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By James P. Connell

The Berkeley Pit of The Anaconda Company is located on the southeast slope of the Butte Hill, the legendary "Richest Hill on Earth," and is one of the largest pit operations in the world completely dependent on truck haulage. Through October 31, 1968, the Berkeley stripping and mining operations have moved more than 442,589,000 tons of material. Present scheduled production is at the rate of 260,000 tons per day, with a record quantity of 306,900 tons having been hauled on September 23, 1968. Although the Berkeley Pit has been in production only a little more than ten years, it has been the proving ground for many of the presently used large trucks. Beginning with the original R. G. LeTourneau 75-ton electric truck in 1960, Unit Rig 85- and 100-ton electric drives, Haulpak 65- and 105-ton electric drives, and Caterpillar 100-ton electric drives have all been tested under production conditions. In addition, engine development has kept pace with both 1000-hp diesel and 1100-hp gas turbine engines now under test. As the size of the Berkeley operation has grown, the truck fleet has changed in size and appearance in order to maintain economic mining costs. The original fleet consisted of forty-three 36-ton trucks with conventional mechanical drives. The present fleet is made up of eighty-nine trucks: nineteen 85-ton Unit Rig electrics with 700-hp diesel engines; sixty-nine 100-ton Unit Rig electrics with either 700- or 1000-hp diesel engines; and one 100-ton Unit Rig electric with an 1100-hp gas turbine engine.

Jan 1, 1969

By Mohan Dutt

This paper is concerned with applied platinum resistance thermometry which involves many considerations absent in precision thermometry. The historical development of the Callendar-Van Dusen Equation which describes the resistance- temperature relation of pure platinum is discussed. The advantage of using platinum resistance temperature sensors over thermocouples is described, and the improvements in design and construction of these sensors that have come about in the past few years are discussed. Integral and remote bridges that convert resistance changes into voltage together with signal conditioning techniques and equipment for voltage or current signals are described. Errors encountered in temperature measuring schemes and methods to reduce these errors are summarized.

Jan 1, 1969

By A. L. Barnes, A. M. Rowe

A heat transfer study was made of hot gas injection into oil shale through wells interconnected by vertical fractures. This analysis involved the simultaneous numerical solution of a nonlinear, second-order partial differential equation that describes two-dimensional conduction heat transfer in oil shale and a nonlinear first-order partial differential equation that describes convection heat transfer in the fractures. Three nonlinear, temperature-dependent coefficients were used in this work; they are thermal conductivity, thermal capacity and retorting endothermic heat losses of oil shale. Vertical fractures were considered to be of finite height. Although vertical conduction heat transfer was not considered, an estimate of the error resulting from this limitation was made. The effects of injected gas temperature, injection rate, system geometry, cyclic injection and time upon retorting efficiency were investigated. Results from this study show that the rate of retorting oil shale is a direct function of both injection temperature and rate, and the theoretical producing air-oil ratio:(AOR) is an inverse function of temperature. Retorting rates are constant until "breakthrough" of the 700 F isotherm at the producing well, assuming constant injection parameters. Retorting rates for bounded systems are higher than the analogous unbounded systems and likewise AOR's are less. The use of an alternating injection-soak routine with high injection rates is less efficient than continuous injection at lower rates. These results indicate that injection temperatures on the order of 2000F or greater may give theoretical AOR's in the economic range. INTRODUCTION Over half of the known oil shale reserves are located in the U.S., and most of them lie in the Piceance Creek basin of Western Colorado. The Colorado oil shale outcrops on the edges of the Piceance Creek Basin. At the outcrops the shale beds are relatively thin, from 25 to 50 ft thick. In the center of the basin the oil shale is as great as 2,000 ft thick and is covered with 1,000 ft of overburden. It has been estimated that there are over 1,000 billion bbl of oil in shales having an oil content over 15 gal/ton in this basin. Oil shale does not contain free oil but an organic matter called kerogen. Kerogen yields petroleum hydrocarbons by destructive distillation. It must be heated to approximately 700F, at which temperature it decomposes into shale oil, gases and coke. The U.S. Bureau of Mines and, more recently, oil companies have conducted considerable research on surface retorting methods to economically recover oil from this shale. Another approach to exploit the oil shale deposits, in particular that portion having 1,000 ft of overburden, is to retort the oil shale in place and produce the liquid and gaseous hydrocarbons through wells drilled into the shale. Some research has been done on this approach.l,2 There are several variations to the in situ retorting approach. These variations fall into one of two groups, depending upon the geometry of the system: (1) retorting in a highly fractured or broken up matrix; (2) retorting from single fractures between production and injection wells. The latter is the group studied. Several investigators,3-6 using various assumptions, have studied flow of heat through horizontal systems. The objective of this work was to make a heat transfer study of in situ retorting oil shale by hot gas injection through wells interconnected by single vertical fractures of finite height. The oil shale thermal conductivity, thermal capacity and retorting endothermic heat losses were considered to be functions of temperature. A knowledge of the

