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By R. F. Hehemann, D. J. Cometto, G. L. Houze

The w transformation in the Zr-Nb system was studied using X-ray diffraction, dilatometric, re-sistornetric, hardness, and metallographic techniques. w forms in a diffusionless, completely reaersible manner on quenching and in a diffusion-controlled manner- on aging. The temperature at which w begins to form on quenching was determined as a Junction of composition and was found to decrease with increasing solute content. w formed bv aging establishes a metastable equilibrium with an enriched ß phase. The ß/w + ß transus has been determined for this metastable equilibrium and employed to rationalize retrogression and reversion phenomena observed in these alloys. The decomposition mechanism is discussed in terms of a gradual or continuous transformation from ß to the w state. BETA- stabilizing alloying elements lower the MS temperature of the martensitic bcc (ß) to hcp (a') transformation in zirconium and titanium alloys. In certain titanium alloys, a lower symmetry modification of the martensitic structure, termed (a"), also has been reported.1,2 These martensitic transformations are suppressed when the amount of the ß-stabilizing element exceeds a critical level. However, the high-temperature ß phase cannot be quenched to room temperature without change. At alloy contents just above the critical level, |ß trans-forms to the w phase when cooled rapidly.3-6 The amount of w in quenched alloys is reduced by increasing alloy content, and this phase virtually disappears above a critical composition.5 In addition to the transformation during cooling, w also can be formed by aging ß at temperatures below approximately 500°C, and significant alloy enrichment of retained 13 accompanies the isothermal transformation.1-8 The structure of LC is closely related to that of the ß from which it forms.9-15 The bcc (ß) lattice can be generated using a hexagonal cell with three atoms located at (000) and ±(2/3, 1/3, 1/3). This cell has an axial ratio of 0.612 and is oriented with respect to the cubic cell such that (0001)H (111)C and [1120]H [101]C. Consequently, there are four possible orientations of the hexagonal cell, associated with the four (111) planes of the bee lattice. Formally w can be obtained from 0 by allowing the two atoms at the ±(2/3, 1/3, 1/3) positions to approach the coordinates ±(2/3, 1/3, 1/2) and there are four equally probable orientations of w for each 0 grain. In titanium alloys w retains the cubic axial ratio of 0.612" and hence also can be indexed as triply cubic, but this is not the case for aged Zr-Nb alloys where w is clearly hexagonal with an axial ratio of 0.622." The lattice parameters and atomic positions of w depend on thermal history and alloy content. The atomic positions (000), ±(2/3, 1/3, 1/2) provide reasonable agreement between calculated and observed diffracted intensities for w in the fully aged condition.10,14 In the quenched condition, on the other hand, the atoms appear to be displaced from the central plane12,13,15 and assume positions ±(2/3, 1/3, Z = 0.42-0.48) rather than ±(2/3, 1/3, 1/2). This results in a structure with trigonal rather than hexagonal symmetry. The readily detectable parameter and axial-ratio changes of w in Zr-Nb alloys make this system especially attractive for studying the structural changes that occur in the formation and aging of w. Particular attention in this investigation has been directed to the relationship between the structure of w in the quenched and aged conditions, and to certain aspects of the reaction kinetics. MATERIALS AND PROCEDURE Zr-5, 12, 17.5, and 25 pct Nb alloys were prepared by a double arc-melting practice, encased in stainless-steel cans and hot-rolled to 1/8-in.-thick sheet.* Charged weights have been employed for the niobium contents and interstitial analyses are reported in Table I. Dilatometric, X-ray diffraction (filtered CuK, and MoK, radiation), metallographic, and hardness techniques have been employed to follow the transformations during isothermal and quench-aging heat treatments. In quenched specimens, the electrical resistivity also was studied. Betatizing was conducted for 1 hr at 900°C. With the exception of the isothermal dilatometric studies, samples were

