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By W. T. Benson

The Bureau of Mines has examined selected deposits of titanium minerals throughout the United States. The titaniferous magnetite deposits in the western San Gabriel Mountains, Los Angeles County, Calif., were among those selected for study, and in 1956-58 field work was conducted to determine the extent and character of the titaniferous magnetite deposits occurring in the area. This report describes this work and summarizes earlier work in the area by the Bureau and others. The titaniferous magnetite occurs disseminated as seams and lenticular pods in an anorthosite belt 4 to 6 miles wide that trends about. N. 80° W., extending from sec. 13, T. 3 N., R. 12 W., to the west boundary of R. 14 W., at which point the titaniferous magnetite-bearing rocks disappear beneath the sediments in the Santa Clara River Valley.

Jan 1, 1962

By Foster Fraas

A method is presented for the linear evaluation of adsorption data using the equations dC = Ae-rv dv and v = [jT] - q, where dC is the phase composition increment, v a calculated parameter, T the absolute temperature, and A, r, h, g, and q the constants. The value of v is calculated from the composition C for both the adsorption surface and the immersion phase. A plot of v for each phase on Cartesian coordinates results in straight line graphs. With temperature variation, a plot of v versus,[ ] also results in straight line graphs. The equations are applicable to electronic and salt equilibria.

Jan 1, 1962

By John Wulff, David A. Stevenson

The rates of solution of copper, nickel, and three copper-nickel alloys in liquid lead were studied at 527° and 727°C under dynamic conditions. The relative velocity at the solid-liquid interface was varied from 8.65 to 125 cm per sec. Analysis of the data for the pure metals indicates that the solution rate is transport corztrolled at lower velocities, but a transition to mixed control occurs at higher velocities, higher temperatures, and higher percent saturation. 1 HE present work concerns the effect of relative velocity at a solid-liquid interface on the dissolution kinetics of pure solid materials in liquid metals. This general problem is of interest in electrode kinetics, in electrolytic processes, and more recently in the field of liquid metal corrosion. Considerable work has been done on dissolution kinetics in aqueous environments because of the obvious importance to electrolytic processes.1,2 In purely metallic systems investigation has been more limited. There are, of course, extensive data from loop tests which are used in an engineering evaluation of liq- uid metal corrosion. Here, however, the dissolution process is complicated by several interdependent processes. In general, one of two factors is considered to be rate limiting in the dissolution process: the transport of material from the solid-liquid interface into the bulk liquid, or an activation process directly at the interface. A number of studies of the dissolution rates of solid metals in liquid metals under static conditions have been published.3- Since the attendant hydrodynamic conditions imposed by thermal gradient convection and concentration gradient convection are difficult to analyze, it is doubtful if a clear interpretation of the experimental findings of these papers in terms of the mechanism involved in the dissolution process can be made. A clearer picture of the dissolution process is provided by

Jan 1, 1962

By Leonard Obert

This report describes a gage which, when used with my procedure for producing strain relief, will measure the resulting borehole deformation, From the borehole deformation the magnitude and direction of the principal stresses in a plane normal to the axis of the borehole can be calculated. The design considerations, mechanical construction, sensitivity, and stability of the gage are discussed. INTRODUCTION During the past two decades an increasing mount of consideration has been given to the problem of measuring and evaluating stress in rock around underground openings. Several investigators have made theoretical and model studies of the stress and (or) strain concentrations around simulated mine openings or in structural members, such as mine pillars or immediate roof. Other investigators have developed gages for directly or indirectly measuring stress or strain, and a number of reports present the results of measurements made with these gages. Because various methods and instruments have been developed, factors involved in this type of measurement will be briefly considered.

