. TV cameras mounted on the tripper now provide bin level indication to the conveyor operator at the crusher position so he is able to control the entire loading operation remotely, Fig. 3. By means of a switch, the picture from either camera is alternately available on a single viewer, or monitor, Fig. 4. Each camera is mounted on the tripper by means of a simple adjustable support and looks down into the bin, which is identified by the number of cross members on the vertical rod. Each associated power unit is located on a platform above the camera, Fig. 5. This centralized control by means of TV often has produced superior results, and in many instances saving in operating costs has been sufficient to write off equipment costs within six months to a year. Where a key portion of a process may be enclosed or otherwise inaccessible, TV again reduces the likelihood of mistakes and permits closer control by making available to the operator valuable information he might otherwise never possess. An example of this can be found at a strip mine where the coal seam lies 50 ft or more below the overburden, which is removed by a large wheel shovel. From his centrally located position the shove1 operator was unable to judge accurately to what extent the wheel buckets engaged the earth. His chief indication of efficiency was the amount of overburden on the belt conveyor as it passed his control point 75 ft from the wheel. Now, two television cameras mounted on the tip of the boom permit the operator to view the wheel from each side and provide him with a close-up view of the buckets so that he can take immediate and continuous advantage of their capacity, quickly compensating for ground irregularities and avoiding obstructions, Fig. 6. While the word television conjures up visions of highly complex and intricate apparatus such as that employed in modern TV studios and transmitting stations, the term industrial television should indicate compact, straightforward equipment. Most present-day ITV systems contain fewer than 25 tubes including camera and picture tubes. The average home television receiver alone requires at least that many tubes. Equipment like that illustrated in Fig. 1 contains only 17 tubes, of which 3 are in the camera. It can operate continuously and dependably, without protection, in any temperature from 0" to 150°F. It consumes less current than a toaster and weighs under 140 lb. Camera and monitor may be separated by 1500 to 2000 ft and by greater distance with additional amplification. This equipment is designed to withstand vibrations up to 21/16 in. and will operate successfully under more severe conditions of vibration and heat when suitable enclosures are provided. Any number of cameras may be switched to a single monitor, and any number of monitors, within reason, used simultaneously. Two types of applications in the mining industry have already been described. A third under serious consideration by several organizations will make use of ITV for remote observation of conveyor transfer points at copper concentrating plants so that evidence of belt breakdown and plugging of transfer chutes can be spotted immediately and costly overflow of material avoided. A television camera will soon be installed to view a trough conveyor near the exit of an iron-ore crusher to indicate clogging of the crusher as evidenced by reduction or absence of material on the