Jan 1, 1965

By Robert E. Green

Experiments were performed in order to investigate the influence of magnitude of driving force, recouery, and previous heat treatment on grain boundary migration in deformed aluminum crystals. The frequency of occurrence of strain-free grains possessing Preferred crystallographic orientations was studied both as a function of heat treatment and as a function of amount of deformation of the matrix crystal. Aluminum of such composition as to exhibit precipitation-hardening behavior was used. CONSIDERABLE work has been devoted to the factors influencing grain boundary migration in metals.1'52 Aust and Rutterl-9 have studied grain boundary migration into matrix crystals containing a striation substructure, which provided a thermally stable driving force during the course of the migration experiments. These authors state that, while variations in the striation pattern were sometimes observed, it was possible to obtain reasonably uniform and reproducible striation structure by careful control of the solidification conditions. Admittedly, this source of driving force is a unique one and has served well in numerous experiments. However, although the striation substructure provides a thermally stable driving force, the subject of its reproducibility from crystal to crystal is questionable. In fact, Aust and Rutter3 attribute the scatter shown in some of their experimental points and several anomalies in boundary migration rates to variations in the substructure driving force along a single specimen. A further limitation on striation-induced driving force is that the driving force cannot be varied over wide ranges in a controlled manner. More often used as a source of driving force is the strain energy stored in a crystal during plastic deformation. This type of driving force has the disadvantage that it is not thermally stable due to recovery taking place simultaneously with the grain boundary mobility measurements. On the other hand, this strain-induced driving force is very reproducible from crystal to crystal since it is very easy to grow single crystals possessing the same purity and crystallographic orientation and then to strain them identically. In order to measure grain boundary migration rates two different methods are primarily used. Most often the technique employed is the heat-cool-etch method1' which involves thermal cycling, while the other technique, developed by Graham and Cahn11 using an X-ray diffractometer and goniometer furnace, involves continuous heating only. Thus the influence of thermal cycling vs continuous heating is a factor to be considered in grain boundary migration rate measurements, particularly in cases where the source of driving force is the strain energy stored in the deformed matrix, and recovery is likely to occur. Numerous recent investigations have shown that extremely small impurity additions to zone-refined metals exert a marked effect on grain boundary migration rates1-5, 9, 12-27 and a few have considered the effect of the distribution of impurities.28-35 The concentration of impurities and their distribution as influenced by heat treatment must also be taken into account in migration-rate studies. In the present article consideration is given to the influence of the magnitude of driving force, recovery, and previous heat treatment on grain boundary migration rates. In order to vary the driving force over a large range it was necessary to use as a source of driving force the energy stored in the matrix crystal during plastic deformation. A majority of the investigations were performed on aluminum specimens which were of such compositions as to exhibit precipitation-hardening behavior.

Jan 1, 1965

By Edna A. Dancy, Ronald L. Pastorek, Gerhard J. Derge

In an earlier study1 in this laboratory, it was found that there is a minimum in the specific conductance of Ni-S melts in the region of the stoichiometric composition, Ni3S2. This and similar observations on other sulfide1 and telluride2 systems suggest that short-range order exists in the molten phase for several hundred degrees above the melting point, and a qualitative energy-band model has been proposed, with intrinsic semiconduction at the stoichiometric composition and degenerate electron and hole conduction at metal- and tellurium-rich compositions. This suggestion has been substantiated for the telluride systems by Seebeck coefficient measurements which showed a change in sign from negative on the metal-rich side to positive on the tellurium-rich side. In the present investigation, in order to substantiate still further the proposed model, Seebeck coefficient determinations have been extended to the Ni-S system over a composition range in the vicinity of Ni3S2. The experimental method was essentially the same as that used for the telluride systems, with minor modifications on cells for high sulfur melts to permit the use of tungsten wires and W— W-Re th~rmocouples instead of the chrome1 or alumel wires and chromel-alumel thermocouples originally used. Chrome1 and alumel both deteriorate very rapidly in atmospheres containing sulfur. The Ni-S alloys were prepared as described in the conductivity paper. Initially, a portion of the solidified melt was analyzed at the end of a run, but after this was found to be inaccurate because of segregation during cooling, the whole sample was analyzed. The nickel content, only, was determined, the sulfur content being obtained by difference. The results are summarized graphically in Fig. 1, and clearly show a change in the sign of the Seebeck coefficient in the region of the stoichiometric composition. This change of sign near Ni3S2, coupled with the minimum in the conductivity, is suggestive of an intrinsic semiconductor at the stoichiometric composition, with degenerate electron and hole conduction on either side of this composition, in keeping with the proposed model. The negative temperature coefficient of conductivity, normally indicative of metallic conduction, is not inconsistent with this model. In the completely degenerate region it would be expected, while in the vicinity of Ni3S2 the suggestion originally made by Argyriades, Derge, and pound3 for the Fe-S system can probably be applied. They proposed that the forbidden gap between the valence band and the conduction band is small, and that the increase in the number of the conducting species with increase in temperature is not large enough to compensate for the loss of mobility through thermal scattering. The research was sponsored by the Office of Naval Research under Contract NONR-760(22) Project NR 039-081. 'E. A. Dancy and G. J. Derge: Trans. Met. Soc. Aime, 1963, vol. 227, pp. 1034-38. 'E. A. Dancy: Trans. Vet. soc. AIME. 1964, vol. 233, pp. 270-77. 'D. Argyriades, G. Derge, and G. M. Pound: Trans. Met. Soc. . 1959, vol. 215, pp. 909-12.