Jan 1, 1969

By J. V. Vogel

Jan 1, 1969

By L. C. Brown, A. J. Stewart

Phase transformations have been studied in Ag-Zn alloys quenched from the high-temperature bcc 0 phase and lying in the composition range 37.4 to 50.0 at. pct Zn. On quenching, the alloy with the lowest zinc content transformed to massive a (fcc); all other alloys formed the ordered (3' phase. On deformation, a martensitic reaction took place forming a close-packed structure. At Lou' zinc contents transformation to this structure was complete. However, above 43 at. pct Zn a p.rogressively increasing amount of ß' was retained following deformation. The close-packed structure was fcc at lower zinc contents (under 47 at. pct Zn) and either hcp or a mixture of fcc and hcp at high zinc concentrations. The structures produced by cold working were unstable and on aging transformed to the ß' phase or the complex hexagonal to phase. For low zinc contents (under 43 at. pct) the fcc st-ructure transformed directly to the equilibrium To phase. With higher zinc contents, some 13' was retained following defownation, and on aging the amount of this phase relative to the close-packed structure increased. On further aging both structures transformed cornpletely to PO. Metallographic examination indicated that the nature of the deformation product depended very markedly on the mode of deformation. Tensile deformation gave a microstructure characteristic of thermal martensite. KING and Massalski1 have shown that an alloy of Ag-50 at. pct Zn quenched from the high-temperature bcc ß phase undergoes a low-temperature ordering reaction forming ß' which can be retained to room temperature. On deformation an hcp phase is produced, although this is unstable and the structure reverts completely to ß' on aging. In the present paper, the work of King and Massalski is extended to cover a wide composition range in the p phase, observations being made of the structure of the quenched 13 and of the effects of deformation and aging. The relevant portion of the Ag-Zn phase diagram is shown in Fig. 1. King and Massalski have shown that close to stoichiometry the ß' phase is the equilibrium structure at low temperatures. The approximate composition range of this phase, taken from a recent paper by Pops and Massalski,3 is shown on the phase diagram. The locations of atom sites are very similar in the ß' and to structures, and the 4, structure can be derived from the 0' structure by a small movement of atoms mainly in the direction of the cube diagonal.4'5 However, the probability of filling any particular atom site by a silver or a zinc atom is markedly different in the two structures. The structure can be considered partly ordered but the arrangement of the ordered atoms is completely different from that in the p' structure and transformation from ß' to requires a large fraction of the atoms to change position. It has been shown that the ß' transformation is thermally activated involving normal nucleation and growth processes.5,8 Massalski and Barrett7 have shown that in the Cu-Zn binary the (3 phase can be retained in the ordered state to room temperature over a wide composition range. On deformation a new close-packed phase is produced, the structure varying from fcc to a mixture of fcc + hcp to hcp alone with increasing zinc concentration. It appears that an ordering reaction is necessary to retain the bcc phase to room temperature. In CU-Ga,8 the bcc phase cannot be retained to low temperatures as it transforms by a massive reaction above the ordering temperature of the ß phase. The structure of the massive phase is very similar to that in Cu-Zn, varying from fcc to fcc + hcp to hcp with increasing zinc concentration. Similar structures have also been observed in CU-A1,9 Ag-Cd,10,11 and Ag-Al.12 EXPERIMENTAL The alloys were prepared by melting fine silver (99.99 pct purity) and electrolytic zinc (99.999 pct

Jan 1, 1969

By R. C. Dorward

DIFFUSION considerations are necessary to describe many technologically important metallurgical and physical processes. Since most commercially important alloys are comprised of more than two components, diffusion calculations applicable to binary systems are often unjustified. However, in many instances the more general equations valid for three-component systems may be employed. The phenom-enological description of ternary diffusion is now well-established,1-4 and the theory has been applied with some success to a few practical situations.5"7 The flux equations for the solutes (components 1 and 2) of a ternary solution may be expressed by:

Jan 1, 1969

By Richard E. Dawes

Physical variables, a principal factor in the economies of mineral production, affect both capital and direct operating costs. By using a revenue-cost system for the framework, the analyses of revenue and cost categories demonstrate the relative importance of groups of physical variables, whether explicitly defined or not, to a lead-zinc mining operation. Physical variables affecting the producer represent about 60 percent of the total system influence as expressed by cost ranking. Other physical variables affect the remaining costs as controlled by the smelter, the transporter, and the landowner. Such resource conservation aspects as mineral losses due to mining method and mineral processing constitute a portion of the total revenue effects of physical variables. The physical variable revenue-cost system presented in this report offers a framework for cost-benefit analysis of mineral related research.

