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By J. E. Harris

By elimination of other possible nucleation processes, it has been demonstrated, for commercially pure magnesium and a Mg-Al alloy, that at stresses less than that necessary for triple-point cracking creep cavities are most probably nucleated heterogeneously at second-phase particles. Evidence for the existence of such particles is presented and the role of grain boundary sliding in the nucleation process is examined quantitatively. DURING creep deformation of polycrystalline magnesium and its dilute alloys in the temperature range 0.45 to 0.7 Tm (Tm = absolute melting temperature) cavities form mainly along grain boundaries oriented normal to the stress axis and failure eventually occurs by their growth and impingement.' The possibility of low-ductility creep failure of magnesium-alloy reactor cans during service has prompted a number of studies of cavity formation in these materials.2-5 In this paper divergent theories of cavity nucleation6-10 are examined critically and conclusions drawn regarding the most probable mechanism of formation of cavities in magnesium. The paper is divided into two parts. The first section consists of the review and quantitative assessment of the possible role of grain boundary sliding in the nucleation process. In the second part an experimental program is described where an electron-microscope technique has been used to determine if second-phase particles exist in as-received commercially pure magnesium and in a magnesium alloy 1) THEORETICAL REVIEW Possible nucleation sites for creep cavities are: a) high-angle grain boundary triple points,11-14 b) subboundary/grain boundary intersections,15-18 c) ledges in the grain boundary, 19-25 d) second-phase particles. 9,26-30 Each of these possibilities is now considered with special reference to deformation of magnesium. 1.1) Triple-Point Cracking. The stroh31 condition to nucleate fracture is: " > vr [1] where ss = applied shear stress, ? = surface energy, C = shear modulus, L = length of sliding interface. This relationship is independent of the nature of the interface and it is possible to calculate the stress concentration at the end of a sliding high-angle grain boundary and thus deduce, approximately,* the minimum applied stress necessary to nucleate triple-point cracking. Such theoretical predictions for Nimonic alloys have been made by McLean13 and found to agree quite closely with the minimum stress determined by experiment. Stresses capable of nucleating triple-point cracking should also be sufficient to nucleate fracture at a grain boundary due to intragranular slip, for the lengths of sliding interface in the two cases are approximately equal. Thus the minimum stress for triple-point cracking should represent a demarcation between failure due to general "cracking" and that due to cavitation. Hauser, Landon, and Dorn32 have demonstrated that for polycrystalline magnesium in the temperature range 78° to 298°K the fracture stress is inversely proportional to the square root of the mean grain diameter. As pointed out by stroh31 this result indicates that Eq. [I] describes the fracture characteristics of magnesium at low temperatures. Heal3 has reported that for rapid deformation (112 pct hr-1) of polycrystalline magnesium the transition from cracking to cavitation occurs in the temperature range 175" to 275°C. He also presented the fracture-stress values for the same material tested under similar conditions. From Eq. [I] taking G = 1.3 x 10" dynes , ? = 600 ergs . cm-2,33 and L = 0.017 cm, a Stroh-McLean13,31 tensile stress of -266 kg. cm-2 is calculated, corresponding to a transition temperature of -190°C; this is in

Jan 1, 1965

By Robert C. Johnson

Single crystal whiskers of ZrO2 and TiO2 were grown by solution and crystallization of these oxides in molten baths. Mixtures of Na2B407 and LiC1 were the most suitable growth media for zirconia. Sodium borate alone and Na2CO3 plus SiO2 were best suited for titania. The solubilities of zirconia and titania in molten sodium borate were determined, Whether zirconia whiskers were dendritic or nondendritic depended on the temperature used. The best single crystal whiskers were grown below 1,100° C. Titania whiskers always grew as single crystals. The tensile strengths of zirconia and titania whiskers were about 15,000 psi and 50,000 psi, respectively. Modulus of rupture was about 49,000 psi for zirconia whiskers and 75,000 psi for titania whiskers. Chemical analyses showed the zirconia and titania whiskers to be pure. The zirconia and titania whiskers were shown by X-ray analysis to be, respectively, baddeleyite and rutile.