Jan 1, 1955

By C. F. Allen, G. B. Walker

The sink-float methods designated by heavy-media separation processes were pioneered by C. Erb Weunsch for the treatment of base metal ores as an improvement over jigs. The work of Weunsch was further developed by Victor Rakowsky and The American Zinc, Lead and Smelting Co. Early in the development of the processes, the inherent unsuitability of galena as the solid constituent of the medium was recognized and ferrous media amenable to magnetic recovery and control were developed. The high efficiency and low cost of magnetic recovery and cleaning of ferrous media regardless of particle size, slime contamination, or surfacial oxidation had led to the adoption of ferrous media by all of the sink-float plants operating under the heavy-media separation processes patents controlled by American Zinc, Lead and Smelting Co. Approximately 2,000,000 tons of base metal and nonmetallic minerals are treated each month by these methods. Heavy-media separation processes are a modern practical and economical adaptation of the well-known laboratory procedure for separating a mixture of two solids by immersing the mixture in a liquid having a specific gravity intermediate the specific gravities of two solids. The lighter solid floats while the heavier sinks. This method of separation has been attempted on a commercial scale, but the high loss and high cost of the organic liquids halted the development of the process. Many attempts have been made to simulate a heavy liquid by using a suspension of a finely divided solid in water. If the solid phase of the suspension is ground fine enough, the suspension can be made stable or so slow settling that a substantially uniform specific gravity can be maintained from top to bottom of the bath. However, any material separated by such methods will inevitably be contaminated by some slime which will eventually accumulate in the bath and cause a viscous medium at the expense of separating efficiency. Therefore, it is necessary to provide means for continually cleaning a portion of the medium to eliminate slime at the same rate at which it is introduced to the medium. The problem of efficiently cleaning the medium limits the minimum grain size of the solid of the suspension in the case of the Chance sand process for cleaning coal, because de-cantation is the only cleaning method available. If the sand is too fine, it will be lost along with the slime. Therefore, coarse sand must be used, and to maintain a semblance of a uniform suspension, it is necessary to use strong rising water currents. The combination results in a separation based more on hindered settling classification than on sink-float principles. As previously mentioned, galena was used as the solid constituent of the medium during the early stages of the development work. The high specific gravity of galena made it suitable for the preparation of medium for high specific gravity separations. Galena can be cleaned by either decantation or by froth flotation. As with sand, de-cantation limits the minimum particle size of the media that can be cleaned without excessive loss. Froth flotation for cleaning galena medium has been used, but the problem of floating fine galena that has been exposed to extensive oxidation is well known to be a most difficult one. Last year the largest heavy-media plant m the world, and the second plant to be installed, converted from galena medium to ferrous medium despite the fact that the ore contains galena which can be used as medium. The change to ferrous medium has been beneficial in many ways. Today all the heavy-media plants have been converted from galena to ferrous media. Unquestionably, ferrous media have the widest application of any media developed, for the following reasons: 1. Ease of recovery and cleaning by magnetic means. Particle size or surface condition not a factor. 2. Low consumption per ton of ore treated. 3. Resistance to abrasion. 4. Widest range of media densities, including higher workable densities (1.25 to 3.4) than have been found possible with nonferrous media. 5. Space required for recovery and cleaning of ferrous media is considerably less than that for nonferrous media. 6. Ferrous media require lower capital investment and operating costs for media recovery and cleaning. Advantages of Heavy-media Separation Processes Heavy-media separation processes offer the following positive advantages, amply demonstrated on a wide variety

Jan 1, 1950

By N. J. Olson, G. W. Toop

A series of equations previously derived for calculating ternary thermodynamic properties using binary data has been applied to the problem of predicting ternary phase diagrams and quaternary excess free energy. The methods are considered to be rigorous for regular ternary and quaternary systerns and empirical for nonregular systems. The equations have been used to predict ternary phase boundaries in the Pb-Sn-Zn system at 926°K and the Ag-Pd-Cu system at 1000ºK. Calculated quaternary excess free-energy values are presented for the Pb-Sn-Cd-Bi system at 773°K. A method for predicting the location of ternary phase boundaries would be a useful supplement to experimental measurements in ternary systems. This has been recognized with the considerable work that has been done to find models to predict or extend thermodynamic properties and phase diagrams in binary and ternary systems1-18 for which direct experimental measurements are limited. With the access to highspeed digital computers and mechanical plotting devices, it is currently rather easy to compare mathematical models with experimental data. The regular-solution model is consistent with systems which exhibit negative heats of mixing, positive heats of mixing, and miscibility gaps, and therefore it is applicable to simple phase diagrams. The purpose of this paper is to illustrate the use of regular-solution equations to predict, empirically, phase equilibria in some types of nonregular ternary systems. Corresponding equations for regular quaternary systems are given and used to calculate empirical quaternary excess free-energy data. METHOD FOR PREDICTING THE LOCATION OF TERNARY PHASE BOUNDARIES USING BINARY DATA Meijerin1,6 has used the regular-solution model to calculate common tangent points to ternary free energy of mixing surfaces and hence to determine phase boundaries in ternary systems involving miscibility gaps. He used the following equation to calculate ternary excess free energy of mixing values: stants characteristic of the binary solutions, and Ni is the mole fraction of component i. An alternate expression which gives for regular solutions as a function of binary values of along composition paths with constant N1/N2, N2lN3, and N1/N3 may also be derived:15 ternary r xs 1 ?c-*n.Ti*.U*. This expression for is more useful for the empirical calculation of ternary excess free-energy values for nonregular systems because actual binary AFXS data may be used in the expression rather than attempting to find suitable constants for Eq. [I]. The results of this feature of Eq. [2] are illustrated in Table I where calculated excess free-energy values for the Ni-Mn-Fe system at 1232°K are compared with experimental data of Smith, Paxton, and McCabe.19 Although regular-solution equations have been shown to give calculated thermodynamic quantities which agree quite well with experiment for single-phase nonregular ternary systems,14,15 care should be exercised in the use of the equations to predict thermo-dynamic properties of multiphase ternary systems in which strong compound formation is suspected. This precaution is consistent with the simple regular-solution model which for negative values of ai_j will indicate a tendency toward compound formation but even for very large negative values of ai-jwill not give multiphase binary or ternary systems involving a distinct stable compound. Hence, calculated ternary free-energy data using Eq. [2] might be expected to vary between being rigorous and poor, in the following order, for ternary systems which are: a) regular solutions, b) nonregular single-phase liquids in which random mixing is nearly realized, c) nonregular single-phase solids, d) nonregular multiphase systems exhibiting miscibility gaps, e) nonregular multiphase systems with binary compounds but no ternary compounds, f) nonregular multiphase systems with highly stable binary and ternary compounds. The calculated data will be expected to be least accurate for the last two cases. The general method adopted in this paper involves two-dimensional plots of ternary activity curves. The principle used is that tie lines indicating two-phase equilibria join conjugate phases a and B for example, for which a1(a) = a1(B), a2(a) = a2(B), and a3(a) = a3(B). Tie lines may be determined by plotting the ternary activities of two components along an isoactivity line for the third component and the unique points where the above equalities hold may be found graphically.

