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By K. H. G. Ashbee, J. W. Heavens

One consequence of the distribution in orientation of Bragg diffracting planes in an elastically bent foil is that simultaneous diffraction occurs from ±g pairs, where g is the reciprocal lattice vector to a diffracting plane. If such Bragg contour pairs are indexed, then the variation in orientation with respect to the incident electron beam is known. This note describes a construction by means of which Bragg contour pairs may be indexed by inspection. Referring to Fig. 1, the Ewald sphere radius is l/h, where is the wavelength of the electron beam, and the half spacing of first-order reciprocal lattice planes is l/d, where d is the corresponding spacing in direct space. The angle subtended by the zero and first-order planes at the center of the Ewald sphere is a = sin-' Thus, to represent a pair of first-order Bragg contours on a stereographic projection, measure ±a from, and along the normal to, the zero-order plane. The traces of the required Bragg contours pass through these points and parallel to the zero-order trace. In practice, it is desirable to enlarge a stereographic projection of the zero-order planes before making the construction. As an example, a stereographic projection of first-order Bragg contours up to line 27 for an fcc crystal is given in Fig. 2; if required, higher-order contours can easily be added. Fig. 2 is, of course, a map of first-order Brillouin zone boundaries. One use of this construction is the measurement of large elastic fields in electron microscope specimens. Fig. 3(a) shows a pattern of Bragg contour pairs due to lattice distortions near a large precipitate. This particular example is of a T-phase precipitate in Hidu-minium 54 (A1 + 6 wt pct Cu, 0.5 wt pct Mn). Foil buckling is produced by annealing during observation and may be evidence for evaporation from the precipitate.' Comparing Figs. 2 and 3(0), it is evident that the axis of high symmetry in Fig. 3(a) is [lll]. The strain in a bent foil is approxinlately t/2r, where / is the foil thickness and ? the radius to which the foil is bent. From the projections of grain boundaries and of helical dislocations, it was estimated that ( - 3000A, and values for ? were obtained from the

Jan 1, 1968

By ARTHUR S. DWIGH

Discussion of the paper of W. W. NORTON, presented at the Salt Lake meeting, August, 1914, and printed in Bulletin No. 92, August., 1914, pp. 1993 to 1999. ARTHUR S. DWIGHT, New York, N. Y.-Mr. Norton's chief argument is directed against the idea that the D. & L. sinter is any better material for the blast furnace than the H. & H. product. He supports this by citing two experimental furnace runs. Reducibility.-To discuss a furnace record like that quoted by Mr. Norton for the five days' run in August, 1912, is manifestly difficult for an outsider, but a possible explanation for the poor reduction on Furnace No. 5, smelting D. & L. sinter, may lie in the fact that both sets of furnaces carried the same fuel charges. Other things being equal, if 11 ½ per cent. coke was right for the furnaces smelting H. & H. product, it Was too much for the furnace smelting D. & L. product, as I shall endeavor to show later, and incipient overfire, accompanied by higher leads in slag and matte, was induced. It may sound like a paradox to say that excessive fuel sometimes produces poor reduction, but it is a sad fact. In certain plants where practically the entire charge to the blast furnaces receives a preliminary treatment by being sintered on the D. & L. machines the peculiarities of this problem have had to be very carefully studied, for serious metallurgical difficulties presented themselves when the change was first made to D. & L. sinter in large quantities. Some of these plants had blast pots before they had D. & L. machines, and many opportunities were afforded for comparative study of this very point. There is reason to believe that, clue to the long period of blowing and the higher temperatures developed in the pots from greater mass action, the iron in the H. & H. product is present chiefly as Fe203, perhaps in the form of ferrites, while in the D. & L. product the iron is present as FeO. The fuel charge in the blast furnace must be so proportioned as to exactly meet the chemical and thermic requirements of reduction and melting. If ally of these functions have been performed before the material enters the furnace, a corresponding allowance should be made or the fuel balance will be disturbed and bad work will result. One of the functions of the coke is to reduce enough metallic Fe for the matte requirements, leaving the remainder of the iron as FeO to go into the slag. In smelting almost any other material than D. & L. sinter the iron must-be reduced from the higher oxides, Fe203 or Fe304, to the protoxide, FeO, before a true comparative basis is reached. Experience has shown that with about one-half D. & L. sinter on the charge the coke should-be cut about 10 per cent. This theoretical benefit is borne out by the practical blast-furnace results on a large scale in numerous plants. In fact, wherever this very important factor is ignored the evil symptoms of excessive fuel will be indicated,