Jan 1, 1965

By J. H. Brophy, A. L. Prill, H. W. Hayden

An error lzas been found in the conventional way of determining the time exponent of linear shrinkage for the solution-precipitation stage of liquid-phase sintering. Large amounts of shrinkage due to initial rearrangenzent result in erroneously low exponents and tni si dentification of the rate-controlling process. Two alternative, mathematically correct, methods of calculation are applied to existing data on Fe-Cu, WC-Co, and Tic-Ni-Mo. This results in reidentifi-cation of the rate-controlling process and somewhat better agreement with related data. In each case the solution-precipitation process is solution-controlled and not diffusion-controlled. THE liquid-phase sintering process has been the object of a considerable amount of research for many years. Linear shrinkage vs time data at various sintering temperatures have been used recently in an attempt to identify the prevailing mass-transport processes in a number of metallic and nonmetallic systems. There is an analytical error inherent in the methods previously used for handling data during the "solution-precipitation" stage of shrinkage which must be recognized before the correct rate-controlling processes can be determined. It is the purpose of this paper to show how the error has affected previous conclusions and to suggest corrections. A number of mechanisms have been proposed to explain experimental observations during sintering in the presence of a liquid phase. The earliest of these is due to Price, Smithells, and williamsl who attributed the observed growth of the solid phase to the simultaneous solution of smaller particles and growth of larger particles. From the work of Lenel et al.2,3 and Gurland and Norton4 has come the suggestion that the liquid-phase sintering process may be divided for analysis into three steps: 1) rearrangement upon formation of the liquid phase; 2) solution and reprecipitation of the solid phase in the liquid; and 3) "coalescence" or a final stage of sintering, characteristically slower than the solution-precipitation process. The sequence of steps is shown schematically in Fig. 1. Kingery5 presented a thermodynamic and kinetic analysis of the first two "stages" of the liquid-phase sintering process in which the functional dependence of lineal shrink- age on time at temperature was used to identify the rate-controlling mass-transport process. Table I summarizes the time dependences and processes considered by Kingery.5 This method of data presentation has been employed by Kingery and coworkers for Fe-CU,6 WC-Co, and a number of nonmetallic systems," and bv Whalen and Humenik for Tic-Ni-Mo and Fe-cu.8 In each of these studies, the rate-controlling step during the "solution-precipitation" stage was identified from the slope of the curve in that stage on a logarithmic plot such as Fig. 1. However, in all of the previous studies, at a certain composition, relatively large amounts of shrinkage due to rearrangement preceded the solution-precipitation stage. Under these conditions, the larger the amount of rearrangement shrinkage the