Jan 1, 1970

By H. M. Zoerb

Based on the belief that operating details are a definite contributing factor to major economies, this paper traces the development of crushing cavity design in Symons cone crushers to attain maximum liner utilization. Wear rates are analyzed and compared in this presentation and drawings illustrate succeeding design changes. IN these times of rising labor and material costs, it has become more and more necessary that attention be paid to some operating details which, in their obscurity, may he the key to major economies. Liner wear in crushing cavities of secondary and tertiary crushers can become an appreciable cost item when the material to be crushed is hard and abrasive. This item of cost not only includes the value of the crushing members, but also more intangible costs such as labor and lost production due to more frequent replacement. The variables which are encountered in ores and minerals to be reduced; the design of plant and machine application; the sizes, shape, and fineness, characteristics of the crushed product; the moisture; hardness; friability; and abrasiveness of the material to be crushed are all influencing factors which must be taken into consideration in the selection of a crusher, and particularly in the design of crushing cavity and liners to be used in a crusher. Through a research program undertaken in cooperation with many operators of Symons cone crushers a new approach to crusher cavity design was made, resulting in the development of liners for specific operations which showed: 1—maximum utilization, as high as 70 to 80 pct of original weight of metal, and 2— maximum capacity of unit during the greater portion of its life. It has been found that liners so designed for a given operation will show added economies in power consumption, maintenance, and general wear and tear on the crushing unit. Initial work in the so-called tailoring of crushing cavitles was begun on the tertiary or fine crushing units where as a rule reduction ratios were low, varying from 3 to 6. Parallel or sizing zones in the lower portion of the crushing cavity were too long, resulting in a tendency to pack. It was found that very little additional crushing was done in the parallel zone after the initial impact in that zone and that a relatively small amount of&apos; additional crushing was done by attrition, which required very careful feed control. A small amount of over-feeding would result in packing which not only consumed power but caused unnecessary liner wear as well. The illustrations which follow in this discussion will show only contours of crushing cavities, and for purposes of simplification the cavities will be considered only in their closed position. The first step, therefore. was to reduce the sizing zone to a minimum. This was done by removing the lower portion of the liner as shown in Fig. 1. The result of the change was a saving of 15 to 20 pct in liner cost, less power consumption, with no change in capacity. This change in design, while an improvement, did not go far enough. As wear took place, the change in the liner was not uniform throughout its entire length, resulting in a restriction of the feed opening and thereby loss of capacity. Furthermore, progressive wear of the liner had the effect of lengthening the parallel zone until finally the entire crushing cavity was all parallel zone, see Fig. 2. It is obvious from the reduced feed opening of the worn liner that the ability of the machine to receive material is lessened considerably. Furthermore, the long parallel zone with its worn, irregular profile did not operate at its highest efficiency. The first attempt to overcome this difficulty was carried out on a 5 1/2-ft crusher installed in a plant producing roofing granules. The material being crushed was a very hard graywacke and the crusher was closed-circuited with a screen having .232-in. slotted openings. A radical change in contour was developed, as illustrated in Fig. 3. Equal wear lines on both concave and mantle are designated 1, 2, 3, etc. The method of development of this contour is as follows: Since adjustment for wear is vertical, corresponding intersections of wear lines and vertical lines developed concave and mantle contours which maintained equal but lengthening wear surfaces in the parallel zone. The ideal contour, of course, is one in which the length of the parallel zone remains constant, but because of present foundry practice and heat treating characteristics this is impossible.