Jan 1, 1965

By E. Miller, J. M. Eldridge, K. L. Komarek

The liquidus curve of the Mg-Pb system was accurately redetermined. The compound Mg2Pb decomposes peritectically at 538.2° ± 0.3°C to liquid and to a compound p' which melts congruently at 35.0 at. pct Pb and 549.0° ± 0.3°C. The solidus curve of ß' was determined. X-ray diffraction studies indicate that 4' has an orthorhombic structure. Activity values of magnesium calculated from the phase diagram agree with those published in the literature. EXPERIMENTAL thermodynamic properties of binary metallic systems have to be consistent with values calculated from the phase diagram. In systems forming intermetallic compounds the shape of the liquidus curve near a compound is determined by the thermodynamic properties of the coexisting solid and liquid phases. Hauffe and Wagner' neglected the temperature dependence of the chemical potentials and obtained the potential differences of the components of the liquid alloys, relative to stoichiometric liquid. Their calculations were based on the liquidus curve and on the heat of fusion of the compound, and were only valid near the congruent melting point. Steiner, Miller, and Komarek2 developed equations which account for the temperature dependence and obtained the chemical potentials of liquid Mg-Sn alloys over the entire phase diagram from the liquidus and solidus curves and from enthalpy values with the pure components as the standard states. The Mg-Pb phase diagram has been studied by several investigators whose results have been compiled and critically evaluated by Hansen.3 Although the liquidus curve was poorly defined, the general features of the diagram, i.e., one congruent melting compound, Mg2Pb, of essentially stoichiometric composition, two eutectics, and limited terminal solid solubilities, seemed to be suitable for a similar thermodynamic analysis. A careful redeter-mination of the liquidus by thermal analysis revealed, however, the existence of another compound. The liquidus curve between the two eutectics was precisely delineated and the structure and solidus curve of the new compound were investigated. The revised phase diagram was thermodynamic ally analyzed to evaluate the activity of magnesium in the liquid alloys. EXPERIMENTAL PROCEDURE The magnesium metal (Dominion Magnesium Ltd., Toronto, Canada) had a purity of 99.99+ pct; lead (American Smelting and Refining Co.) contained 99.999 pct Pb. Most experiments were carried out in graphite crucibles. Several experiments were made in high-purity alumina (Triangle R.R., Mor-ganite, Inc.) and in Armco iron crucibles to test the inertness of the graphite crucibles. Chemical analysis of magnesium and detailed description of the procedure for thermal analysis have been given previously. For the determination of the solidus curve of the compounds, specimens of initial composition Mg2Pb were equilibrated in a closed isothermal system with magnesium vapor. The source of the magnesium vapor was an alloy which had a gross composition lying in the 0' + L field at the temperature of equilibration. As equilibrium was approached, the specimens lost magnesium to the two-phase reservoir thereby lowering the activity of magnesium in the specimens until activity and composition equaled that of the ß'/ß' + L boundary. Crucibles (1.9 cm ID by 2.2 cm OD by 4.1 cm high) and tightly fitting lids were machined from a molybdenum rod; small, shallow trays were fashioned from thin (0.005 in.) molybdenum sheet, and all the molybdenum components were degreased in hot carbon tetrachloride and then dried. The pieces were then degassed in vacuum at 950°C for about 6 hr. The two-phase alloy was placed at the bottom of the crucible and small specimens of the Mg2Pb compound, weighed on an analytical balance, were placed in two molybdenum trays above the two-phase alloy. The crucible was closed by forcing its lid on and then inserted in a titanium crucible. This crucible was evacuated, flushed twice with argon, and welded under argon. The specimens were equilibrated for about 1 week in a resistance furnace regulated by a Celectray controller, and the runs were terminated by water quenching. The specimens were again weighed and the equilibrium compositions were calculated on the basis that the weight losses were solely due to a loss of magnesium to the two-phase alloy. The structure of the B' phase was investigated by the Debye-Scherrer X-ray diffraction technique. Selected ingots from thermal-analysis experiments containing about 35 at. pct Pb were re-melted, slowly cooled, and crushed in an argon-filled glovebox until the entire ingot passed through a 50-mesh sieve. The powder was thoroughly