Jan 1, 1965

By E. R. Gilbert, D. E. Munson

Creep of copper under 75 to 1.50 kg per sq cm stresses at temperatures near the melting point was found to he a complex reaction controlled by three mechanisms acting in parallel. In order of appearance with decreasing temperature, the auerage activation energies, Qc , are 168, 79, and 24 kcal per mole. Stress dependence of the minimum creep rate was found to he an exponential for the two high-Qc processes and a power law for the low-Qc, process. Transition of control occurs from one mechanism to another. The relative transition temperature depends upon the applied stress, and the range oiler which the transition occurs depends upon the difference in the activation energies of the mechanisms. The creep behavior at high temperature is explained by the climb of dislocations through thermally or mechanically formed jogs, CREEP in pure fcc metals at temperatures in excess of one half the absolute melting point is normally controlled by dislocation c1imb.1,2 A climb model which seems applicable, according to an extensive analysis of data,3 was derived by Weert-man.4 This model assumes jog-saturated dislocations and predicts an activation energy, Qc, nearly equal to that for self-diffusion, USd. Although the requirement of jog saturation is restrictive, agreement between theory and experiment seems adequate. Many other theoretical treatments, including an early model by Mott,5 include detailed consideration of jog formation as an initial requirement for climb. These models predict activation energies for creep which differ from those of self-diffusion. Seeger6,7 postulates an observed activation energy related to the stacking-fault energy. Thus, Usd <Qc<5Usd + Uj where Uj is the jog-formation energy. Seeger incorporated qualitatively the influence of the relative numbers of thermal and athermal jogs. Expanding this concept, Shoeck8 explicitly states a function based on formation mode and relative numbers of vacancies: e r ci exp {-uf/k T} exp {-Um/k T} [ 1 ] where Uf and Um are energies of vacancy formation and migration, respectively. The concentration of jogs, Cj, depends upon the manner of jog production. For intersection jogs, Cj is not sensitive E. R. GILBERT, Junior Member AIME, formerly with De- to temperature; for thermal jogs, Cj is proportional to exp {—Uj /k T}. Schoeck regards each mode as a distinct mechanism; therefore, the mechanisms may act together.299 The diversity predicted by theory, surprisingly, has not been substantiated by experimental results. A significant investigation must include the extremes in stacking-fault energy. Extensive creep studies of aluminum10 and nickel,11,12 high stacking-fault energy metals, have been made. Comparable studies on a low stacking-fault energy metal, such as copper, have not. It is the purpose of this paper to report the results of an investigation of the creep of copper under conditions which favor thermal jogs. EXPERIMENTAL Cylindrical compression creep specimens (0.240 in. in diameter by 0.400 in. long) were machined from cold-drawn rods of electrolytic tough-pitch copper containing 0.0007 Mg, 0.002 Fe, 0.001 Ni, 0.0005 Ag, Cd < 0.005, and Pb < 0.005 wt pct impurities. Undetected spectrographically was a nominal 0.04 wt pct 0, which occurs as a Cu2O constituent distributed discontinuously at grain boundaries. Vacuum annealing at 900°C for 15 min produced a stable 0.03-mm average grain diameter. Testing was carried out using apparatus similar to that described by sherby,13 modified by enclosing platens and a push rod in a vacuum cylinder. Normally this arrangement resulted in pressures less than 10 Only a slight surface tarnish, less than 0.0005 in. in thickness, occurred during the test. The applied stress, corrected for atmospheric pressure, was maintained within 2 pct of the desired true stress by the addition of lead shot at fixed strain increments. Creep strain was measured with dial gages as a relative displacement of the upper and lower platens; accuracy of measurement was 0.0001 in. Two creep-test methods were used, the differential or cyclic temperature14 and the isothermal, to obtain creep data at stress levels of 150, 100, and 75 kg per sq cm over the temperature range of 620° to 1032°C. Minimum creep rates were used from both test methods; this was considered proper because comparable temperature tests or cycling to the same temperature gave the same creep rate, within experimental error. The cold vacuum test chamber, with the unstressed specimen in place, was heated to temperature by placing a preheated furnace over the chamber. Temperature equilibrium was attained within 30 min. For the cyclic tests, the stress was removed during the 5 to 10 min necessary to effect the temperature change and re-

Jan 1, 1965

By Arnold B. Hubbard

Automatic control instruments were utilized by the Bureau of Mines for routine assays of large numbers of oil shale samples and other bituminous materials. The standard Fischer assay method was automated by automatically controlling the heating cycles of a battery of 12 electric heaters with electronic controllers and programmers. The condensers were cooled with a modified automatically controlled refrigeration bath. The complete assembly consisted of 12 retort units, necessary control instruments, and the refrigeration bath. This equipment was capable of producing more consistent results than those previously obtained with the gas-heated retorts and of increasing the output of assays substantially with no increase in operating personnel.

Jan 1, 1965

By C. H. Schack

Extractive metallurgy techniques currently employed to recover silver from primary ores and secondary scrap were reviewed and evaluated to identify and delineate metallurgical problems whose resolution would increase the supply of silver from domestic materials. The survey revealed that practically all primary silver is recovered by froth flotation concentration of various types of ores, followed by smelting and refining of the separate lead, copper, and zinc concentrates. Silver losses during the complex processing are, with rare exception, inconsequential. Furthermore, any silver production gain from base metal ores, which contribute about two-thirds of the total primary silver, is directly dependent no improvement in the market for the base metals. Statistical data on new and old silver scrap are wholly inadequate to make reliable conclusions about scrap processing problems and the possibility of increasing the recovery of silver from the many forms of secondary silver-bearing materials. The available information indicates (1) that efficient silver reclamation practices are employed by the larger users of silver, and (2) that recovery of additional secondary silver involves solution of problems of collection rather than of processing. Several possibilities exist for limited increases in silver production from primary ores by improvement in metallurgical practices. Specifically, research is needed to (1) solve the problem of recovering silver from the copper ores of the Copper Range district, Michigan; and (2) devise economically feasible methods for recovery of silver from presently marginal or submarginal ores char because of grade, location, and frequently complex nature cannot presently be exploited by conventional techniques.