Jan 1, 1969

By J. R. Szedon, T. L. Chu, G. A. Gruber

Amorphous adherent filnzs of silicon dioxide have been deposited on silicon substrates by the oxidation of silane at temperatures ranging from 650 to 1050C. Various diluents (argon, nitrogen, hydrogen) were used to suppress the formation of SiO2 in the gas phase. Deposition rates of the oxide were determined over the temperature range in question as functions of' re-actant flow rates. Etch rate studies were used for a cursory comparison of structural properties of deposited and thermally grown oxides. From electrical evaluation of metal-insulator-silicon capacitors it was determined that the interface charge density of deposited films is similar go that of dry-oxygen-grown films in the 850° to 1050 C temperature range. Deposited films exhibit several ionic instability effects which differ in detail from those reported for thermal oxides. Stable passivating films of silicon nitride over deposited oxides appear to be practical for use in silicon planar device fabrication. Such films can be prepared under temperature conditions which have less effect on substrate impurity distributions than in the case of grown oxides. AMORPHOUS silicon dioxide (silica) is compatible with silicon in electrical properties and is the most widely used dielectric in silicon devices at present. Silica films can be prepared by the oxidation of silicon or deposited on silicon or other substrate surfaces by chemical reactions or vacuum techniques. The ability of thermally grown silicon dioxide films to passivate silicon surfaces forms one of the practical bases of the planar device technology. Properly produced and treated films of grown SiO 2 can have low densities of interface charge (-1 X 10" charges per sq cm) and can be stable as regards fast migrating ionic sgecies. 1 To maintain these properties, even with an otherwise hermetically sealed ambient, the Sia layers must be at least l000 A thick. Such thicknesses require oxidation in dry oxygen for periods of 7.8 hr at 900°C or 2 hr at 1000°C. Although oxidation in steam or wet oxygen can reduce these times to 17 and 5 min, the resulting oxides must be annealed to produce acceptable levels of interface charge., Oxidation or annealing involving moderate to high temperatures for extended periods of time can be undesirable. Under some conditions, there can be changes in the distribution of impurities within the underlying substrate. A chemical deposition technique using gaseous am-bients is particularly attractive and flexible for preparing oxide films. With a wide range of deposition rates available, films can be produced under condi- tions of time and temperature less detrimental to impurity distributions in the silicon than in the case of thermal oxidation. The pyrolysis of alkoxysilanes, the hydrolysis of silicon halides, and various modifications of these reactions are most commonly used for the deposition of silica films.3 Silica films obtained in this manner are likely to be contaminated by the by-products of the reaction, organic impurities, or hydrogen halides. The use of the oxidation of silane for the deposition process has been reported recently.4 The deposition of silica films on single-crystal silicon substrates by the oxidation of silane in a gas flow system has been studied in this work. The deposition variables studied were the crystallographic orientation of the substrate surface, the substrate temperature, and the nature of the diluent gas. The electrical charge behavior of Si-SiO2-A1 structures prepared under various conditions was investigated by capacitance-voltage (C-V) measurements of metal-insulator-semiconductor (MIS) capacitors. The experimental approaches and results are discussed in this paper. 1) DEPOSITION OF SILICA FILMS The overall reaction for the oxidation of silane is: The equilibrium constants of this reaction in the temperature range 500° to 1500°K, calculated from the JANAF thermochemical data,= are shown in Fig. 1. In addition to the large equilibrium constants, the oxidation of silane is also kinetically feasible at room temperature and above. However, the strong reactivity of silane toward oxygen tends to promote the nucleation of silica in the gas phase through homogeneous reactions, and the deposition of this silica on the substrate would yield nonadherent material. The formation of silica in the gas phase can be reduced by using low partial pressures of the reactants. Argon, hydrogen, and nitrogen were used as diluents in this work. 1.1) Experimental. The deposition of silica films by the oxidation of silane was carried out in a gas flow system using an apparatus shown schematically in Fig. 2. Appropriate flow meters and valves were used to control the flow of various reactants, i.e., argon, hydrogen, nitrogen, oxygen, and silane. Semiconductor-grade silane, argon of 99.999 pct minimum purity, oxygen of 99.95 pct minimum purity, and nitrogen of 99.997 pct minimum purity, all purchased from the Matheson Co., were used without further purification. In several instances, a silicon nitride film was deposited over the silica film. This was achieved by the nitridation of silane with ammonia using anhydrous ammonia of better than 99.99 pct purity supplied by the Matheson CO.' The reactant mixture of the desired composition was passed through a Millipore filter into a horizontal water-cooled fused silica tube of 55 mm