Jan 1, 1962

By Harry Perry

One of the most notable achievements of the iron and steel industry in the United States in this century has been the general increase in productivity of individual blast furnaces and the reduction in coke rate. Most of the improvement in furnace operations has occurred within the past decade. During this time the output of the average furnace increased about one-third, while fuel rates decreased from 15 to 20 percent. For example, in 1949, the iron and steel industry produced 811.2 short tons of pig iron per blast-furnace day with a coke rate of 1,870.4 pounds per ton of pig iron, By 1960, the average production of pig iron per blast-furnace day had risen to 1,182.4 tons, while the coke rate had decreased to 1,497 pounds per ton of pig iron. These figures are averages for the entire industry; many furnaces produced over 2,000 tons per day and one furnace, operating on pellets, reached 2,700 tons of pig iron per day, Coke rates of individual furnaces varied, but some furnaces operated on less than 1,200 pounds per ton of pig iron. The significance of this decrease in coke rate is shown clearly when data on pig-iron production and coke consumption in 1959 are compared with 1948. In 1948, 57.3 million short tons of coke was charged into blast furnaces to produce 60.1 million tons of pig iron; in 1959 only 47.6 million tons of coke was needed to produce 60.2 million tons of pig iron. Thus, in 1959, nearly 10 million tons less coke was required to produce about the same amount of pig iron as was produced in 1948.

Jan 1, 1962

By I. Nilsson, G. Sundkvist, A. Danielsson

A spectrochemical method of slag analysis is descibed which utilizes fusion of the sample with a flux, then cooling and crushing to put all samples into a common form. The powder, is then fed onto adhesive tape and passed through a spark by means of a special device to provide very reproducible discharge conditions. Combined with a direct-reading optical emission instrument, this system provides speed and accuracy of antilysis heretofore unobtainable for. slag samples by any other method. THERE are many suggested methods for spectro-chemical analysis of slags. The most important are fusion-pellet methods and solution methods. In our company the fusion-pellet method has been used earlier, and is described by Lounamaa. W. H. Tingle and C. K. Matocha have made refinements of the pellet method.' A Committee of the British Iron and Steel Research Association has investigated different methods of spectrochemical analysis of slags. Its purpose was to formulate a method which would give the complete analysis in 30 min with an accuracy of ±3 pct. The committee recommends a solution technique, which was thought to correspond best to their requirements. The method to be described is a fusion-tape method. The sample is isoformed by fusion and grinding. The powder is analyzed with the tape technique. The tape machine and some of its applications are described earlier.4'5 The powder to be analyzed is continuously fed onto a moving adhesive tape, which passes through the spark gap. The sparks break through the tape and vaporize and excite the material to be analyzed. The most outstanding feature of the tape machine is its very high reproducibility. The concept of isoformation has been introduced earlier.= It means a pretreatment of the samples to make them uniform from the spectralanalytical point of view, i.e., cancelling systematic differences between the samples. The purpose of the isoformation is to reduce the influence of particle size, as well as chemical and mineral composition. Before describing the isoformation by fusion plus grinding, which is the purpose of this paper, a few words will be said about two other types of isoformations, i.e., grinding with buffer and ion exchange plus grinding as they have been considered during the application of the tape technique for slag analysis. Grinding with buffer might be a sufficient isoformation in some special cases, where the mineral composition is defined. The time of grinding must, however, be rather long, at least 5 to 10 min, even when using such an efficient mill as the Swing Mill from Messrs. Siebtechnik, Mühlheim, Germany. This type of isoformation is not recommended due to its limitations and due to the fact that the gain in time compared with the fusion technique is almost negligible. The principle of ion exchange plus grinding and some of its applications have been described.5 The following elements of interest in slag analysis can be determined in this way: Na, K, Cu, Mg, Ca, Ba, Zn, Pb, Al, Cr, Mn, Fe, Co, Ni. The very important element Si, however, cannot be analyzed with this method. Although the ion exchange isoformation for slag analysis cannot be looked upon as a routine method, it can be used for