Jan 11, 1914

By J. K. Edgar

For a number of years the production and use of super-purity aluminum (better than 99.99 pct) has been steadily increasing. High-grade lots of. such aluminum show certain outstanding characteristics not found in lower grades containing principally silicon, iron and copper as impurities. One such characteristic is the so-called "self annealing," that is, the re-crystallization of the heavily cold worked metal at room temperature.' Interest therefore is aroused as to the effects of the impurities. It is well known that the amounts of silicon and copper which occur in aluminum of better than 99.95 pct are completely soluble, at least at elevated temperatures (above 200°C). Iron, on the other hand, is known to be fairly insoluble in solid aluminum. Thus, a knowledge of the limits of this solubility would he of considerable use in studying the characteristics of the high purity metal. All investigators have agreed that iron has very low solubility in solid aluminum. Rosenhain, Archbutt and Hanson2 reported traces of an aluminum-iron phase in the "purest samples of aluminum obtainable." Gwyer and Phillips3 reported that an iron constituent was visible under the microscope in metal containing ".0088 per cent iron." Roth4 found that in the solid state the solubility of iron in high purity aluminum was 0.01, 0.01, 0.017 and 0.022 pct at 225, 320, 500 and 600°C respectively. Dix5 working with alloys containing less than 0.03 pct impurities, concluded from microscopic and chemical analyses of eutectic areas that the eutectic composition was close to 1.7 pct iron. Dix placed the eutectic temperature at 65s°C. Archer and Fink,6 using high purity aluminum-iron alloys, found that the hypoeutectic liquidus intersects the eutec-tic horizontal at 1.7 pct. This is in fair agreement with the investigation of the aluminum-iron system by Gwyer and Phillips who placed the eutectic at 1.89 pct iron with a freezing point of 653'C. Preparation and Chemical Analysis oP Alloys Electrolytically refined aluminum (99.991 pct aluminum) and a high purity alumi-num-iron alloy (11.45 Pet iron) were used in the preparation of the alloys for this investigation. To aid in controlling the iron content of the experimental alloys, an alloy of lower iron content was prepared first from these materials. The high purity aluminum was melted and heated to about 700°C in a plumbago crucible coated with alundum cement and the aluminum-iron alloy was then added. The alloy was thoroughly stirred, fluxed and skimmed and then chill-cast into notch bars. The aIlalyses of the three materials are given in Table I. The alloys for the determination of the solid solubility of iron in aluminum were prepared by melting 600 g total of the aluminum plus the required quantity of the aluminum-iron alloy (No. 92531). These

Jan 1, 1949

By Billy L. Crowder, John M. Fairfield

The implantation of B+ , P+, and As&apos; into silicon has been studied with the purpose of making shallow p-n junctions. The influence of such parameters as 1) ion energy, 2) target orientation and temperature, 3) total dose, and 4) annealing schedule was investigated. An energy range of 70 to 300 kev was used for boron and phosphorus implants and up to 500 kev for arsenic. It is found that the experimental projected range agrees well with theory and that shallow junction depths can be made reproducibly. ION implantation has received much attention recently as a technique for doping semiconductors. Specifically, it has the potential of supplementing or replacing the diffusion process as a method for making p-n junctions. In a few specific cases it has been used successfully to make semiconductor junction devices. Potential advantages of ion implantation doping over diffusion techniques are: 1) It affords greater control of shallow junction depths (< 0.2 µ) while maintaining high peak concentrations. This is particularly important for high-speed switching devices, since lower junction capacitances and resistances can be achieved. 2) More precise registration of small planar structures can be realized if proper masking procedures are employed. This advantage is especially useful in the design of high-density integrated circuits. It has been used to advantage in FET fabrication since the edge of the source or drain can be aligned precisely at the edge of the gate electrode.&apos; 3) Ion implanatation permits lower temperatures than diffusion techniques. This factor alleviates the problem of compatibility of diffusivities often encountered when designing multiple-junction structures. Also, the lower temperatures create fewer thermal defects and dislocations, which may account for the high efficiency of some ion-implanted solar cells.2 4) Impurity profiles can be more easily tailored to resemble ideal distributions. Successful exploitation of the potential advantages of ion implantation techniques will depend on increased knowledge and understanding of the subject. The factors likely to be influential in determining impurity distribution profiles in ion-implanted single-crystal targets have been reviewed by J. F. Gibbons.3 In addition to the mass and energy of the implanted ion, the total dose, target orientation, and target temperature are important parameters. The annealing temperature required for removing lattice damage and incorporating the implanted species on an electrically active site is very important. This paper describes an investigation of some of these factors. Implants of boron, phosphorus, and arsenic into silicon have been studied. Energy ranges of 50 to 300 kev were used for boron and phosphorus and up to 500 kev for arsenic. In addition to the implantation energy, the effects of total dose, target temperature, and post implant anneal have been investigated. EXPERIMENTAL PROCEDURE The implantation targets were silicon wafers cut from Czochralski-grown crystals, lapped, and chemically polished. The orientations were (111), (110). and (100) with misorientations of up to 7 deg from the principal axis. For this study, accurate target alignment (i.e., within 0.1 deg) was not available and quoted misorientation values should be regarded as approximate . The implantation equipment consisted of an ion source, a 300-kev linear accelerator tube, an electromagnetic separator, and the associated target supporting and beam focusing assemblies. The ion source was a simple oscillating electron type source,4 which has been described elsewhere.5 The gaseous compounds BF3, PF5, and AsH3 were used as ion sources for B+, P+, As+, and AS+&apos;. Analyzed current levels of up to 20 pamp could be obtained; however, for this investigation target current levels of 1-3 µ amp were usually employed. The analyzed ion beam was collimated through a double slit (1.4 x 0.4 cm) and swept perpendicularly to the long axis of the slit such that an area of about 2 sq cm on each target was covered. Dosages of around 1015 cm-2 were normally employed, but smaller amounts were also used for comparison. A uniform flux density over the bombarded area was assured by the continuous use of profile monitors similar to those described by Wegner and Feigenbaum.6 Post-implant annealing was accomplished in an argon atmosphere in a temperature range of 600" to 950°C. It was not part of the purpose of this investigation to study the annealing kinetics; however, some isochronal and isothermal anneal experiments were conducted to determine the time and temperature necessary to render a reasonably high portion of the implanted ions electrically active (i.e., higher than 50 pct). Post-implant anneal temperatures of around 900° and 600°C were required for boron, and arsenic and phosphorus implants, respectively. Arsenic and phosphorus implants increased in conductivity rather abruptly at the proper anneal temperature of the isochronal curve, but boron increased more gradually over a wider range. Isothermal anneal curves were reasonably flat after 10 min, so an anneal time of 1/2 hr was used for the experimental results described below. The profiling techniques were: 1) neutron activation analysis, 2) differential sheet resistance,7 and 3) junction staining.8 The differential sheet resistance technique is commonly employed in this type of study. Its principal disadvantage is the uncertainty of the ef-