Jan 1, 1965

By G. L. Gates

The Bureau of Mines studied the scales formed in producing wells in the Wilmington field, California. The scales were primarily barium sulfate and resulted from the mixing of injected sea water and formation waters; there was excess sulfate in the injection water and the formation waters contained appreciable barium. After breakthrough, the produced brines were supersaturated with barium sulfate. Laboratory tests indicated that barium sulfate precipitated quickly When the supersaturated brines were agitated with crystals of barium sulfate and fairly rapidly when more sulfate solution was added. Precipitation occurred slowly on standing or under nonturbulent conditions. Both the apparent and equilibrium solubilities of barium sulfate in these brines were determined and compared with equilibrium solubilities in distilled water and sodium chloride solutions.

Jan 1, 1965

By H. J. Ramey

Conventional calculation of total system isothermal compressibility for a system containing a free gas phase involves, among other things, evaluation of the change of oil and gas formation volume factors and the gas in solution with pressure. Preferably, this information should be obtained from laboratory measurements made with particular oils and gases. Often, experimental measurements are not available. In this case, it is necessary to obtain pressure-volume-temperature relationships from general correlations such as those of Standing&apos; for California oils. In order to speed estimates of compressibility, generalized plots have been prepared of the change of both oil formation volume factors and gas in solution, with pressure from Standing&apos;s correlations. A generalized plot for estimating the change in the two-phase (oil and gas) formation volume factor with pressure is also presented. Usually, the effect of gas dissolved in reservoir water upon the total system compressibility is neglected for gas saturated systems, due to the low solubility of gas in water. Results of this study indicate that the increase in total system compressibility caused by solution of gas in water is often as large as the compressibility of wafer, and can be magnitudes larger for low pressure systems. Generalized results for estimating the change of gas in solution in water with pressure are presented in tabular and graphical form. INTRODUCTION During the past decade, pressure build-up and drawdown techniques have gained an important place in reservoir engineering. Build-up and drawdown analyses are only two special applications of the broad field of transient fluid-flow theory. All solutions of transient fluid-flow problems contain a parameter called the total system isothermal compressibility. This property of fluids and porous rock is a measure of the change in volume of the fluid content of porous rock with a change in pressure, and it may vary considerably with pressure. Evaluation of total system isothermal compressibility is not difficult, but it is tedious and time-consuming. Often compressibilities are estimated roughly, or transient flow methods are neglected completely. The benefits of using accurate system compressibility in properly-executed build-up or drawdown analyses are: 1. Better planning of pressure build-ups may be achieved to avoid unnecessary loss of revenue due to excessively long shut-in periods, or to shut-in periods too short to yield useable data. 2. Better and more reliable estimates of static formation pressures for reserves estimates and rate performance estimates. 3. Reliable information for evaluation of well completion effectiveness, and planning and interpretation of well stimulation efforts. The purpose of this paper is to clarify the nature of the total system isothermal compressibility, and to present useful methods for estimation of compressibility, particularly for systems containing a gas phase. DEVELOPMENT Numerous publications have presented solutions to transient single-phase flow of slightly compressible fluids, stressing pressure build-up applications. In transient flow, a compressibility* term arises to permit volume content of fluids in porous rock to change as pressure changes. The basic nature of the compressibility term is usually taken for granted. Problems arise in practical applications of transient fluid theory because most published works consider only one flowing fluid—in an ideal porous system containing only one fluid. In 1956, Perrine2 presented an intuitive extension of single-phase flow pressure build-up methods to multiphase flow conditions. Later, Martin- established conditions under which Perrine&apos;s multiphase build-up method had a theoretical foundation. Perrine has shown that improper use of single-phase build-up analysis in certain multiphase flow situations can lead to gross errors in estimated static formation pressure, permeability and well condition. It is likely that, much pressure build-up data for oil wells should be analyzed on the basis of multiphase flow. For both single-phase and multiphase build-up analysis, the isothermal compressibility term in dimensionless time groups often should be interpreted as the total system compressibility. All real reservoirs contain one or more compressible fluid phases. In addition, rock compressibility can contribute in an important way to the total system compressibility. The proper total system compressibility expression may contain terms for compressibility of oil, gas, water, reservoir rock and terms for the change of solubility of gas in liquid phases.