Jan 1, 1965

By P. G. Sprang, S. Rosen

The Y-Al- C ternary phase diagram for the com -position range from 55 to 100 at. pct Y and for a temperature of 950°C has been constructed from metallographic and X-ray diffraction data. The significant features of the isothermal section which is presented are the small solubility of aluminum in the binary Y3C phase and the presence of a ternary carbide phase with a small homogeneity range around the composition Y3AlC. The similarity in structure and composition between these two carbide phases is discussed in the light of the misci-bility gap which exists between room temperature and 1300°C, which was the temperature range studied. THE occurrence and stability criteria of ternary T3BC, carbide phases having the L'12 structure and the general formula T3BCx have been discussed in detail by stadelmaier1 and more recently by the present authors., Stadelmaier found many representatives of these phases formed between the T metals Mn, Fe, Co, and Ni and the B metals Mg, Al, Zn, Ca, Ge, Cd, In, Sn, Hg, T1, and Pb. The present authors reported on a new series of iso-structural carbide phases formed between the T metals of the Sc group and the B metal, aluminum. These new phases are unique in that many of the Sc group elements form stable binary carbide phases which occur about the composition T3C and which crystallize with a structure similar to that of the T9BCx ternary carbide phases. Furthermore, these binary and ternary phases are found to coexist in equilibrium with each other. The similarity in structure and composition between, for example, Y3C and Y3AlC in the light of the mis-cibility gap which had been found to exist between these two phases indicated a need for a more thorough knowledge of the phase relations which occur in alloys based upon these compositions. Consequently, an investigation of the phase equilibria in the yttrium-rich portion of the Y-A1-C phase diagram was undertaken. The limiting Y-A1 binary diagram determined by Lundin and Klodt3 and the results of Spedding et al.4 governing the Y3C phase were used as guides in , constructing the diagram. EXPERIMENTAL Alloys weighing about 10 g were prepared by arc-melting powder compacts made from the various components on a water-cooled copper hearth using a tungsten electrode in a gettered argon atmosphere. Good homogeneity was obtained by melting the alloys three times. The purity of the yttrium used was 99.9 pct (0.07 pct rare earths). The purity of the aluminum and the carbon was 99.99 pct. The results of chemical analysis on five representative alloys showed that losses during the alloying process were predominantly carbon losses and that in no instance did the measured concentration of this component differ by more than 3 at. pct from the intended composition. For this reason the alloy compositions which are reported are those of the charges prepared for melting. Three alloys which were analyzed for copper, tungsten, nitrogen, and oxygen compositions showed that no contamination had occurred either during casting or during the subsequent annealing treatments. For the major part annealing treatments were carried out on specimens which were placed in

Jan 1, 1965

By H. Fechtig, R. H. Buck, A. G. Guy

MULTIPHASE diffusion has been studied for many years in two-component systems1,2 and many of the experimental aspects are now fairly well understood.314 Although by no means all of the problems connected with the two-component case have been solved,' attention has recently been directed to the more complex situation involving three components. The pioneer work of Clark and Rhines6 yielded a qualitative picture of the types of behavior that can occur, and Clark7 has suggested conventions for describing the various phenomena. Kirkaldy and co-workers8,9 have made quantitative studies in several ternary systems and have offered explanations of the occurrence of isolated and nonisolated precipitates. At present, however, there is no comprehensive theory for the variety of phenomena observed in ternary, multiphase diffusion. By analogy with several studies that have been made of multiphase diffusion in the binary Cu-Zn system,2'10'11 a similar exploratory study was made of Cu-Zn-Ni alloys lying along the line in the ternary diagram from the point 80 Cu-20 Ni to the zinc corner of the diagram, Fig. 1. A principal question to be answered was whether initially plane interfaces would remain plane during the course of one-dimensional diffusion. The diffusion specimens studied are described in Table I. The five separate alloys from which they were made were melted in evacuated Vycor capsules from 99.9 pct purity copper, zinc, and nickel. Since some of the alloys were too brittle to be swaged, all of the alloys were used in the cast condition. To facilitate later homogenization, the molten alloys were solidified by plunging the capsule in water. Homogenization heat treatment was done at 720°C for 20 hr. The five nominal compositions in weight percent zinc and nickel, respectively, were: 37.5, 12.5; 44.0, 11.2; 50.0, 10.0; 55.0, 9.0; 65.0, 7.0. Ln Table I the alloys are identified only by their zinc content. Sandwich-type diffusion specimens were prepared by pressure welding disk specimens, each about 3 mm high by 10 mm in diameter. Welding was done in a special threaded vise which was heated at 500°C for about an hour in an atmosphere of flowing hydrogen. A measurement of the separation of the phase interfaces was made on a polished flat on the welded specimen, and then the specimen was sealed in an evacuated capsule and given the diffusion treatment shown in Table I. The diffused specimen was sectioned longitudinally