Jan 1, 1970

By Dorsey Hager

DORSEY HAGER, Tulsa, Okla.-I have been asked why the Dexter region is dry. I would like to know myself. I drilled two dry wells on that same anticline which has production to, the east and west and south and north. That same anticline has seven domes that have been drilled and only three have proven productive out of the seven. In other words, you have one well-defined anticline with seven domes along its length, all mappable, all checked carefully, and only three of those seven have produced. Now why the others did not produce, I do not know. L. L. HUTCHISON, Tulsa, Okla.-There is no appreciable difference in the character or structure of the sands? DORSEY HAGER.-NO, I have never .been able to see any appreciable difference in the sands where we got production and Where we did not get it. I will say that the deepest wells we drilled, in the vicinity of Dexter, had no sands at the point where they got the production farther north. I. N. -KNAPP, Ardmore, Pa.-I first went to the Kansas-Oklahoma field in 1895 and occasionally thereafter until 1899, when I began drilling; for oil. I started close to wells that were producing gas and which, when drilling, lead made good oil showings in a sand above the gas. I thought these showings were good enough evidence of an oil pool for me without looking for any anticline and I made a paying development in what&apos; I was afterward told by geologists was probably a synclinal trough. If I remember correctly Dr. Orton&apos;s report on the lola gas pool (about 1898) he distinctly said that he found no evidence of anticlinal structure and concluded from the records of a large number of wells that there, was a terraced structure of the productive gas sands, of which there were no surface indications.