Jan 1, 1969

By P. T. Chiang

Chemical etching methods for the simultaneous revealing of the tellurium or selenium Phase and the chalcogenide grain boundaries of the alloy systems are given. A tellurium eutectic was found Present in zone-melted ingots. Similarly, a selenium monotectic was present in ingots. In general, the second phase (tellurium or seleniumn) occubies three different sites; viz., along the chalcogenide grain boundaries, as inclusions within the chalcogenide grain, and on the undersurface of the ingot. The detection limit for the tellurium phase is about 1 u in width. THERMOELECTRIC materials based on Group V (bismuth, antimony) and Group VI (selenium, tellurium) elements have aroused considerable interest in recent years in the practical application of thermoelectric cooling. In many cases, a small amount of excess tellurium (or selenium) was added to the material to optimize its thermoelectric properties. Then the question immediately arises as to the number of phases present in the resultant alloy. In the binary systems of Bi-Te, Sb-Te, and Bi-Se, the congruent melting compositions have been reported to be non-stoichiometric and are represented by Bi~Te respectively. It is to beexpected and known that Bi2Te3 and SbzTe3 crystallize from the melt with an excess of bismuth and antimony in the lattice and that tellurium forms a eutectic.~' The same could be assumed to take place in the pseudo binary systems of (Bi,Sb)zTe3 and Bi2(Se,Te)3 as well as in the system studiedby puotinen5 and other workers. Likewise, BiaSe3 crystallizes from the melt with an excess of bismuth in the lattice and selenium forms a monotectic.~ Therefore, in practice, alloys solidified from the melt often contain a second phase (tellurium or selenium) in one region or another of the solid mass even without the addition of excess tellurium (or selenium). ~u~~recht' studied the thermoelectric properties of (Bi,Sb)2Te3 alloys with excess tellurium and simultaneous additions of selenium. He mentioned that the materials show two phases because of the considerable excess of tellurium or selenium. However, he did not report as to how the tellurium or selenium phase was identified. It is generally believed that the presence of an excessive amount of tellurium or selenium phase in the alloy would adversely affect its thermoelectric properties and its uniformity. Consequently, there is a need for a simple method for the identification of the tellurium and selenium phase. The quantity of the second phase present is usually too small to be detected either by chemical analysis or by normal X-ray techniques. This investigation was therefore carried out, first, to devise a simple metallographic method for the identification of the tellurium or selenium phase coexisting with the chalcogenides and, second, to determine the distribution and specific location of the tellurium or selenium phase in the ingots. EXPERIMENTAL PROCEDURE The starting materials used for the alloy preparations were 99.999 pct pure bismuth, antimony, and tellurium and 99.997 pct pure selenium. The bismuth and antimony were obtained from Consolidated Mining and Smelting Co. of Canada Ltd., while the selenium and tellurium were obtained from Canadian Copper Refiners Ltd. The tellurium was purified further in the laboratory by zone refining. The elements were pulverized in a stainless-steel pestle and mortar. The amounts for the desired composition were weighed out each time on an analytical balance to make up a 100-g sample. Then the sample was introduced into a Vycor ampule (19 by 150 mm), pumped down to a vacuum of 10"5 Torr for 15 min, and sealed off. The ampule was then heated in a horizontal resistance furnace at 800" to 900°C for about 20 hr. During this period the assembly was rocked back and forth several times to ensure good mixing. At the end of the heating period, the ampule was quenched in cold water and then transferred to the zone-melting apparatus described in a previous publications to grow large-size aligned polycrystals. The background and ring-heater temperatures were adjusted to make the freezing solid-liquid interface slightly convex to the liquid. The recorded temperature gradient in the vicinity of the freezing solid-liquid interface was around 15°C per cm. The ampule was moved horizontally at a speed varying from 0.4 to 2 cm per hr so that the ring heater would cover the whole ingot length from end to end. A single zone-melting pass was used for the Bi-Te, Sb-Te, and Bi-Sb-Te ingots. Two passes in the forward and reverse directions were carried out for the Bi-Se and Bi-Se-Te ingots. Six passes in the forward and reverse directions were performed for the Bi-Sb-Se-Te ingot. The zone-melted ingots were found to contain several large crystals, with their basal planes (0001) approximately parallel to the growth axis. Samples of bismuth and antimony tellurides coated with a layer of tellurium, and bismuth selenide coated with a layer of selenium, were prepared for comparison in phase identification. These coatings were made by dropping a piece of the zone-melted ingot into some molten tellurium or selenium under argon atmosphere and allowing them to cool slowly to room temperature. The metallographic specimens were prepared by

Jan 1, 1969

By M. C. Flemings, R. Mehrabian, G. E. Nereo

Analytical expressions derived previously are used to describe quantitatively effects on macrosegregation of some solidification and mold design variables. Al-4.5 pct Cu alloy is used as example. It is shown that abrupt changes in heat transfer rate result in solute-rich or solute-poor "bands". Severe solute-rich bands accowzpany "reheating" that can result, for example, from abrupt formation of an air gap at a mold-metal interface. With planar isotherms, solute-poor regions also result from reduction in cross section through which fluid flow to feed shrinkage takes place. It is suggested that the negative "cone" of segregation often found at the base of large ingots results from this reduction in cross section for feeding. Consideration is given to the positive and negative segregation to be expected in laboratory ingots in association with changes in ingot cross section. Under-riser positive segregation is considered and it is concluded this segregation results when vertical temperature gradient is low in the region of the riser; the segregation is accentuated by the temperature gradient reversal which can occur in inadequately insulated risers ("'hot tops"). Finally it is shown for Al-4.5 pct Cu alloy that the assumption of constant k and p in analytic solutions gives calculated results close to those obtained for the case of ziariable k and 0. A basic "local solute redistribution equation" was derived earlier' for calculation of macrosegregation resulting from flow of solute-rich liquid to feed solidification shrinkage, thermal contraction, and/or other contractions occurring during solidification. This expression relates fraction liquid, g~, to liquid composition, CL, at a given position x, y, z, in a solidifying Eq. [I] is for the general case of three-dimensional heat and fluid flow assuming constant solid (but not necessarily liquid) density during solidification, negligible net solute change from diffusion, and no pore formation. In this paper we first demonstrate application of this equation for calculation of macrosegregation in several examples involving one-dimensional heat and fluid flow. Specifically considered are examples in which segregation results from sudden changes in heat flow conditions. Next, Eq. [I] is used to describe segregation in examples where isotherms remain planar but where fluid flow is no longer one-dimensional. Application of this expression illustrates the type of segregation to be expected in unidirectionally solidified ingots of gradually or abruptly varying cross section. For segregation calculations, A1-4.5 pct Cu alloy is employed with constant k and p Vz = 0.172, 4 = 0.055), eutectic composition (CE = 33 pct Cu). In all examples, fraction eutectic is neglected in velocity calculations; this was previously shown to introduce little error.' A linear distribution of fraction liquid in the liquid-solid zone is assumed. In a concluding section it is shown that the assumption employed of constant k and /3 gives results close to those obtained when the actual (variable) values of k and 0 are employed.