Jan 1, 1965

By Arnold M. Lansche

DOMESTIC OUTPUT of white arsenic, As2O3, was derived entirely as a byproduct of smelting arsenic-containing copper ores by The Anaconda Company at Anaconda, Mont., and American Smelting and Refining Company at Tacoma, Wash. Arsenic metal was not produced. Consumption, and Uses.-Most of the white arsenic produced in 1964 was consumed in manufacturing lead and calcium arsenate insecticides. In the 12 year period since 1951 the production of lead arsenate insecticide has varied between 7,800 tons and 4,900 tons, indicating that lead arsenate has maintained its position in competition with organic insecticides.

Jan 1, 1965

By K. G. Davis, P. Fryzuk

A study has been made of the effect of undercooling on the grain structure and solute distribution in small ingots of pure bismuth and of a 100 ppm Ag in bismuth alloy. Autoradiographic evidence shows that in undercooled melts a network of dendrites is formed throughout the melt immediately after nu-cleation. At large undercoolings the dendrites are very thin and closely spaced. The origin of the observed grain morphology can be explained on the basis of information about the mode of solidification revealed by the impurity substructure. WHILE a great number of studies of nucleation in undercooled molten metals have been made, comparatively little attention has been given to the mode of solidification from melts with large undercool- ings. Colligan and Bayles1 and Walker2 have measured the rate of advance of the solid-liquid interface in undercooled nickel melts, but the morphology of the solidifying material remained a matter of speculation. Fehling and Scheil3 have described the grain structure in ingots formed from undercooled melts of nickel, palladium, and copper, and a series of Ni-Cu and Ni-Pd alloys. At small undercoolings, equiaxed structures are observed, the grain diameter tending to increase as the temperature of nucleation is lowered. At greater undercoolings, a columnar structure is developed, while with still further undercooling there is a smaller grain size incorporating rather coarse subgrains. All-bright and Colligan4 examined the grain structure shown by ingots solidified from melts of nickel and of Ni-Ag alloy at an undercooling of 105°C, and concluded that considerable grain growth had taken place after solidification. The object of the present work is to correlate the mode of solidification from undercooled melts with both the grain structure and impurity segregation, using tracers to examine the latter.

Jan 1, 1965

By J. P. Hansen

Wustite beds were reduced with carbon monoxide and mixtures of hydrogen and nitrogen in the temperature range 900° to 1,300° C to determine the effect of temperature, gas flow, and surface area on the rate of reduction to iron. The composition of the gas stream as it passed through the wustite bed was continuously measured with infrared absorption cells and heated-wire methods. The change in composition was used to calculate the reaction rates. Arrhenius plots of the data give heats of activation of 34 kcal for particles using CO, 27 kcal for particles using H2, 24 kcal for pellets using C8, and 6 kcal for pellets using H2. The velocity of reduction is dependent on the area of reacting interface and the driving potential of the gas (reducing gas concentration minus equilibrium concentration) as well as the exponential temperature effect. The reaction rate was independent of the gas velocity over the range of conditions studied.

Jan 1, 1965

By Barry Hunsaker

I cannot help but be reminded, as I stand here today, of my boyhood years and heritage, both of which are inextricably tied to this very valley and are, in a: bay, apropos of the theme of this Keynote Session. I remember the scarcity of people. For example, 48, 000 in Phoenix and 436, 000 in the State in 1930 and 65,000 in Phoenix and 499, 000 in the State in 1940. Today Phoenix boasts a population of over 500, 000 and the State a population of 1, 500,000. I remember the&apos; lack of facilities, goods and services, including gas and electric power. I recall stories of my grandfather who had the freighting or teaming contract to haul all the supplies and generating equipment, by wagon mind you, up the old Apache Trail to Roosevelt Dam. . .a three day trip from the nearest railhead which, by the way, was not Phoenix, for it did not merit a railhead on those days, but the village of Maricopa approximately 25 miles south of Phoenix. I remember chopping firewood, heating wash water on an open fire in a No. 3 wash tub at the rear of the house and doing my school homework by the light of a kerosene lamp just 25 to 35 years ago within what is now a large metropolitan area