Jan 4, 1917

By G. B. Misra

While investigating on the aerodynamic resistance of airways supported with peripheral timber sets, at regular intervals, the following theoretical equations were developed by the author to estimate the resistance coefficient of such airways: [ ] for S < 1, where f is Darcy-Weisbach resistance coefficient of the airway, C is modified drag coefficient of the supporting member, D is equivalent diameter of the bare airway, 8 is ratio of the approach velocity over the sets to the average velocity of the bare airway, A is cross-sectional area of the bare airway, a is projected frontal area of the sets, A., is cross-sectional area of the air stream at the vena contracta inside the set, S is spacing of the sets, f, is resistance coefficient of the bare airway, l is length of aerodynamic influence of sets, p is perimeter of the bare airway, p, is setted portion of the perimeter of the bare airway, pe is unsetted portion of the perimeter of the bare airway, and P shielding factor. The equations were verified experimentally in a model rectangular airway supported with one- (bars), three-, and four-piece sets of square-section timber of three different sizes and were found to hold true. The work has been further extended to one-, three-, and four-piece sets of round timber of 2.6, 3.2, and 3.8 cm diam with the same experimental set up. Tests have been carried out for spacings of 25, 50, 75, 100, 150, and 200 cm over a regime of flow defined by the Reynolds number (with respect to the equivalent diameter of the bare duct) ranging from about 1.5 X 106 to 5 X 106 using the same experimental techniques. The values of f are calculated in the manner indicated in [Ref. 1]. Unlike with square-section timber, the resistance coefficient f of the airway setted with round timber shows a distinct variation with the Reynolds number of flow. This conforms to observations made by Sales and Hinsley.2 In order to have a comparable value of f for all types of sets with all sizes of timber, it was necessary to select the value of f at a fixed Reynolds number of flow. Since f is chiefly a function of the drag coefficient of the sets, the appropriate Reynolds number RE is that with respect to the diameter of timber in the set. Considering the diameters of timber used and the regime of flow over which measurements were made, f was chosen at a value of RE = 20,000 in all cases. The f vs. S curves are maximal in nature and in conformity with theory, the f vs. 1/S curves are straight lines up to a value of S = 1 beyond which they show a distinct flexure. The observed values of 1, the length of aerodynamic influence of sets, agree with the relation 1 = 42 e, developed for square-section timber sets, thus suggesting that the shape of timber has little influence on the length of aerodynamic influence. The value of the modified drag coefficient CD for round timber was calculated in the same way as for square timber in Ref. 1, taking the contraction factor Z = 1.5 for round-edged constrictions. CD has an average value of 0.96 with a standard deviation of 6.08% as compared to the free stream drag coefficient of 1.2 at RE = 20,000 for long cylindrical obstructions The shielding factor [ ] is plotted against S/1 in [Fig. 1]. The curves are more or less independent of the size of timber, but are different for the different types of sets, possibly due to their different degree of symmetry. Values of f calculated by the author&apos;s [Eqs. 1 and 2], using experimental values of CD&apos; and [ ] and taking I = 42 e, are plotted in [Fig. 2] against experimentally measured values of f for different types of sets with different sizes of round timber. The values agree closely with a standard deviation of only 5%, thus establishing the veracity of the theoretical equations developed by the author for round timber as well. A comparison was made between the Xenofontowa4 equations (the only other reasonable relations available for the estimation of the resistance coefficient of supported airways) and the author&apos;s [Eqs. 1 and 2] by comparing in [Fig. 3] the values of the resistance coefficient f computed by the Xenofontowa relations with those experimentally measured by the author. In order to make

Jan 1, 1975

By Hsun Hu, B. B. Ruth

The rates of migration of high-angle boundaries in zone-refined aluminum crystals rolled 20 to 70 pct in the (110)[i12/ orientation were studied. Following a recovery anneal at an appropriate temperature to stabilize the polygonized structure, boundary migration rates of artificially nucleated grains were measwed isothermally at several temperatures. Results indicate that the rate of boundary migration depends strongly on the amount of deformation and on the cell size of the polygonized matrix, and is related to the driving free energy by a power function. The degree of anisotropy in growth 0.f the re crystallized grains nn&apos;th preferred mientation is independent of deformation; the migration rates of the fast-moving and the slow-moping boundary segments of a gowing grain differ by as much as one order of magnitude. The actir\ation energy fm a grain boundary migration, although nearly the same for both the fast-moving and the slow-moving boundaries for a given deformalion, decreases from 45 to 30 kcal per mole with an increase in deformation from 20 to 70 pct reduction. Re crstallization by the growth of the artificially nucleated grains results in preferred orientation. The Percentuge of&apos; grains favorably oriented for growth increases with increasing deformation. None of these grains corresponds to the ideal Kronberg-Wilson orientation relationship. The observed growth aniso-tropy is discussed in terms of boundary structure. The boundary velocity as a function of the cell inter -facial area, or the driving free energy, is discussed in the light of current theories of boundary migration. It is well established that recrystallization with re-orientation occurs by the migration of high-angle boundaries of strain-free grains. The driving force for this process is provided by the free energy stored in the metal during deformation. A quantitative study of the effect of varying driving force on grain boundary migration in deformed metals has not been possible heretofore, primarily because of: 1) concurrent recovery steadily decreasing the available driving free energy for boundary migration, &apos;-3 and 2) in-homogeneity of strain in the deformed metal.4 Aust and Rutter3 studied grain boundary migration in striated single crystals of zone-refined lead. Although the driving free energy in such crystals remains unaltered during annealing, this method does not provide a range of driving free energies over which measurements of grain boundary migration can be made. In the present investigation, the rates of migration of high-angle boundaries in deformed aluminum zone- refined single crystals were studied at various temperatures, after deformation ranging from 20 to 70 pct reduction by rolling at -78°C in the (ll0)[i12] orientation. The boundary migration rates along different crystallographic directions were determined under steady-state conditions, i.e., in the absence of competing recovery processes or impingement of recrystallized grains growing into the deformed single crystal matrix. Simultaneous recovery was eliminated by suitable anneals prior to the boundary migration measurements. The recrystallized grains, which grew a ni so tropically into the homogeneously polygonized matrix, developed flat boundary segments during early stages of growth. These boundary segments subsequently migrated along a direction approximately normal to the boundary plane into the matrix rystal. Increasing deformation over the range employed was estimated to increase the driving free energy for boundary migration by about five times. The kinetics of the boundary migration process, examined under these conditions, indicate that the boundary velocity is greatly affected by a small change of the driving free energy in the matrix crystals. These results were examined in the light of the current theories of grain boundary migration. EXPERIMENTAL PROCEDURES Single crystal strips (9 by 1 by 0.125 in.) of zone-refined aluminum, were seed-grown by the Bridgman method in a high-purity graphite mold (<lo ppm ash) at 1 in. per hr. Precautions were taken to minimize contamination of the metal during crystal preparation and subsequent handling. Spectrographic analysis of the metallic impurities in the grown crystals is Qven in Table I. The crystals were rolled in the (110)[112] orientation at -78°C to various reductions in thickness, ranging from 20 to 70 pct, in 10 pct increments. The desired reduction was achieved by many rolling passes, each being no more than 0.002 in. To minimize surface friction, the crystal was rolled between two thin layers of teflon. For those crystals rolled more than 40 pct, it was necessary to remove the disturbed surface layers by electropolishing at -5" to -10°C at an intermediate stage of rolling. The edges of deformed crystals were removed by a jeweler&apos;s saw while submerged in alcohol at -78° C to obtain samples of about ? by i in. The distorted metal at the cut edges and the surface layers were then removed by electropolishing, with removal of a minimum of 0.004 in. from each surface. The thickness of the crystals prior to rolling was chosen so that the final thickness was 0.025 in. for all samples. These deformed single crystals were each prean-nealed for 1 hr at an appropriate temperature in the range of 130" to 280°C, depending upon the amount of deformation. The purpose of this preannealing was to