Jan 1, 1965

By Mark J. Klein

An internal-friction profile induced by nitrogen in Cr-35 at. pet Re was studied as a function of nitrogen concentration and heat treatment. From these studies, the solubility of nitrogen in this alloy was deduced. The equilibrium solubility of nitrogen in chromium does not appear to be substantially changed by the addition of 35 at. pet Re to chromium. However the precipitation kinetics of nitrogen from solution are significantly decreased. IT has been found that rhenium has a beneficial effect on the low-temperature ductility of Group VI-A metals. As part of a study to investigate the mechanism of this increased ductility, it was of interest to compare the concentration of interstitials retained in solution in one of these ductile bee alloys with the concentration retained in solution in its base metal. In this regard, a study of the solubility of nitrogen in ductile Cr-35 at. pet Re was selected for this phase of the investigation because the solubility of nitrogen in the base metal, chromium, has been determined over a fairly large temperature span.1-3 In addition, nitrogen is known to have an embrittling effect on chromium,4 but does not appear to have a comparable embrittling effect on Cr-35 at. pet Re.5 The experimental method selected for this study was the measurement of internal friction. This technique allows interstitial-concentration measurements to be made in bee metals that are sensitive to small changes in the concentration of a particular interstitial, even when other interstitials are present. When subjected to a cyclic stress, interstitial atoms in solid solution give rise to an internal-friction peak whose origin is the stress-induced ordering of interstitials into preferred lat- tice sites. These internal-friction peaks signify a dissipation of elastic energy which is greatest when the period of oscillation is comparable with the relaxation time for the attainment of an equilibrium interstitial distribution. For dilute interstitial binary alloys, the height of the internal-friction peak is proportional to the concentration of interstitial atoms in solid solutions. snoek8 has shown that the internal friction, Q-1, may be expressed by the equation where A is the relaxation strength, ? is the angular frequency, and 7 is the relaxation time. The relaxation strength, A, is proportional to the concentration of interstitials taking part in the relaxation if no interaction occurs between solute atoms. Thus values of peak height, which can be determined as a function of temperature, give a measure of the relative concentration of interstitial atoms in solution at various temperatures. If equilibrium has been attained, the peak heights will be proportional to the interstitial solubilities. The constant that relates A to the interstitial concentration can be determined experimentally from peak-height measurements as a function of concentration for specimens of constant crystallographic orientation. When this has been done, Q-1 measurements can be used to determine solubilities according to the equation C - KQ-1 where C is the soluble interstitial concentration and K is a constant that can be experimentally determined. It is possible, however, that lattice imperfections may bind interstitials to certain lattice sites. Internal friction does not measure these interstitial~, but does measure interstitials which are free to move in the normal lattice sites when subjected to an applied oscillating stress. On alloying the pure metal with a substitutional