Jan 1, 1969

By Michael D. Martin

Pima Mining Co., managed and 50% owned by Cyprus Mines Corp., with Union Oil of California and Utah Construction and Mining Co. sharing equally in the remaining 50%, is a medium-sized open pit copper mine situated in the very active Twin Buttes mining district, 22 miles southwest of Tucson, Ariz. In 1965, a three-part paper described Pima's growth from 3,000 tpd (tons per day) in 1957 to 18,000 tpd nine years later. Within months of the completion of the last stage of this sixfold expansion, studies were being wound up on a further major expansion, this time to 30,000 tpd. This expansion is now a reality. Details of the enlargement of the crushing and concentrating plant have already been covered in a recent paper, and the present paper will cover pit engineering studies, equipment selection, and current operating practices. Key factors in top management's decision to go ahead with the latest expansion were: (1) a substantial increase in ore reserves coupled with an appreciable decrease in grade, (2) a generally favorable outlook for copper prices, and (3) better than expected performance by mine and mill equipment purchased for the expansion to 18,000 tpd. For the pit design studies, particular attention was paid to pit stability, a problem area at times in the past, and to the location and grades of the final ramp systems. In drawing up the long-term mining schedule, the attitude of the ore, with the higher grade material lying deeper, was a critical factor and considerable stockpiling of lower-grade material in the early years had to be accepted in order to keep the annual grades close to the average of the orebody. The expansion called for major purchases of mine equipment in order to gear up the mine for delivery of 30,000 tpd to the concentrator. In general, equipment chosen was of types already proven at Pima, al- though there were some exceptions to this practice. One of these excep-

Jan 1, 1969

By Hans Allenius, R. T. Hukki

This paper describes in quantitative terms the effect of sharpness of classification on the performance of the closed grinding circuit. The analysis is based on a large number of laboratory experiments designed to simulate the two most common industrial closed grinding systems. The experimental results show quantitatively the degree of improvement achievable by more efficient classification. In an earlier paper1 the senior author has presented a trend showing qualitative analysis of mill and classifier performance in tile closed grinding circuit. According to this analysis, the master key to a major improvement appeared to be effective removal of finished fine material from the classifier sands, or in other words, improved sharpness of classification, leading simultaneously to a substantial reduction of the circulating load. One purpose of this paper is to present the results of a quantitative investigation of the closed grinding circuit. Another is to set forth the essential pertinent variables revealed by the quantitative experiments carried out by the junior author. In the two most common systems of closed-circuit grinding, (1) feed to the circuit is introduced into the grinding unit, normally the ball mill, operating in closed circuit with the classifier; or (2) feed to the grinding circuit is introduced into the primary grinding unit, normally the rod mill, discharging into the classifier in closed circuit with the secondary grinding unit, normally the ball mill. In the following discussion, these two systems are analyzed separately in the indicated order. BALL MILL - CLASSIFIER CIRCUIT The Test Apparatus and Procedure: The test appara- tus included: (1) a F 195 mm x 220 mm laboratory ball mill rotated at a speed 77% of the theoretical critical speed, and a 7-kg batch of F 20 mm-F 50 mm steel balls; (2) a conventional 65-mesh test sieve and a Ro-Tap sieve shaker serving as a classifier; and (3) a Permaran instrument manufactured by Outo-kumpu Co. for surface area determinations by the permeability method. As no continuous closed-circuit experiments could be brought about on a laboratory scale, the process was broken down into alternating grinding and sizing steps in such a way that the new feed plus the returning sands always formed a batch of 1000 gm. For each selected grinding period and for each selected sharpness of classification the basic steps were repeated six times. Steady-state conditions were then reached. Crystalline vein quartz was used as a test material. Feed to the process consisted of -10-mesh fraction of this quartz crushed in rolls. This fraction included 15% of-65-mesh material. Experimental Results: The general flowsheet is shown in Fig. 1. Table I gives the essential data obtained representing steady-state conditions under the indicated set of variables. The table is based on 110 grinding experiments, 440 screen analyses and an equal number of specific surface area determinations. Fig. 2 shows the relationship between the cumulative net energy consumption and the cumulative number of mill rotations as evaluated by separate experiments. Note that this relationship is not linear but is instead represented by a slight curve. The data given in Table I are presented in graphical form as follows: Fig. 3 shows the produced -65-mesh material in grams per minute vs. time of grinding in minutes; the sharpnesses of classification at 65 mesh were 100%, 75% and 50%. It is clearly indicated that the highest-capacity figures call for relatively short grinding times and for the sharpest possible classification. Fig. 4 presents the specific surface area on the final -65-mesh product in square centimeters per gm vs. time of grinding in minutes. In conventional mineral dressing processes, a final product characterized