Jan 1, 1970

One of our members, in Colombia, has written the following interesting account of his experience in trying to remit his dues to the Institute. "Last year I was away at the end of the year and on my return I was unable to obtain a draft in Honda until April, I believe. To avoid delay this year I remitted cash, early in January, to a friend in Bogota who I imagined could sell or procure for me various small drafts to cover my annual subscriptions. After many weeks&apos; delay, I was informed that he could not get them for me and was remitting the cash to Honda where they were obtainable. After another long delay, I was informed that no one in Honda would sell drafts or checks for small amounts. Eventually I found a friend who was willing to oblige me in the matter and at once forwarded the amount."

Jan 8, 1919

By Thomas C. Wilder, Walter E. Galin

Measurements of the electromotive force of the cell at 995°C have shown that the cell may be used to detennine the zinc content of molten Cu-Zn alloys to the nearest 0.05 wt pct. The cell is used for brass melts to which no ZnO is added intentionally, because essentially all oxygen in the Cu-Zn-O system is present in the form of ZnO. The cell is also used to detev,nine the thernodynamic activity of zinc for Cu-Zn al1oys of the brass composition range, from which the equilibrium partial pressure of zinc for such alloy may also be calculated. The electrochemical measurement of the concentration of the most active metal in other engneering- alloy systems by a similar technique is also considered. IN recent years there have been many studies concerning the direct electrochemical measurement of oxygen content in molten engineering metals.&apos; These investigations employ galvanic cells in which the electrolytes are various solid mixed-oxides which conduct current by movement of oxide ion vacancies under the influence of an oxygen potential gradient. Similar cells have also been used to measure the thermodynamic properties of mixing of solid alloys,&apos; one component of which has a much greater affinity for oxygen than the other component(s). One alloy system of obvious engineering importance comprised of two metals of greatly differing affinity for oxygen is copper-zinc. At the casting temperature of molten brasses, the zinc concentration is very difficult to control not only because its vapor pressure is very high, but also because of its high affinity for oxygen to form ZnO. Inasmuch as brass castings may be required to have a zinc concentration within very narrow limits, it would be advantageous for the brass industry to have a means for quickly measuring the zinc content in the molten alloy just prior to pouring. A calculation based on earlier thermodynamic studies of oxygen and zinc in dilute solution in binary Cu-O and CU-Z&apos; alloys indicates that the oxygen concentration of molten 70 wt pct Cu-30 wt pct Zn brass must be much less than 1 ppm for the separate phase ZnO not to exist in the ternary Cu-Zn-O system. Thus it can be assumed that all molten brasses, both in the laboratory and in the foundry, are sufficiently saturated with oxygen for the separate phase ZnO to be present. In view of the foregoing reasons, the cell investigated at 995°C for the purpose of measuring the zinc concentration in molten copper-zinc alloys, particularly those of brass compositions. In this cell the left hand electrode is a reference electrode comprised of a mixture of the pure powders of nickel and nickel oxide, to which a platinum contact is made. The electrode of interest is a molten Cu-Zn alloy of unknown zinc concentration with a tantalum wire contact. The electrolyte is the commercially available (Zircoa) calcia stabilized zirconia. The ZnO in the Cu-Zn electrode compartment is not intentionally added, but is naturally present as a result of the infinitesimal amount of oxygen required for its formation in this alloy system. In cell [A] nickel oxide is reduced at the cathode where O= represents the electrolyte. At the anode dissolved zinc of the Cu-Zn alloy is oxidized to form ZnO(s) in its standard state Thus the overall reaction is for which the molar free energy change is where 5 is the Faraday equivalent (23,063 cal per v equivalent), is the electromotive force of the cell in volts after correction for the Pt-Ta thermocouple, FOf (ZO) and AFF (NO) are the standard molar free energies of formation of the respective oxides, and a2n is the thermodynamic activity of zinc in the molten Cu-Zn alloy. The reference state of zinc in this case is taken to be the pure liquid. At constant temperature all the terms of Eq. [I] are constant except and azn Thus since all other participants in the electrochemical reaction are in their standard states, the change in the electromotive force of Cell [A] is represented only by a change of the thermodynamic activity of zinc at constant temperature. The zinc concentration is related to the activity by sampling the alloy for chemical analysis after cell measurements are taken. EXPERIMENTAL A typical cell construction is shown in Fig. 1. This and other experimental details were similar to that described earlier with the exception of some minor modifications which are detailed below.