Jan 1, 1962

By H. H. Bleakney

The merit of reduction-in-area as a criterion of quality in metals is shown to lie in its influence on breaking stress, but the virtue of elongation is not easy to find. In order to assess the value of elongation, either as a measure of quality or as a guide to design, it will be necessary to separate the overall de-formation occurring in tension tests from the localized deformation associated with localized reduction in area. The obstacles to a successful solution of this problem have been shown to be more formidable than is generally appreciated, and a new solution to the problem has been suggested. This solution involves a de-vice by which an electric circuit is broken when the particular value of strain is reached that is to be taken as the point of separation between general and localized deformation. The report presents results from a number of tests on both low-carbon and alloy steels. These results indicate that the selected criterion of separation is accurately identified by the proposed method; that it

Jan 1, 1962

By R. Barany

The heats of formation at 298.15° K of calcium tungstate, calcium molybdate, and magnesium molybdate were determined by solution calorimetry. For the heats of formation from the elements, the values obtained were calcium tungstate, -402.4 ± 0.5 kcal/mole, calcium molybdate, -369.5 ± 0.3 kcal/mole, -334.8 ± 0.2 kcal/mole. For the heats of formation from the oxides J the values obtained were calcium tungstate, -49.2 ± 0.4 kcal/mole, calcium molybdate, -39.6 ± 0.1 kcal/mole, and magnesium molybdate, -12.9 [ ] 0.1 kcal/mole.

Jan 1, 1962

By W. M. Johns

The word "Flatland" should read "Flathead" in the title of the paper by Willis M. Johns on page 184 of the June 1962 issue. The correct title is "Belt Series in Lincoln and Southwest Flathead Counties, Montana." In the same paper, reference 12 on page 191, the publication is Bulletin 12, Montana Bureau of Mines and Geology, rather than Bulletin 17.

Jan 1, 1962

By H. A. Wriedt

A method of calculating activities in binary systems having miscibility gaps is described. The method, which applies only to the phase in which the gap occurs, is exact when the function defined by the equation varies linearly with composition. Analytical and numerical solutions (as a function of the conjugate phase compositions) are presented for two coefficients A and B from which the thermodynamic activities can be calculated. Deviations from Henry's law, calculable by the method presented, are shown graphically for the particula~ case of the component i at the edge of the miscibility gap more remote .from pure component i. For symmetrical gaps, the deviation from Henry's law at this gap edge becomes smaller as the gap becomes wider, The interrelation of gap location, the direction of departures from Henry's law and the occurrence of maxima and minzma in these departures is discussed in some detail. Values for a and for activity calculated from phase diagrams show fair to excellent agreement with corresponding experimental values in the Al-Zn and CaO-SiO2 systems. WHEN structurally similar phases, B and 6, lie at the sides of a two-phase region in a constitution diagram, it can be assumed that, stably or metast-ably, they will become completely miscible at a higher temperature. The B and 6 phases are particular composition ranges of a single B6 phase region with a miscibility gap. Below, as above, the critical solution temperature, the free energy of formation of the 06 phase is a continuous function of composition through the range of the miscibility gap. It is the purpose of this paper to use this continuous free-energy function in order to develop a simple method for computing the thermodynamic activities in the B6 solution of a binary system. To make these calculations it is assumed that the function ai, familiar from Gibbs-Duhem integrations and defined by the equation

Jan 1, 1962

By H. C. Fuller

Rhodonite, a manganese silicate, occurs as an important component of extensive veins in the San Juan district of Colorado. Recent work by the Bureau of Mines has demonstrated that typical ores of the area can be upgraded to about 30-percent manganese content. Because of their siliceous nature, such concentrates require further processing to convert the manganese into more usable forms. The investigation described in this report demonstrates the technical feasibility of producing silicomanganese from a rhodonitic concentrate by electric smelting methods. The rhodonitic concentrate used in the smelting research was prepared by dry high-intensity magnetic separation of ore from the Silver Queen vein. The concentrate contained 29 percent manganese, 2 percent iron, and 41 percent silica. The principal minerals in the concentrate were 35 percent rhodonite, 30 percent rhodochrosite, and 25 percent quartz and chalcedony. Limestone was used as the flux and coal was used as the reductant. These minerals were crushed and screened to minus 1/2-inch plus la-mesh size.