Jan 1, 1954

By H. C. Gatos, J. T. A. Pollock

It is well known that the superconducting critical current densities of many alloy superconductors may be increased by cold working and in some cases further enhanced by a short heat treatment. This latter enhancement has been attributed to the redistribution of dislocations into cell-like networks&apos; and to the precipitation of second phase particles,2&apos;3 which act as flux pinning centers. In a manner analogous to dislocation pinning in precipitation hardening alloys,4 it is expected that here also a critical distribution of the pinning centers should result in maximum pinning effect. Concentration inhomogeneities exist in most or all commercial alloys yet there have been only a few attempts made to determine their effect on critical current capacity in the absence of cold working. Sutton and Baker,5 and Kramer and Rhodes6 have found that the complex precipitation processes occurring during the aging of Ti-Nb alloys can result in critical current density enhancement. Livingston7-10 has clearly shown, for lead and indium based alloys, that the distribution of precipitated second phase particles is of critical importance in determining magnetization characteristics. However, these &apos;(soft" alloys age at room temperature and the time involved in specimen preparation prevents metallographic examination in the state in which the superconducting measurements are made. Thus results with such alloys are expected to be biased towards larger precipitates and interpar-ticle spacing. The present study of Ta-Zr alloys was undertaken to examine the influence of second phase precipitation, as controlled by heat treatment, on the critical current capacity of well annealed polycrystalline material. A study of the published phase diagram11 indicated that annealing supersaturated samples containing up to 9 at. pct Zr at suitable temperatures would result in the precipitation of a zirconium-rich second phase. It was MATERIALS AND PROCEDURE The alloys were prepared from spectrochemically pure tantalum and zirconium. Analysis was carried out by the supplier. Major impurities in the tantalum were: 12 pprn of 02, 17 pprn of N2, 19 pprn of C, and less than 10 ppm each of Mo, Nb, Al, Cr, Ni, Si, Ti. The crystal bar zirconium was pure except for the following concentrations: 15 pprn of 02, 17 ppm of C, 23 ppm of Fe, 11 ppm of Cu, and less than 10 pprn each of Al, Ca, N2, Ti, and Sn. Samples were prepared in the form of 8 to 10 g but-tons by arc melting using a nonconsumable electrode on a water-cooled copper hearth in a high purity ar-gon atmosphere. Each button was inverted and re-melted three times to ensure an even distribution of the component elements. The samples were then homogenized at temperatures close to their melting points for 3 days in a vacuum furnace maintained at 5 x 10-7 mm Hg. After this treatment the buttons were cold rolled to sheets approximately 0.020 in. thick from which specimens were cut, 0.040 in, wide and 1 in. long suitable for critical current density (J,) and critical temperature (T,) measurements. These strips were then recrystallized and further grain growth was allowed by an additional vacuum heat treatment at 1800°C for 60 hr. Some second phase precipitation occurred during cooling of the furnace and a solution treatment was necessary to produce single phase supersaturated samples. This treatment was successfully carried out by sealing the samples together with some zirconium chips in quartz tubes under a vacuum of 5 x 10-7 mm Hg, heating at 1000°C for 5 hr and then quenching into water or liquid nitrogen. The samples were then heat treated at either 350" or 550°C and quenched into water or liquid nitrogen. All samples which were heat treated at 350°C were quenched in both cases by cracking the capsules in liquid nitrogen. The samples treated at 550°C were quenched by dropping the capsules into water. Analysis for oxygen in randomly selected samples indicated that the oxygen content was in the range of 175 to 225 ppm. Values of Tc were determined by employing a self-inductance technique. Jc measurements were made at 4.2oK by increasing the direct current through the wire in a perpendicularly applied field until a voltage of 1 pv was detected with a null meter. The risk of resistive heating at the soldered joints during these latter measurements was reduced by first plating the ends of the wires with indium and then soldering to the copper current leads using tin. Metallographic examinations were performed after mechanical polishing of the same samples and etching in a 4H20:3HN03 (conc):lHF(conc) solution.