Jan 1, 1969

By R. D. Nelson

The purpose of this technical note is to briefly present some data on a phenomenon—recrystallization with concurrent deformation—that has been found to occur in a plutonium. This phenomenon is unusual because a plutonium is considered brittle, not easily deformed, and not easily recrystallized; the a phase is simple monoclinic having 8 atoms per unit cell and it is stable below about 115°C. The properties of the recrystallized metal were different from the as-cast metal. Even though a plutonium is difficult to deform, Ianniello successfully rolled it' and he also observed some recrystallization at 120°C.2 Pavlick and Hanson3 detected some recovery at 109°C but they observed no recrystallization. Gardner4 and Bronisz5 studied the compression properties up to 100°C but they did not report having seen recrystallization. In the present deformation studies of electrorefined plutonium pronounced recrystallization took place concurrently with plastic deformation in compression between 24" and 115°C. The metal contained less than 300 ppm total impurities with the major impurities being 100 ppm Am, 30 ppm C, 40 ppm W, and 25 ppm U; all other impurities totaled less than 100 ppm. The compression specimens were machined to dimensions of 1.2 cm long and 0.8 cm diam from as-cast rods having a density of 19.65 g per cu cm. They were heated to the test temperature in a high-temperature silicone fluid that was evacuated to 10-4 Torr. With this procedure the specimens oxidized a negligible amount, and the temperature was maintained within ±0.2°C for times up to 3 weeks. Deformation and recrystallization

Jan 1, 1969

By T. O. Massalski, J. D. Ayers

A massive transformation, 0 —am, takes place in a number of copper-based systems where the ß phase field at high temperatures extends to compositions that are slightly less solute-rich than the limits of the a phase field that exists at lower temperatures. Consequently a solid-state transformation becomes possible that does not involve a change of composition. Within this narrow range of composition the massive am phase can be usually produced in two ways: by a fast quench from the ß phase through the a phase field, or by pulse heating into the a phase field of an undecomposed ß phase retained at room temperature by a prior quench. In the Cu-Ga system the occurrence of a massive am phase has been also observed in alloys whose composition falls outside the equilibrium a phase field1 but not in the Cu-Zn system.2 We have recently observed the occurrence of the ß — am transformation also in two silver-based systems, Ag-Zn and Ag-Cd. The a and 0 phase fields in these systems again slightly "overlap" in a narrow composition range. In the Ag-Zn system this range falls between 36.7 and 40.2 at. pct Zn, and in the Ag-Cd system between approximately 41 and 42.5 at. pct Cd. Alloys were prepared from high-purity materials and cast in quartz tubes under inert atmosphere. No significant change of composition occurred during casting. After homogenizing in the 0 phase field, small pieces of each alloy were reheated at the homogenizing temperatures for a few minutes and quenched into various media. There were examined metallographic-ally after removal of surface layers that may have suffered from contamination or from the loss of the solute element. In the Ag-Zn system extensive areas of the am phase (identified by selective etching, observation of the slip trace variants, and occurrence of twinning) were observed in a comparatively low-zinc alloy (37.8 at. pct Zn) for all quenching media employed: iced

Jan 1, 1969

By J. F. Smith, J. E. Davison

The heat capacity of CaMg2 was measured over the temperature interval, 4.8° to 287°K, by the technique of low-temperature adiabatic calorimetry. Heat content measurements were performed with a drop calorimeter over the temperature interval, 273" to 673°K. From these data the thermodynamic functions, (FT - H0)/T, ST - So, and & - Ho, were evaluated. A third-Law calculation of the standard entropy of formation of CaMg2 yields a value of -0.25 * 0.06 cal per (°K g-atom) , and the free-energy function derived from this study when combined with existing equilibria data yields a value for the standard enthalpy of formation which is in agreement with direct calorimetric enthalpy measurements. The accompanying paper' shows that the enthalpy of formation of CaMg2 has been determined with good precision by three different calorimetric techniques.'-= TWO independent determinations of the Gibbs free energy of formation of CaMg2 have also been made; both determinations were based on vapor pressure measurements, being in one case hydrogen vapor pressures over ternary Ca-Mg-H alloys4 and in the other case magnesium vapor pressures over binary Ca-Mg alloys.5 The present determination of heat capacity of CaMg2 below room temperature and of the heat content of CaMg2 above room temperature was undertaken to provide supplementary data. These data are useful in their own right but can in addition be used to evaluate an entropy of formation for CaMg2 which, because of the interrelation of free energy, enthalpy, and entropy, can be used as a check of the self-consistency of the composite of the presently available information. LOW-TEMPERATURE HEAT CAPACITY The heat capacity of CaMg2 was measured over the temperature interval 4.87° to 286.64°K in an adiabatic calorimeter. The physical details of the calorimeter and the experimental procedure for measuring the heat capacity of a specimen have been adequately described by Gerstein et a1.6 The source and purity of the calcium and magnesium are described together with the methods of sample preparation and chemical analyses in the accompanying paper.' Results of chemical analyses of the material which was used in the present investigation are shown in Table I. These analyses show that, on the basis of the published phase diagram,7 the heat capacity sample contained a slight excess of a calcium while the heat content sample contained a slight excess of magnesium. However, in both cases the excess was small, and X-ray diffraction patterns showed reflections which were without exception attributable to CaMg2. The sample which was used for heat capacity measurements weighed 69 g while the sample container and addenda weighed 132 g. The sample was in the form of annealed powder, 50 to 60 mesh, and was sealed into the sample container under 0.1 atm of helium. Copper fins inside the sample container facilitated thermal equilibrium of the powdered Sample. Time intervals of the order of 10 min were required for thermal equilibration, and such times are normal for this calorimeter regardless of the form of the sample. The observed heat capacities were corrected for the small excess of a calcium through use of the heat capacity values tabulated by Hultgren et a1.8 The corrected heat capacities are tabulated as a function of temperature in Table II. The free-energy function and the absolute entropy of CaMg2, which were calculated from the experimental heat capacity data, are listed in Table 111. A smooth curve was fitted to a plot of the experimental values of the heat capacity and in only two instances above 30°K did the plotted points deviate from the curve by more than 0.2 pct. Below 10°K the deviation of several of the points was as much as 50 pct. These large percentage deviations were attributed to the small value of the heat capacity and to the low sensitivity of the platinum resistance thermometer in this temperature range. The deviations in the region of 10°to 30°K were less than 5 pct. Although the percentage deviations of some of the low-temperature measurements are large, the actual value of these deviations is small since the magnitude of the heat capacity in that temperature range is small. The error in the value of the third-law entropy at 298.15°K was estimated to be less than 0.01 cal per (°K g-atom). A value of -0.25 ±0.06 cal per (°K g-atom) was obtained for the standard entropy of formation at 298.15°K from the relation:

Jan 1, 1969

By J. P. McGee

A 1,000-hour test with a gas turbine at 1,200° F showed a working fluid of 1 gr of ash per 100 scf of power gas (79 percent of the ash 7 to 35 microns in diameter) to be excessive for acceptable blade wear for commercial practicability. Blades in the turbine consisted of about 20 percent each of chromium, cobalt, and nickel; 3 percent molybdenum; 2-1/2 percent tungsten; and smaller amounts of manganese, columbium, and tantalum. Erosion of both the fronts and backs of the turbine nozzles was particularly heavy, the trailing edges being worn to a featheredge. Erosion of the buckets was less marked, although the leading edges were somewhat pitted. A refractory-lined combustor performed efficiently and with little abrasion of the lining by the ash-laden gas.

Jan 1, 1969

By John Ward Smith

An analytical method developed by the Bureau of Mines to determine dawsonite, nahcolite, and nondawsonite alumina (called excess alumina) extractable from Green River Formation oil shales is presented. The method requires water extraction of nahcolite followed by HCI-extraction of dawsonite and an unidentified mineral yielding excess alumina from the water-leached residue. Instrumental determination of sodium in the water extract and sodium and aluminum in the HCI extract measures the sample's content of the minerals. Detailed evaluation shows the method to be adequately specific, precise, and reproducible and free from uncorrectable interferences. The method's results define precisely the production of sodium carbonates and alumina possible from a sample of oil shale and the interval it represents. Shale-oil yields, nahcolite contents, and yields of extractable alumina determined on 83 samples representing an 821-foot section of dawsonite-nahcolite-bearing shale from .Colorado Corehole No.3, drilled in the north part of Colorado's Piceance Creek Basin, are presented. These samples resulted in nahcolite contents to 53.3 percent, oil yields to 48.3 gallons per ton, and alumina yields to 5.80 percent. Use of these data to evaluate the production potential of a section of the formation are suggested.

Jan 1, 1969

By G. D. Rieck, G. H. G. Vaessen, D. L. Vogel

Both doped and undoped tungsten single crystals exhibit hardness anisotropy with respect to the direction of testing in each of the crystallographic phes investigated. The hardness anisotropy of undoped single-crystal tungsten is rather pronounced in (001) and (110) planes but very minor in (111) planes. The anisotropy in (122) planes of the doped and drawn tungsten after recrystallization is in accordance with a previously published concept of a stringlike distribution of the doping material in the metal. ANISOTROPY in mechanical properties of single-crystal tungsten was investigated by Rose et al., Garlick and Probst,2 and Beardmore and Hull. 3 Although data on the Vickers microhardness of tungsten have been published (see, e.g., Boosz 4 and the references cited by him), no data on the microhardness anisotropy are available. We report, therefore, some of our own results on the microhardness and its anisotropy. The microhardness has been determined of the following samples. A) Polycrystalline tungsten samples taken from: 1) powder metallurgical tungsten "normally" doped with potassium-silicon-aluminum oxides (final contents inppm: K, 100; Si, 100; Al, 20; Cr, 20; Fe, 50; Mo, 400; Ni, 10) and in the form of: a) a 10-mm-diam swaged ingot annealed at 1600°C, the grain sizes varying between 15 and 250 p; b) a sheet rolled at about 800°C and recrystallized at 2000°C7 the grain sizes varying between 15 and 150 p; c) a 2-mm-diam swaged rod, as-worked, with elongated grains (average diameter of about 25 , lengths up to 1 mm); 2) undoped electron-beam-melted tungsten with very large grains (contaminations in ppm: K < 10; Fe < 20; Cr < 10; Cu < 0.1; Ni not detectable; inter-stitial~ not determined). B) Single-crystal samples taken from: 1) pure tungsten grown on a Pintsch wire by the van Arkel procedure (main contaminations inppm: Mo, 100; Si < 10; Cu and Fe, 2; A1 < 2; interstitials not determined); 2) zone-melted undoped tungsten (analysis as under A2); 3) large crystals in secondary recrystallized tungsten