Jan 1, 1962

By W. H. Young

The thickness of the coal seam is one of the more important items influencing the productivity and general overall efficiency of operation of a coal mine. The average thickness of coal seams mined in the United States has changed very little in the past 40 years. The first measurement of thickness of bituminous coal and lignite seams was made for 1920, when the average thickness was 5.3 feet.4/ The average thickness for later years was as follows: 1945, 5.4 feet; 1950, 5.3 feet; 1955, 5.2 feet; and 1960, 5.5 feet.5/ Table 1 includes data on number and production of bituminous coal and lignite mines classified by I-foot intervals of seam thickness mined in 1920, 1945, 1950, 1955, and 1960. Though bituminous coal and lignite are mined today from seams of exceedingly variable thickness -less than 2 feet to more than 50 feet - a large majority of the production, 62 percent in 1960, came from seams 3 to 6 feet thick. This is not surprising since the coal seam of moderate thickness presents the least mining difficulties.

Jan 1, 1962

By N. Pessall, A. D. McQuillan

The phase relalionsllips in an isothernzal section of the Ti-Zr-H system at 750°Chave been investigated by measurement of hydrogen equilibrium pressures. The resulting diagram indicates that the hydride phase has an anomalously wide range of homogencity extending from 66.6 to 30 at. pct H in alloys containing about 15 al. pet Zr. Measurement of the heat of solution of hydrogen as a function of alloy composition in ß-phase alloys indicates no anomalous behavior in the region of 15 at. pet Zr, and suggests that the extensive range of homogeneity in the hydride phase at about this composition must he attributed to an enhanced stability of the, hydride phase. THE manner in which titanium and zirconium react with hydrogen and the constitutional diagrams of the two metal-hydrogen systems are qualitatively very similar,'-6 as can be seen from Fig. 1 which shows the constitutional diagrams of the two systems. Quantitatively, however, there are some differences. For example, the exothermic heat of solution of hydrogen in ß titanium is smaller than that in ß zirconium, and consequently the equilibrium hydrogen pressure of a Ti-H alloy is higher than a Zr-H alloy at the same temperature and hydrogen concentration. Other differences manifest themselves in the hydride phases which exist at high hydrogen concentrations. In the Ti-H system, above room temperature, there exists only a single hydride phase in which the metal atoms are arranged on a fee lattice, but in the zirconium system there are two hydrides, and whereas the hydride of lower hydrogen concentration has a fee structure, the higher hydride has a face-centered tetragonal structure. The tetragonal hydride retains its stability up to temperatures in excess of 450oC.7 From the foregoing, it would be expected that the constitutional diagram of the ternary Ti-Zr-H system would have a very simple form, especially as titanium and zirconium are completely miscible in both the a and ß forms.8 The present work, which consists of a study of an isothermal section of the ternary system, was carried out in order to check the assumption frequently made that the electronic structure of the two metals and the mechanism by which hydrogen is held in solution in the metals is the same for each. Although this proved largely to be true, certain inter esting and unexpected features of the ternary system emerged which must be explained before we can really say that the reactions of titanium and zirconium with hydrogen are fully understood. EXPERIMENTAL PROCEDURE The most convenient method of studying hydrogen-metal systems is by the measurement of the hydrogen pressure in equilibrium with the hydrogen dissolved in the metal as a function of hydrogen concentration and temperature. In binary systems, the results are easily interpreted in terms of alloy constitution, since two-phase regions can be recognized by the fact that the hydrogen pressure at constant temperature does not vary with the hydrogen concentration in the alloy when it is in the two-phase condition. This criterion does not apply in ternary systems, but there is usually a marked change of slope in the isothermal pressure-composition curves when a phase boundary is crossed, and with care, and a knowledge of the limiting binary systems, the phase structure of the alloys can usually be deduced. In the