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Jan 1, 1965

By W. C. Hayes

The site selected for the United States prototype pumped storage project of Union Electric CO. was Proffit Mountain, five miles from Taum Sauk, the highest point in Missouri. Factors influencing final location were: high local relief; satisfactory rock type and structure; and an economic location in respect to existing transmission systems. The upper reservoir was constructed by excavating rhyolite porphyry from the crest of Proffit Mountain and constructing a rock fill dike encircling the area to form a 4350-acre foot reservoir. A 6564-ft tunnel connects the upper reservoir with the generating and pumping facilities. A concrete gravity dam on the East Fork of the Black River forms the 6350-acre foot lower reservoir. Precambrian rhyolite porphyry forms the crest of Proffit Mountain and the floor of the upper reservoir. The tunnel was excavated in rhyolite prophpy, granite porphyry, dolomite, shales and conglomerate. Abutments and the foundation of the gravity dam are in rhyolite porphyry, and much of the valley floor of the lower reservoir is underlain by dolomite and shale. Core drilling provided data on soundness of rock type, structure, depth of weathered zone and potential water loss in the fractured igneous rocks. After a six-year study of pumped storage and cost comparison with alternate stream generating units, the Taum Sauk pumped storage project was authorized by Union Electric Co. on Dec. 11, 1959.' The site selected is located in the St. Francois Mountains of southeast Missouri approximately 90 miles south of St. Louis (Fig. 1). The lower reservoir was provided by damming the East Fork of the Black River, a small tributary of the Black River with a minimum flow of about 1 sec ft. Construction of the upper reservoir was effected by quarrying the crest of Proffit Mountain - five miles from Taum Sauk Mountain, the highest point in Missouri — to provide material for a rock fill dike surrounding the quarried area. This provided a 55-acre mountain top lake with a water depth of 92 ft (Fig. 2). A vertical shaft and tunnel connect the upper and lower reservoirs through the two reversible pump-turbine motor-generator units operating under 800 ft of hydraulic head (Fig. 3). The output rating of the plant is 350,000 kw with daytime generation of about 2.2 million kw-hr under normal use. Night pumping will replenish water to the upper reservoir in about 91/2 hours3. The automatic operation is remotely controlled from the Osage plant and from the dispatchers office in St. Louis. GENERAL GEOLOGY Mountains of the St. Francois area consist of Precambrian granites, granite porphyries, extrusive fel-sites and basic dikes. Basal conglomerates overlain by Upper Cambrian Bonneterre dolomites and shales onlap the exhumed Precambrian knobs and hills and are exposed in the narrow valleys. Cambrian and Ordovician residuum as much as 200 ft thick is present on the slopes of many hills. Proffit Mountain consists of rhyolite porphyry and granite porphyry. All excavation for the upper reservoir was in rhyolite porphyry, and the same rock is present under the Bonneterre at the plant site and under alluvium at the lower reservoir dam site. The region has been dissected to the stage of early maturity with only small upland flats remaining. Considerable local relief (a requisite for the project) approaches 1000 ft. Streams flowing across the Precambrian ridges have formed restricted narrows, termed shut-ins. A shut-in approximately two miles downstream from the plant site provides an excellent site for the lower reservoir dam. TEST BORINGS Preliminary to final approval of the project, 12 test borings were made to determine subsurface geologic conditions (Fig. 2). Drill hole No. 12 at the lower reservoir dam site showed 20 ft of alluvium over solid rhyolite porphyry. Drill holes No. 1, 2 and 3 were drilled in the tail race area to depths of 66 ft, 75 ft and 95 ft respectively, and all bottomed in Bonneterre. Drill hole No. 4 at the plant site provided NX core to a total depth of 98 ft in Bonneterre. Drill

Jan 1, 1965

By Goerge F. Weaton

Since 1909, when an agreement between Minnesota's Tax Commission and the University of Minnesota's School of Mines was worked out, it has been the annual responsibility of the School to evaluate and classify the iron ore deposits within the State. These unique duties of an academic institution have provided School officials with an excellent view of the past, present and probable future of the mining industry in Minnesota as the average grade of iron ore (excluding taconite) * diminishes while at the same time it competes with beneficiated taconites and foreign high-grade ores for use in America's eastern blast furnaces. SYSTEM OF EVALUATION In the latter part of November of each year, the Mining Division of the Department of Taxation makes a preliminary study of the active mines which the Department wants the School of Mines to review. These are discussed with the engineers of the Ore Estimate Division of the School of Mines and with the mining companies. After these discussions, a list of the mines of each of the major operating companies is submitted to the Ore Estimate Division of the School of Mines with the request that these properties be reviewed by them as of the next assessment date (May 1st). At the same time, a letter is sent to the mining companies requesting that they submit to the Division their own estimates on the selected mines operated by them, together with all computations, drill records, maps and cross-sections. The mining companies are re- quested to send in this information during the first half of the year, and, as far as is possible, they have always complied with this request promptly. Much of this information received by the School of Mines is of a confidential nature and is treated as such.