Jan 1, 1969

By George V. Smith, Daniel E. Sonon

Various mechanical properties of the Ni-Co-C alloy system were investigated to delineate the strengthening effect of carbon. Carbon concentration, cobalt concentration, vain size, temperature, and strain rate were varied so that thermal activation analysis and the Hall-Petch analysis could be used to evaluate the strengthening effect of carbon. Increasing carbon increased the strength of nickel and a Ni-60 pct Co alloy , with the effect becoming more pronounced at lower temperatures. Yield stress depended linearly on carbon concentration in nickel, but it depended on the square root of carbon concentration in the Ni-60 pct Co alloy. The Hall-Petch slope of nickel increased with carbon concentration; however, that of the Ni-60 pct Co alloy did not. The yielding behavior of these alloys was sensitive to composition, grain size, and temperature. Cobalt eliminated serrations in the flow curve of carbon-containing nickel at 300&apos; and weakened them severely at higher temperatures. Pairs, or clusters, of carbon atoms appear to be responsible for the observed strengthening behavior. FLINN&apos; conducted several experiments with carbon in nickel in an effort to provide information on the strengthening effect of interstitial impurities in solid solution in fcc metals and alloys. Strengthening which increased with decreasing temperature led him to conclude that carbon causes Cottrell locking in nickel. Fleischer2 analyzed Flinn&apos;s data and calculated that the strengthening effect of carbon in nickel was smaller by a factor of fifty than the strengthening effect of carbon in a! iron. Fleischer2 termed the magnitude of strengthening of carbon in nickel "gradual" and that of carbon in a! iron "rapid". He attributed "gradual" hardening to hydrostatic strains and localized changes in modulus of elasticity around solute atoms, whereas he attributed "rapid" hardening to tetragonal strains around solute atoms. Sukhovarov et a1.3-7 reported strain aging and serrated plastic flow in nickel, both of which they attributed to the presence of carbon. Serrated plastic flow has been rationalized by a process involving a series of dislocation pinning and multiplication steps.8, This process is more probable when screw dislocations are strongly pinned. Screw dislocations cannot be pinned by pure hydrostatic forces from the symmetrical strains of an interstitial impurity in an fcc lattice, except for small, second-order effects. However, they might be pinned by localized changes in modulus of elasticity around solute atoms,&apos; by the pinning of the edge components of the partial dislocations of an extended screw dislo~ation,&apos;~ or by clustered groups of solute atoms whose net elastic stress field is unsymmetric. The purpose of the present work was to investigate various mechanical properties of the Ni-Co-C a1loy system which are sensitive to pinning effects in order to delineate the specific pinning mechanism of carbon. Carbon concentration, grain size, temperature, and strain rate were varied so that thermal-activation analysis and the Hall-Petch analysis could be used to evaluate the pinning mechanism. Cobalt was added to lower stacking fault energy so that the number and extension of split, screw dislocations would be increased in order to test the possibility of pinning by carbon at extended screw dislocations. EXPERIMENTAL PROCEDURE Nickel and cobalt (both 99.98 pct-. pure) were melted with graphite in stabilized zirconia crucibles and cast at lo-&apos; Torr to form Ni-C and Ni-60 pctCo-C alloys. Two ingots were heated to 1250°C and were forged to 1-in.-sq bars. These bars were machined to 4-in.-round bars, and then swaged cold to 0.144-in. -diam rods. Reductions in area of approximately 75pct were used with intermediate anneals at 900°C for 1 hr. The carbon content of batches of 0.144-in.-diam rods from each ingot was reduced to two levels by annealing 5-in. lengths in palladium-purified, dry hydrogen at 1100°C for 25 and 100 hr. The remaining material from each ingot was annealed at 10"5 Torr for 1 hr at 1100"~. These treatments gave a total of three carbon levels for both the nickel and the Ni-60 pct Co alloy. The 0.144-in.-diam rods were swaged to 70-mil wire, cut into test specimens, and then re crystallized at lom5 Torr in capsules for 1 hr at temperatures ranging from 760" to 1050" ~. The capsules were broken and the specimens were immediately quenched into water. Average grain size was measured using Hilliard&apos;s method of circular intercepts." Annealing twin boundary intercepts were counted in addition to grain boundary intercepts to establish an average grain size. Average grain sizes ranged from 5 to 140 p depending on the cobalt concentration and re-crystallization temperature. Tension tests were made in duplicate at various temperatures at a crosshead speed of 8.34 x 10"4 in. per sec with an Instron Universal Testing Machine. Specimens of 1-in. gage length with soldered ball ends were used at atmospheric and cryogenic temperatures. Pinch grips were used on specimens at elevated tem-

Jan 1, 1969

The design of the grinding section is discussed and details are given of the equipment installed for the autogenous grinding of ores from the C.S.A. mine at Cobar.The first section of the concentrator commenced treating ore in June, 1965 and operating experience and maintenance requirements since that time are outlined.

Jan 1, 1969