Jan 1, 1962

By J. F. Neill, O&apos

The manganiferous schists occurring in the vicinity of Kings Mountain, North and South Carolina, suggest significant tonnages of potential submarginal ores. Although some reconnaissance work in connection with these deposits has been reported, no recent information has been published. Evaluation of the schists as a possible domestic manganese resource has not always adequately considered the fact that the manganese content occurs quantitatively both as oxide and as the silicate, spessartite. The Bureau of Mines investigation herein reported includes preliminary studies to indicate the extent of manganese oxide mineralization and to deter-mine the amenability of the material to sulfur dioxide leaching. The field reconnaissance studies suggest a resource containing in one area an average of 6.4 percent manganese as oxide. The procurement of depth information was beyond the scope of the investigation.

Jan 1, 1962

By F. V. Lenel, G. S. Ansell, J. A. Dromsky

The growth of aluminum oxide particles in a nickel matrix was studied eve?. the temperature vange of 2140° to 2470°F. The instability of the dispersed alumina was shown to be independent of the crystal structure of the alumina. The activation energy for the growth of the dispersed alumina was found to be 84.7 1 2.0 kcal. The particle radius increased as a function of time. These results indicate that the growth is not diffusion controlled. It is believed that the rate controlling mechanism is the dissolution of the aluminum and oxygen atoms into the nickel lattice. THE strength properties of alloys which consist of a finely dispersed second phase in a metallic matrix depend upon the spacing between the second phase particles. It is therefore desirable to achieve very fine dispersions in these alloys. Furthermore, to retain the properties these very fine dispersions must be stable during fabrication and service of the alloys. The best known of the dispersion strengthened materials, the SAP type alloys, which consist of a dispersion of aluminurn oxide in aluminum, have exceptionally good stability up to the melting point of aluminum. There is evidence, however, that other dispersion strengthened alloys, even those consisting of refractory oxides in a metal matrix, may be less stable. This investigation is concerned with the stability of Ni-Al2O3 alloys in the temperature range in which these alloys are usually fabricated. The mechanical properties of Ni-Al2O3 alloys at elevated temperatures have been previously investigated by Crelnens and rant,' and Gregory and Goetzel.2 The behavior of these alloys in stress rupture tests appears to indicate that at temperatures below 1800°F they are highly stable. There is some doubt, however, as to their stability at the higher temperatures used during the conventional fabrication. Cremens and Grant, in preparing their test alloys, cousolidated, by powder metallurgical techniques, nickel powders as fine as 0.13 µ diam and alumina powders as fine as 0.018 µ. Metallo- graphic examination of the alloys following fabrication revealed that none had interparticle spacings of less than 2 µ. Considering the size of the original component powder particles, it is likely that the dispersions coarsened during fabrication. Gregory and Goetzel, in their studies of extruded alloys of 80 pct Ni—-20 pct Cr matrixes with nonmetallic dispersion, observed a definite coarsening of the alumina dispersions in alloys sintered at 2280°F as cantrasted to those sintered at 2000oF. Similar observations on the spheroidization and growth of thoria particles finely dispersed in a nickel matrix were made by D. K. Worn and S. F. Marton.3 As a result of such coarsening, much of the effort expended in the preparation of very fine powder mixtures would be lost. The mechanical properties of the alloys which had experienced coarsening would be expected to be poorer than if the original dispersions had been retained. EXPERIMENTAL PROCEDURE Ni-Al2O3 alloys were produced from powder prepared by a coprecipitation technique. Aluminum hydroxide and nickel hydroxide were coprecipitated from chloride solutions of the metals. The mixed hydroxides were calcined to form metal oxides and the nickel oxide in the mixture was selectively reduced to nickel by treating it in hydrogen. Specimens were compacted from the resultant powder which consisted of a fine, uniform mixture of aluminum oxide and nickel particles. The compacts were sintered by resistance hot pressing4, a densification technique which requires exposure times of the order of only a second or less at elevated temperatures. A conventional sintering process was not used, since the temperature required for densification would have to be in the region in which the stability of the dispersion was to be studied. A series of hot pressed specimens were treated in hydrogen at temperatures from 2140o to 2470°F (1171o to 1355oC, for times up to 120 hr. Changes in the microstructures were studied by electron microscopy using the two-stage preshadowed carbon replica method.5 In performing a lineal analysis on a series of micrographs from each specimen it was found more convenient to determine the mean free path between alumina particles rather than particle radii as the parameter of growth. Although these quantities are directly proportional for only spherical particles, the alumina particles in these alloys