Jan 1, 1965

By J. F. Shirley, H. K. Burke

In January, 1964, three years of laboratory and pilot plant test work reached its culmination. The San Manuel Div. of the Magma Copper Co. switched its molybdenite extraction circuit from the sodium hypochlorite-ferrocyanide process to the new process described in this paper. The San Manuel Div. Concentrator of the Magma Copper Co. is located near San Manuel, Ariz., approximately 45 miles northeast of Tucson. The concentrator treats approximately 35,000 tons of ore per day containing about 0.85% copper and 0.025% molybdenite. The San Manuel ore body is a disseminated copper deposit in quartz monzonite and quartz monzonite porphyry. The primary copper mineral is chalcopyrite; minor amounts of chalcocite, bornite and covellite are also present in varying degrees. Pyrite makes up somewhat more than half the sulfide content of the rock. The molybdenite is nearly always found on fracture faces or associated with quartz veinlets.' On January 9, 1964, the sodium hypochlorite-ferrocyanide process that had been used for molybdenite recovery was replaced by the following process: 1) A conditioning step with hydrogen peroxide, sulfuric acid, sodium cyanide and zinc sulfate. 2) A two stage rougher flotation step with stove oil and sodium ferrocyanide. 3) One cleaning step with sodium ferrocyanide. 4) One cleaning step with sodium hypochlorite and potassium ferricyanide. 5) Four cleaning steps with an anti-foam Exfoam 636 and potassium ferricyanide. COPPER CONCENTRATOR Since molybdenite recovery is closely allied with previous steps in the operation, the copper concentrator will be briefly described first. The ore is ground to approximately 5% plus 65-mesh and 65% minus 200-mesh in a two-step grinding circuit consisting of rod mills in open circuit and ball mills in closed circuit with rake classifiers. A straight forward rougher circuit producing only one concentrate is used. The rougher concentrate is combined with the discharge from the regrind ball mills and is then cycloned, with the overflow going directly to the cleaner circuit and the underflow going to the regrind mills. The feed to the cleaner circuit is approximately 90% to 94% minus 325 mesh. The cleaner circuit consists of two stages in which the tailing from the final cleaner stage is returned to the primary cleaner and the primary cleaner tailing is returned to the rod mill discharge at the head of the circuit. Approximately 0.013 lb of the allyl ester of amyl xanthate (S-3302) per ton of ore is added to the rod mills and approximately 0.006 lb of sodium isopropyl xanthate (2-11) per ton of ore is stage added down the rougher banks. The frother used is methyl iso-butyl carbinol (MIBC) and it is added at various points in the grinding and the rougher flotation circuits. Lime is added to the ball mills and/or to the rod mills to maintain the desired pH in the rougher flotation. The rougher flotation has been operated at various pH levels between 10.5 and 11.5. Fuel oil is added in the regrind mills at a loading of approximately 0.01 lb per ton of ore. Factors Which Directly Affect Molybdenite Recovery: It has been found at San Manuel that, to obtain maximum molybdenite recovery, an oily type flotation collector must be added in the grinding circuit. When molybdenite is crystallized in the characteristic platy form, which appears to be the case almost all of the time at San Manuel, its surface has a greater tendency to adhere to oils than water. 2 Of the several oily type collectors available on the market, the allyl ester of amyl xanthate seems to be the best molybdenite promoter. The floatability of San Manuel's molybdenite does not appear to be affected, at least up to a pH of 11.5, by lime. It has been reported that at several plant operations high lime alkaline circuits have adversely affected the molybdenite recovery.3,4 It has been found through microscopic studies that the bulk of the chalcopyrite will float before the molybdenite in both the rougher and cleaner circuits. It is necessary to add fuel oil to the regrind mills to enhance the

Jan 1, 1965

By R. H. Tien

Temperature distribution as well as position of the solidified front is solved by means of "heat balance integral", for the case of freezing a slab with time-dependent surface temperature. Numerical solutions for the cases of linear variation and exponential decay for surface temperature are given. Application also includes solidification of casting. An increased interest in the heat-transfer problem involving a change of phase has been developed in recent years. Practical problems include solidification of a casting, freezing and thawing of soil, ice formation, and others. Despite the importance of the topic, a literature search reveals relatively few solutions which may be extended to practical problems. Due to mathematical complexity, which comes from the nonlinearity of governing differential equations, exact analytical solutions which have been published are limited to a few cases with simple boundary conditions. Although numerical solutions of these problems have become available after highspeed digital computers were introduced, lack of simple and general methods of programming for computation makes this approach impractical. The case of the semi-infinite slab with constant surface temperature was solved in the 19th century. In honor of Neumann, who first found an analytical solution, this kind of problem is generally referred to as the Neumann solution. As has been shown in Fig. 1, the problem to be analyzed is the freezing of a semi-infinite region (x > 0) which is initially liquid at the melting temperature with the surface (x = 0) maintained at time-dependent temperature. This analysis can be applied to the study of many casting processes where most of the heat removal is essentially unidirectional. "Heat balance integral" which has been used by Goodman1 is employed in this analysis. The concept of "heat balance integral" is to define a quantity, d(t), called the thermal layer. Beyond this thermal layer, for all practical purposes, there is no heat transfer, and the region is at the equilibrium temperature. "Heat balance integral" is obtained by integrating the conduction equation with respect to the space variable over this thermal layer d(t). Choosing some plausible temperature distribution, usually a polynomial or a finite trigonometric series in the space variable, this integral equation becomes an ordinary differential equation, with time as the independent variable, which can be solved by classical methods. The thermal layer and "heat balance integral" are equivalent, respectively, to the boundary-layer thickness and the momentum integral in hydrodynamics. A modern account of Prandtl's concept of the boundary layer and von Karman's momentum integral may be found in Ref. 2. Although the problem considered here has been limited initially to uniform melting temperature, the present method is equally applicable to the case with arbitrary temperature distribution in the liquid. STATEMENT OF THE PROBLEM The physical situation and coordinate system used in the problem to be analyzed are shown in Fig. 1. Notations used are listed in the table of nomenclature. Let us assume a semi-infinite region extending over positive x, initially at the uniform melting temperature. At the surface x = 0, a time-dependent temperature, which has a numerical value