Jan 1, 1965

By H. H. Podgurski, Hsun Hu

Large cryslals of high-purily iron (99.996+ pcl) cannot be obtained by the usual strain-ameal technique. Repealed phase transformation by thermal cycling prior to crilical deformation improves the capabilily of cryslal growith but fails to yield satisfactory crystals. Imperfect columnar crystals can be produced by the phase-transition method. The addition of a small amounl (0.005 wl pet) of nilrogen IT was reported&apos;-4 that for metals of very high purity the usual procedures of the strain-anneal technique fail to produce large crystals. This was eliminates practically all the difficulties in crystal growth by the normal strain-anneal procedures. An actual example is presented, showing that most parts of a strip have been converted into a large crystal by this method. The addition of nitrogen, which can be removed from iron with less difficulty, is believed to be more desirable than carbon additions for the same purpose. thought to be due to the strong tendency for recovery in the high-purity metals: hence the critically strained matrix undergoes polygonization instead of recrystallization upon annealing for crystal growth. Talbot1,2 succeeded in overcoming this difficulty by adding 0.03 to 0.04 pct C to high-purity iron before critical deformation. followed by annealing in hydro-

Jan 1, 1965

By Richard D. Miller

This publication contains routine analyses and related source data for 295 natural gas samples from 18 States collected during calendar year 1963 as part of a continuous survey of the United States for occurrences of helium in natural gas. This survey has been conducted by the Bureau of Mines since 1917. The analyses published herein were made by mass spectrometer and a special helium analysis apparatus, which are described in Bureau of Mines Bulletins 4863/ and 576.4/

Jan 1, 1965

By R. L. Grunes, F. K. Kies, C. D&apos, Antonio

THE several studies concerned with the annealing of thin nickel films have largely been restricted to films of a single thickness.1-4 It is well-known, however, that both physical and mechanical properties depend upon film thickness.5, 6 The strength-thickness relations found in vapor-deposited nickel films in the annealed and as-deposited states, as an example, are at least partially due to the density and arrangement of imperfections within the films.7, 8 For these reasons, the annealing characteristics of thin nickel films as a function of thickness were investigated. Electrical resistance was chosen to monitor annealing behavior since resistance changes are partially dependent upon defect structure. In addition, the equations predicting film resistivity as a function of thickness are already available.9, 10 Further advantages afforded by electrical-resistance measurements are its adaption to continuous readings during annealing and its relative simplicity. Nickel films were vapor-deposited, at average rates of 60Å per sec, on Vycor substrates held at room temperature in vacuums of about 10-5 torr. Afterwards, deposition-thickness measurements were made using a multiple-beam interferometric technique. A more detailed description of deposition procedures and the interferometer appear elsewhere.7, 8 The four-probe method was employed in measuring electrical resistance since this technique measures film resistance without contributions from lead wires and contacts. Resistance measurements were made before, during, and after annealing to temperatures of 700°C under vacuums of approximately 10-4 torr. Measurements were made every 25°C or more often when necessitated by unusual resistance changes. Cooling and heating rates were maintained at approximately 5°C per min. Typical resistivity vs temperature curves are shown in Figs. 1 through 4. It is apparent from these