Jan 1, 1970

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&apos;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&apos;s law at this gap edge becomes smaller as the gap becomes wider, The interrelation of gap location, the direction of departures from Henry&apos;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 D. W. Rudd, D. W. Vose, S. Johnson

The permeability of Mo-0.5 pel Ti to hydrogen was investigated over a limited range of temperature and pressuire (709° to 1100°C, 1.i and 2.0 atm). The resulting permeability, p, is found to obey the The experimental data justifies the permeation mechanism as a diffusion contl-olled pnssage of Ilvdrogen atoms through the metal barrier. 1 HE permeability of metals to hydrogen has been investigated by a number of workers and their published results have been tabulated by Barrer&apos; up to 1951. Since most of the work on the permeability has been accomplished prior to this date, the compilation is fairly complete. Mathematical discussion of the permeability process has been reported by Barrer, smithells, and more recently by zener. From these efforts several facts are observed. First, the permeability of metals to diatomic gases involves the passage through the metal of individual atoms of the permeating gas. This is evidenced by the fact that the rate of permeation is directly proportional to the square root of the gas pressure. Second, the gas permeates the lattice of the metal and not along grain boundaries. It was shown by Smithells and Ransley that the rate of permeation through single-crystal iron was the same after the iron had been recrystallized into several smaller crystals. Third, it has been observed that the rate of permeation is inversely proportional to the thickness of the metal membrane. Johnson and Larose5 verified these phenomena by measurirlg the permeation of oxygen through silver foils of various thicknesses. Similar findings were noted by Lombard6 for the system H-Ni and by Lewkonja and Baukloh7 for H-Fe. Finally, it has been determined that for a gas to permeate a metal, activated adsorption of the gas on the metal must take place. Rare gases are not adsorbed by metals, and attempts to measure permeabilities of these gases have proved futile. ~~der&apos; found negative results on the permeability of iron to argon. Also, Baukloh and Kayser found nickel impervious to helium, neon, argon, and krypton. From what was stated above concerning the dependence of the rate on the reciprocal thickness of the metal barrier, it is seen that although adsorption is a very important process, at least in determining whether permeation will or will not ensue, it is not the rate determining process for the common metals. A case in which adsorption is of sufficient inlportance to cause abnormal behavior has been noted in the case of Inconel-hydrogen and various stainless steels.&apos;&apos; APPARATUS The apparatus used in this study is shown in Fig. 1. The membrane is a thin disc (A), but is an integral part of an entire membrane assembly. The entire unit is one piece, being machined from a solid ingot of metal stock. When finished, the membrane assembly is about 5 in. long. Two membrane assemblies were made; the dimensions of the membranes are given in Table I. The wall thickness is large compared to the thickness of the membrane, being on the average in the ratio of 13 to 1. There exists in this design the possibility that some gas may diffuse around the corner section of the membrane where it joins the walls of the membrane assembly, If such an effect is present, it is of a small order of magnitude, as evidenced by the agreement of the values of permeability between the two membranes under the same temperature and pressure. A thermocouple well (B) is drilled to the vicinity of the membrane. The entire membrane assembly is then encased in an Inconel jacket and mounted in a resistance furnace. The interior of the jacket is connected to an auxiliary vacuum pump and is always kept evacuated so that the membrane assembly will suffer no oxidation at the temperatures at which measurements are taken. The advantages of this configuration are: 1) there are no welds about the membrane itself, so that the chance of welding material diffusing into the membrane at elevated temperatures is remote. 2) It is possible to maintain the membrane at a constant temperature. Since the resulting permeation rate is very dependent upon temperature, it is advisable to be as free as possible from all temperature gradients. 3) It is possible to obtain reproducible results using different specimens. The only disadvantage to this configuration is the welds (at C) in the hot zone. The welding of molybdenum to the degree of per-