Jan 1, 1962

By John W. Weeton, Max Quatinetz, Robert J. Schafer

Nickel powders of 1-, 0.4-, and 0.2- average particle size were combined with 0.05- p MgO powder. Oxide was added in quantities of 4, 12, and 20 vol pct. The mixtures were vacuum hot pressed and extruded at 2100°F. In spite of a general tendency to growth of oxide particles during processing, dispersions of fineness comparable to those of Sintered Aluminum Powder, SAP, were achieved. A small amount of oxide considerably improved 1800°F stress-rupture strength, but further oxide addition resulted in a decrease of strength. RECENTLY there has been much speculation concerning the requisites for strong and stable dispersion-strengthened alloys. The nature of the dispersed phase, the stability of the alloys, and variables influencing the mechanical properties of alloys have been given consideration. Such topics have been reviewed by Bunshah and Goetzel. Of the many parameters related to the mechanical properties of dispersion alloys, mean free path between dispersed particles (a measure of the fineness of the dispersion), particle size, and vol pct of the dispersed phase have been shown to be very important. Generally, strength increases with decreasing mean free path, and there is an optimum vol pct of dispersed phase. Just how fine a dispersion ought to be is somewhat open to debate, but Irmann, Lenel, Backensto, and Rose, Gregory and Grant,4 and others have shown in the original SAP-type alloys, aluminum plus aluminum oxide alloys, that better strength is generally obtained with finer dispersions and the best strengths were obtained when the mean free path was less than . Further, Cremens, and rant' showed that in nickel plus aluminum oxide alloys, stress-rupture strength at 1500°F was definitely increasing with decreasing mean free path. In their investigation, however, the finest dispersions that were produced were about 2.0 mean free path. To determine the potential of the nickel plus oxide type of product, it would be neces- sary to obtain dispersions analogous to those of SAP alloys; namely, ones where the mean free path between oxides is less than . Unfortunately, however, it is very difficult to produce extremely fine dispersions of oxides in metals other than those which naturally form refractory oxide skins. There are several approaches to this problem including such procedures as mechanical mixing, internal oxidation, reduction of mixed oxides, and metal deposition from solution. Work at the Lewis Research Center has shown that metal powders 0.1p or finer could be produced by ball milling, when selected grinding aids were utilized.' Because these unusually fine powders were available, it was an initial objective of this study to determine if by mixing of these fine Ni powders with various amounts of MgO (0.05) a fine dispersion of MgO in Ni comparable to those in Al-Al203 might be achieved. A second objective was then to attempt to relate the parameters of structure to 1800°F stress-rupture strength of the alloys. Nickel powders of 1-, 0.4-, and 0.2-p average particle size were combined with 0.05- average particle size MgO powder. This oxide was added in quantities of 4, 12, and 20 vol pct. The mixtures were hot pressed and extruded at 2100°F.