Jan 1, 1965

By John A. Dunn

Continued increase in electric power requirements for mining, brought on by higher capacity mining machines and total mechanization, emphasizes the importance of proper power system design and planning. How effective a mine operates to produce quality coal at low cost depends to a great extent on how well its power system is planned and how well it is maintained. To be planned well it must be adequate to serve all the needs of the mine, it should be safe, there should be a margin for expansion, and it should be easily maintained. In planning a power system for mining coal it is helpful to establish a reliable base for estimating loads. Since most mines are served electric power by utility, power bills for similar mine loads are useful in setting up a base for estimates.

Jan 12, 1964

By George R. Huebner

The present mine at White Pine has been extracting low grade copper ore by mechanized room-and-pillar methods for approximately eleven years. Increasing depth of mining is decreasing the extraction ratio. It is desirable to mine a higher grade product by extracting values only and increase recovery of the available natural resource. These factors led to the consideration of a caving method such as longwalling. GEOLOGY The White Pine orebody consists of two mineralized shale horizons separated by a relatively barren zone of shale and sandstone. These gently dipping sediments lie at the base of the Nonesuch shale formation and are of late Precambrian age.

Jan 12, 1964

By Philip Lindstrom

T he Radon mine is in the north end of the Big Indian mining district in San Juan County, Utah. Hecla Mining Co. operated the mine from early 1955 to early 1964 through an operating agreement with Federal Resources, Inc. Development consisted of a 3-compartment, 690-ft shaft, 4 main levels driven on the ore horizon and a haulage level below the ore. Evaluation of physical and economic factors showed that this flat-dipping ore occurrence could be mined by a low-cost coal mining method. The value of the deposit was high and unusual pre¬miums were possible by clean mining. Complete extraction without loss of ore pillars, minimum ore dilution and high production per man were obtained by longwall mining.

Jan 12, 1964

By Charles M. Bayer

Reading in the AIME annual reports that certain activities have been financed by the Rocky Mountain Club Fund, less senior members of the Institute may wonder. "What's the Rocky Mountain Club?" Less youthful members will not have to wonder. They will recall the Club as an intriguing, almost fantastic organization, largely of western mining men, that flared across the New York horizon, flamed brilliantly for a little more than two decades, then sputtered out of existence- glorious even in its last flash. It was the only product of its mold, a fabulous group of magnanimous men who unhesitatingly sacrificed a cherished dream for which they had raised millions of dollars so that the money, instead of creating a magnificent club house, could be used instead to save the lives of starving Belgian children in World War I.

Jan 12, 1964

The problem of applying instrument control of variables associated with lead-zinc ore treatment has been under investigation for several years at The Zinc Corp. facilities in Broken Hill, Australia. In 1959 it was decided that there was sufficient knowledge of the problem to enable specifications to be drawn up for a system to automatically control at set conditions the roll crushing, ball milling, lead flotation and zinc flotation sections. In choosing between electrical and pneumatic control systems the broad principle was adopted that if the sensing system was pneumatic the transmission and control would also be pneumatic, whereas if electrical sensing was employed, electrical transmission and control would apply. In general. pneumatic systems were preferred owing to lack of experience with, and standardization of, the electrical systems offered at the time the specification was prepared.

Jan 12, 1964