Jan 1, 1962

South Dakota State School of Mines, Rapid City, S. D. C C O&apos;Harris,-President. A number of technical bulletins have been issued at the South Dakota State School of Mines but, unfortunately, most of them are out of print and as this directory is concerned only with available publications, the following are all that are now to be had Bulletin 11, A bibliography of the geology and mining interests of the Black Hills region (1917), no charge; 14, The geology, mineralogy, and scenic features of Custer State Park (1926), 40 cents plus postage on 1 lb ; 15, The Tertiary mineralization of the northern Black Hills (1927), charge, postage on 1 1b.; 16, The mineral wealth of the Black Hills t418 pages) (1929), 80 cents plus postage on 3 lb

Jan 1, 1933

By L. F. Bryant, J. P. Hirth, R. Speiser

The surface, gain boundary, and twin boundary energies, as well as the surface diffusion coefficient, of cobalt were determined from tests at 1354°C in pure hydrogen. A value of 1970 ergs per sq cm was calculated for the surface energy, using the zero creep method. It was possible to measure the creep strains at room temperature because the phase transformation was accompanied by negligible irreversible strain and no kinking. Established techniques based on interference microscopy were used to obtain values for the other three properties. The gain boundary and twin boundary energies were 650 ad 12.7 ergs per sq cm, respectively, while a value of 2.75 x l0 sq cm per sec was determined for the surface dufusion coefficient. In the course of a general study of cobalt and cobalt-base alloys, information was required about the surface energy of cobalt. Hence, the present program was undertaken to measure the interfacial free energy, or, briefly, the surface energy, of the solid-vapor interface of cobalt. The microcreep method was selected for this measurement because other surface properties could also be determined from the accompanying thermal grooving at grain boundaries and twin boundaries. A brief summary of the methods for determining the various surface properties follows. At very high temperatures and under applied stresses too small to initiate slip, small-diameter wires will change in length by the process of diffu-sional creep described by Herring.1 The wires acquire the familiar bamboo structure and increase or decrease in length in direct proportion to the net force on the specimen. For a specimen experiencing a zero creep rate, the applied load, wo, necessary to offset the effects of the surface energy, y,, and grain boundary energy, y b, is given by the relation: where r is the wire radius and n is the number of grains per unit length of wire. The first results obtained from wire specimens were reported by Udin, Shaler, and Wulff.&apos; udin3 later corrected these results for the effect of grain boundary energy. The grain boundary energy is determined from measurements of the dihedral angle 8 of the groove which develops by thermal etching at the grain boundary-free surface junction. For an equilibrium configuration: Measurements of the angle 8 can be made on the creep specimens4&apos;5 or on sheet material, as was done in this investigation by a method employing interference microscopy.= If the vapor pressure is low, the rate at which grain boundary grooves widen is determined primarily by surface diffusion and, to a lesser extent, by bulk diffusion. The surface diffusion coefficient, D,, is obtained from interferometric measurements of the groove width as a function of the annealing time, t. As predicted by Mullins~ and verified by experiment, the distance, w,, between the maxima of the humps formed on either side of the grain boundary increases in proportion to if grooving proceeds by surface diffusion alone. For this case: where fl is the atomic volume and n is the number of atoms per square centimeter of surface. When volume diffusion also contributes to the widening, the surface diffusion contribution can be extracted from the data by the method described by Mullins and shewmon.8 Where a pair of twin boundaries intersects a free surface, a groove with an included angle of A + B (using the groove figure and notations of Robertson and shewmong) forms by thermal etching at one twin boundary-free surface junction. If the "torque terms", i.e., the terms in the Herring10 equations describing the orientation dependence of the surface energy, are sufficiently large, an "inverted groove" with an included angle of 360 deg-A&apos;-B&apos; develops at the other intersection. The angles A + B and A&apos; + B&apos; are measured interferometrically. When the angle, , between the twinning plane and the macroscopic surface plane is near 90 deg, the twin boundary energy is calculated from the relation: 1) EXPERIMENTAL TECHNIQUES Five-mil-diam wire containing 56 parts per million impurities was used for making ten creep specimens. These specimens had about 15 mm gage lengths with appended loops of wire and carried loads (the specimen weight below the midpoint of the gage length) ranging from 3.7 to 149.8 mg. The wires were hung inside a can made from 99.6 pct pure cobalt sheet. Beneath the wires were placed small specimens of 20-mil-thick, 99.9982 pct pure cobalt sheet from which the relative twin boundary and grain boundary energies and the surface diffusion coefficient were measured. All the specimens were annealed at a temperature of 1354" i 3°C which is 92 pct of the absolute melting point of cobalt. The furnace atmosphere was 99.9 pct pure hydrogen that was purified further by a Deoxo catalytic unit, magnesium perchlorate, and a liquid-nitrogen cold trap. As a precautionary measure the gas was then passed through titanium alloy turnings which were heated to 280" to 420°C and replaced after every test period. The hydrogen was maintained at a