Jan 1, 1962

By H. F. Weaver

The 19th National First-Aid and Mine Rescue Contest was held in the Civic Center, Charleston, w. Va., on October 2, 3, and 4, 1961. The meet was sponsored by the Bureau of Mines and the Joseph A. Holmes Safety Association, in cooperation with State mine inspection agencies, management and labor of the mineral extractive industries, and other groups interested in safety. The Arrangements Committee, as authorized by the General Committee, made the necessary arrangements for conducting the 1961 contest. Members of the Arrangements Committee were: George Trevorrow (chairman), Bituminous Coal Operators' Association; James B. Benson, Southern Coal Producers' Association; Charles Ferguson, United Mine Workers of America; Harry Gandy, Jr., National Coal Association; and James Westfield, Bureau of Mines.

Jan 1, 1962

By S. K. Mitra

A refinement of the Seeger model for intersection process is investigated which is in better agreement with experimental observations than the original. It is shown that, in single crystals, the strain hardening in Stage II is mainly due to the short-mnge interactions when intersection is the rate-controlling process. It is also demonstrated that the creep curves, as predicted by this theory, are in good agreement with the experimental observations. MOTT: Cottrell? and Seeger have developed an approximate theory for plastic deformation of single crystals over the range of variables where the strain rate is controlled by the rate of intersection of dislocations. Although it is now generally agreed that the low temperature deformation of many pure metals is controlled by the intersection mechanism, various dictates of the over-simplified Seeger model are not in good agreement with all the experimental facts. It is the purpose of this paper to reveal that by appropriate extensions of the Seeger model, particularly those suggested by Basinski: a much more reliable theory results. The refined model to be presented here will be shown to account, in a satisfactory way, for the effect of stress, temperature, and strain on the creep rate under constant stress and for the effect of temperature and strain on the flow stress in constant strain-rate tests. EXPERIMENTAL METHOD To Check the theoretical deductions, both creep and tension tests were conducted on single crystals of high-purity Al (99.994 pct Al) so oriented that both the active slip plane and the Burger's vector of the operative dislocations on that plane made angles of about 45 deg to the tension axis. Single crystals of aluminum (5/8 in. by 1/10 in. by 8 in.) were grown in a graphite mold under an inert atmosphere using the Bridgman method. The chemical composition of the aluminum is given in Table I. A common seed was used for all crystals and their orientation is shown in Fig 3. The extensometry consisted of two differential transformers with matched outputs mounted so as to measure the extension in a 2 in. gage length. The amplified difference in output of the two transformers was recorded by a potentiometer. The amplification was calibrated before each run so that one chart division of the recording potentiometer indicated a 105 shear strain on the specimen. Stresses were measured to the nearest 1 x l04 dynes per sq cm. ACTIVATION VOLUME The concept of Basinski that the activation volume is not constant but is a function of the force that aids thermal fluctuation in effecting the cutting of dislocations will be adopted in this section. The force acting due to an applied shear stress on the dislocation being intersected is where L is the mean spacing between the forest dislocations, is the Burger's vector and T is the back stress. A detailed discussion about the origin of back stress will be taken up later in this report. As shown by Basinski, the activation energy, U, that must be supplied by a thermal fluctuation in order to effect intersection, is equal to where x is the distance through which the dislocation must be translated for complete intersection, and Fm is the maximum force encountered in intersection. When the applied stress is decreased abrupt ly F also decreases and the activation energy increases correspondingly as documented in Eqs. [ 1 ] and [2]. The Seeger equation for the strain rate when the deformation is controlled by rate of intersection of where the shear strain rate (per sec) N = the number of points per unit vol at which intersection can take place

Jan 1, 1962

By Stephen Utter

This report summarizes the procedure and results of an investigation to determine the stresses in the rock around an underground opening in the Climax molybdenum mine, Climax, Colo. This study is part of an overall investigation conducted by the Bureau of Mines to determine the stresses induced by block-caving mining. The purpose of this study is to obtain estimates of the magnitudes and directions of the principal stresses, the location of the maximum stress concentrations, and the effect of topography on the stresses.