Jan 1, 1970

By A. P. Svenningsen

IN the early stages of design it was not considered necessary that separate crushing plants be built for the new sulphide concentrator and smelter until sometime in the future. The plan was to use the existing crushing facilities for both oxide and sulphide ore. A few additions were contemplated for the existing plants, such as increased bin capacity, and possibly two new secondary crushing units. The more the problem was studied and discussed with the plant operators, the more it became evident that it was complex. It involved the classification of different kinds of ore from the open pit mine -sulphide, oxide and mixed-and how best to separate them so that each kind of ore was given the proper processing and treatment. It also involved the problem of keeping the different ores from being contaminated in bins, hoppers and chutes. Added to these, transportation became complicated and would involve additional handling and loading of ore from crushing plants to conveyors, to bins, and finally to railroad cars which were to be hauled to the concentrator and dumped into the fine ore bin. General In the early part of 1951 it was decided that the concentrator be constructed with ten grinding units instead of seven as originally authorized. The smelter was to be increased proportionally and naturally also the overall tonnages of ore to be handled by the new sulphide plant. Due to this increase in plant capacity and the larger tonnages involved, the difficulties which would arise by using the existing crushing plants were increased to a point where it became evident that the building of new crushing plants for sulphide ore exclusively was technically, as well as economically, advantageous. Authorization was, therefore, given by the company to construct new crushing plants to handle 30,000 tons of ore per day, and capable of reducing the run-of-open-pit ore to the proper size feed for the 10x14-ft rod mills in the concentrator. The ore, mined in the open pit, sometimes comes in pieces as large as 6 to 7 ft diam. The rod mills may call for ore crushed to 3/4 in. The large .size of ore delivered from the open pit determined that a 60-in. gyratory crusher be used as primary breaker. Such a crusher will have a capacity considerably in excess of 30,000 tons per day. The crusher will be a single discharge unit driven by a 500-hp electric motor through a tear coupling and a floating shaft. This type of drive has proven successful at a number of other crusher installations which our company has operating in the United States, Mexico and South America. The tear coupling will protect both the crusher and motor against damage in case of overload. No new features are incorporated in the design of the crusher itself, except that the, discharge chute is made the full width of the crusher with parallel sides instead of the usual converging sides. This change in detail should eliminate, a feature which has been a bottleneck in some of the operating plants and has caused loss of production due to ore hanging up and blocking the chute. The secondary crushing plants will have three 7-ft standard Symons cone crushers and six 7-ft short head Symons crushers. Between the primary and secondary crushing plants a coarse ore bin will be constructed with a nominal draw-off capacity of 30,000 tons of ore. The standard Symons and the short head Symons will be in separate buildings. All the crushing plants and the coarse ore bin are interconnected with conveyor belts for transporting the ore to the crushers at the tonnage rate desired. The final product of the new crushing plants is produced by the short head crushers. It will be delivered onto a conveyor belt leading to the top of the fines ore bin in the concentrator. A separate conveyor belt running the full length of the fines ore bin and provided with a movable tripper of rugged design will discharge the sulphide ore into the bin. The concentrator bin is planned and designed so that the installation of this additional conveyor will not interfere with the operation of the two railroad tracks on which crushed ore is brought from the existing oxide plant. Thus when completed the bin can be filled simultaneously by ore from the new crushing plant and by ore from the existing leaching plant.

Jan 1, 1952