Jan 1, 1965

By M. C. Lavine, H. C. Gatos, R. S. Mroczkowski

The structure of GaAs-Ge heterojunctions prepared by a back-melting process was studied by X-rav diffraction, melallographic, and electron-micro-analyzer techniques. The boundary region between the GaAs and the germanium was found to consist of a four-layered band. A discontinuity between the two inner bands was brought about by solidification occurring simultaneously from the GaAs and the germanium side. The junction material OH either side of the central discotinuity was found to have grown as a single Crystal with the orientation of the parent substrate. It was found essential to determine the GaAs-Ge phase diagram. This was accomplished by a series of alloys containing 0 to 40 wt pet GaAs. Over this range the diagram is a simple eutectic with the eutectic point at 74 wt pet Ge and 845 C. The limiting- solubility of Coils in germanium was found to bc less than 5 wt pet. The Kossel divergent-beam X-ray technique was used to study orientation relationships across the boundary lager. A great deal of effort has been recently expended on the electrical properties of heterojunctions. Little attention, however, has been given to the metallurgical variables which may be of importance in the formation of the junctions. The present work was undertaken to investigate some of the more pertinent metallurgical aspects of interface-alloyed GaAs-Ge heterojunctions. Such parameters as solidification processes, composition gradients, orientation effects, and the accommodation of crystal structures have been the objects of study in this program. EXPERIMENTAL PROCEDURES Phase Diagram. The phase diagram of the GaAs-Ge pseudobinary system was determined by means of cooling curves. A Bridgeman furnace was employed with the center section maintained at 1200°C and the upper section at 800°C. Melts varying from 0 to 40 at. pct in GaAs content were used. Each charge was incapsulated under a two-thirds atmosphere of argon in a carbon-coated quartz tube. Five min in the furnace hot zone provided rapid melting and homogenization. The capsule was then removed to the cooler portion of the furnace. Cooling times were of the order of 3 min. The resulting homogeneous microstructure indicated that equilibrium conditions were obtained by this procedure. Formation of Heterojunctions. Rectangular parallelepiped single-crystal samples were cut with the large faces of either the (l00), (110), or (111) orientation. The remaining four surfaces were also cut to specific orientations to permit accurate relative orientation of the GaAs-Ge pairs. The

Jan 1, 1965

The principal activities of the Bureau of Mines Explosives Research Center from July 1, 1962, to June 30, 1963, are described briefly in part 1. Part 2 gives short abstracts of publications that appeared during fiscal year 1963; in general, the research reported in these publications antedates the report period.

Jan 1, 1965

By Mulligan John J.

The Bureau of Mines investigated lode tin deposits on Potato Mountain, Seward Peninsula, Alaska. Tin was found to occur as cassiterite associated with quartz, tourmaline, pyrite, arsenopyrite, and earthy clays, but the deposits lack the varied accessory minerals commonly found in tin districts. The tin-bearing deposits are in metasediments along minor breaks and bedding planes but not in the crushed earthy filling of major faults. Cassiterite and sulfides occur with quartz in veins, both with and without earthy clays, and disseminated through tourmalinized wall rocks. The deposits are characterized by irregular segregations containing 1 to 10 percent tin within zones averaging not over 0.25 percent tin. The largest segregation exposed is on the summit of a low hill on the east-central slopes of Little Potato Mountain; most of the outcroppings are in an area trending east to west, roughly 10 to 30 feet wide and 300 feet long. Sample values ranged as high as 12 percent tin, but the average grade may be about 1 percent tin. The extreme irregularity of both grade and composition precludes a more exact determination. Similar concentrations are scattered for over 1,000 feet to the west and north, but these are smaller and lower in grade. Elsewhere on Potato Mountain, generally similar deposits occur as clusters of veinlets at widely separated points in the metasedimentary walls of major faults.

Jan 1, 1965

Of the twelve known ore zones on the Sunro property, acquired by Cowichan Copper Co., only the "B" and "C" orebodies of the "River Zone" had been explored sufficiently to indicate the grade and tonnage. The "B" zone was selected for initial production. The portion of this orebody above the main adit level was developed for horizontal-ring, longhole mining. Ore from the stope would be scraped directly to the coarse ore bin. The lack of a suitable mill site on surface, as well as the 8,000-ft. tramming distance, led naturally to the installation ground. I N November, 1960, a lease was obtained by Co-wichan Copper Co. Ltd. (N.P.L.) from Sunro Mines Ltd., covering the main ore (River) zone of the Sunro property. A total of twelve zones had been located on the property. Nine of these lay within the leased area. With the exception of the "B" and "C" orebodies of the River Zone, there had been insufficient exploration for tonnage and grade calculations. Exploration by previous companies had

Jan 1, 1965

By Frank E. Woolley, Robert D. Pehlke

Jan 1, 1965