Jan 1, 1962

By P. R. Celmer, Leonard R. Weisberg

THE principle of fractional crystallization has been successfully used to prepare high-purity (99.999 pct) Ga. Hoffman and Scribnerl removed single crystals of gallium solidifying in a gallium melt, while Zimmerman2 grew single crystals from the melt by the Kyropolous technique. In contrast, attempts at purifying gallium by zone refining have been less successful. ichards, reported that despite the passage of 40 zones through a gallium ingot, there still remained 5 to 70 ppm each of Cu, Fe, Ca, Mg, Si, Al, and Ag. Previously, Detwiler and Fox4 detected only one impurity, Pb, segregating in zone-refined ingots. These surprising results prompted an investigation of the factors controlling impurity segregation in gallium. Possible reasons for this were insufficient diffusion of impurities in the melt; recontamination of the melt by its oxide film which is not affected by the passage of the zone; reaction of gallium with the boat; sudden freezing of gallium following supercooling, especially since gallium easily supercools to and trapping of impurities at grain boundaries. Impurity segregation tests were carried out by directionally freezing gallium using the Bridgman rnethd, modified in that the molten gallium is lowered out of a furnace into a slush of dry ice and trichloroethylene, thus minimizing supercooling. Since the gallium is contained vertically, the oxide film is in contact only with the tail end of the melt. It was found that Teflon makes an excellent crucible for gallium since it is quite pure, non-reactive, translucent, flexible, machinable, and is not wet by gallium. The gallium crystals could be grown at various speeds, and the melt could be vigorously stirred by a Teflon rod moving through the gallium in a vertical reciprocating fashion. Single crystals could be grown by placing a solid Teflon plug at the bottom of the melt drilled out in such a way to cause the solidifying gallium to follow a winding path. Thus, even if many crystals are originally nucleated, only one grain will predominate. The grain structure of the gallium crystals was revealed by an etchant composed of equal volumes of HC1, HNO3 and HF, diluted with water to half strength. Emission spectrographic analyses were carried out on samples removed from the front and tail ends of the resulting gallium ingots. Typical results of this study are summarized in Table I. The rate of freezing in all three cases was about 1 in. per hr. It can be seen that even though stirring of the melt does help, it is even more important to grow a single crystal of Ga in order to obtain good segregation of impurities. The effect of crys-tallinity on the segregation of impurities was previously observed6 in the directional freezing of germanium; however, in this case, the effect was much less pronounced. This dependence of impurity segregation on the crystalline perfection of Ga may be related to its thermal conductivity which is the most anisotropic of all metals.7 The anisotropic thermal conductivity can cause the solid-liquid interface to be nonuniform, thus leading to trapping of impurities during freeing, and therefore reduced segregation. In conclusion, it is indicated that zone refining of gallium would be more successful if seeding and similar precautions are taken to insure single crystal growth. The authors are indebted to Mr. H. H. Whitaker for the spectrographic analyses and to Drs. B. Abeles and F. D. Rosi for helpful advice and encouragement throughout the course of this work. This research was supported by the Electronics Research Directorate, Air Research and Development Command, under Contract No. AF33(616)-5029. REFERENCES 'J. 1. IToffmon and B. T. Scribrer: I. Research h'atl. Bur. Standards, 1935, "01. 15, p. 205. 'W. Zirnmerman: Science, 1954, vol. 119, p. 41. %J. L. Richards: Nature, 1956, vol. 117, p. 182. 'D. P. Detwiler and W. M. Fox: I. Metals, 1955, "01. 7, p. 205. 5P. W. Bridgman, Proc. Am. ilcod. Sci., 1925, vul. 60, pp. 305,385,423. "S. L1. Christian: private c ommuni cation. 'K. W. Powell: roy. Sac., 1951, vol. 209, p. 525. 'W. G. Pfann: Zone Re fining, p. 20. John Wiley and Sons, Inc., New York, L058.

Jan 1, 1962