Jan 1, 1969

By F. R. Cattoir, R. W. Kimball, C. T. Anderson, V. V. Donaldson

THIS paper is the second of a series on the effect of various elements on hot-working characteristics of Fe-C alloys to be issued by this laboratory. The investigations being conducted at the Ferroalloy Research Branch of the U.S. Bureau of Mines, Redding, Calif., involve fundamental research on the effects of various alloying materials and impurities on the physical properties of high purity Fe-C alloys. This paper deals with the determination of the limit of forgeability of steels containing varying amounts of manganese and sulphur. A paper discussing the hot-working characteristics and the physical properties of the forgeable alloys is being prepared. One of the principal impurities in all steels is sulphur.. The phenomenon, hot-shortness, commonly attributed to sulphur, has long been a source of expense and inconvenience to both the maker and user of steels. In steelmaking practice, this effect of sulphur has been overcome by the addition of manganese which, apparently, acts as a desulphurizer. Manganese is also used as a deoxidizer and alloying material. The critical and strategic position of man- ganese gives added importance to research which may contribute to its conservation and more effective utilization. It is not the purpose or intention in the present paper to give any explanation of the mechanism of either hot-shortness or its prevention but rather to report the results of forging high purity Fe-C alloys of the range of compositions near the limit of hot-forgeability. Temperatures for each phase of reduction were duplicated within 20" to 30°F for all tests. The starting material was sponge iron, which, after melting and purification, gave a high purity iron containing about 0.001 pct each of silicon and phosphorus. Scrap iron was not considered suitable because of its high percentage of contaminants and wide variation in analyses. The sponge iron was melted and refined for melting stock in a three-phase, direct-arc, size ST, Moore Rapid Lectromelt furnace with a 500 kva rating as described in the preceding paper. Additives were carefully selected to avoid addition of contaminants. The sulphur was added as resublimed flowers of sulphur or purified roll sulphur of analytical grade. The manganese used was dehydrogenated high purity electrolytic material produced by the Bureau of Mines plant at Boulder City, Nev. High purity aluminum in the form of wire was used for deoxidation. The limestone was obtained locally and had the following analysis: CaO, 53.7 pct; MgO, 0.8; ignition loss, 42.4; R2O3, 0.2; SiO2,3.0; and P2O5, 0.014.

Jan 1, 1955

By Charles L. Mantell, P. P. Napolitano

High-purity tellurium oJ semiconductor grade may be prepared by a combination of electrowinning from tellurium oxide, electrorefining and controlled atmosphere melting, as detailed in the paper. SEMICONDUCTOR devices such as transistors and rectifiers depend upon extremely pure forms of silicon, germanium, and selenium. Although tellurium is chemically related to these elements, it has not been studied as a semiconductor because commercial forms are too impure. Highly purified tellurium would be an interesting starting point for a study of its solid-state characteristics. Tellurium shows a greater electrical conductivity in the direction of the helices or chains forming the crystals than at right angles to the chains, and thus is a semiconductor. Unlike selenium, the conductivity is only slightly increased by exposure to light. Impurities such as Ag, Cu, Au, Fe, Sn, As, Sb, Bi, Br, and I provide accepters and make extrinsic tellurium of the P type. So far, however, no elements have been found which, when introduced, would act as donors. Small amounts of tellurium dioxide enormously increase the thermoelectric power. Many extremely pure metals have been made by electrolytic refining or electrowinning procedures. Tellurium forms compounds in a number of valences, as indicated in Table I. The physical properties given in Table II do not show any unusual conditions which would interfere with the formation of elec- trodes, or the deposition of the metal on a cathode. Tellurium dioxide could be obtained in relatively high purities of 98 pct TeO2 or better at reasonable prices. Tellurium dioxide is soluble in caustic to form tellurites, which are conductive, ionizable, and from which tellurium metal may be deposited at a cathode. Preliminary solubility tests to saturation of tellurium dioxide in approximately 10 pct sodium hydroxide gave the results of Table III. The temperature range is a practical one for electroplating. Electrochemical test facilities were set up and these met the operating conditions of Table IV. For a determination of purity of deposits, there was available a Jarrell Ash Co. quantitative emission

Jan 1, 1964

By C. E. Nelson

The purpose of this discussion is to outline briefly the practices commonly followed in this country for the melting and refining of magnesium and its alloys. The processes used for the various forms of primary magnesium, as far as there are differences in the physical shape or behavior, will be discussed. The refining of general fine scrap or secondary magnesium was presented in an earlier paper.1 Inasmuch as the use of fluxes is an essential part of all the melting and refining processes, the principal aim of this paper will be to deal with these in sufficient detail to point out their unique characteristics, in order to make their use more effective. Types oF Melting Practice All melting and refining processes for magnesium and its alloys require the use of fluxes. These fluxes have a magnesium chloride base and other halide salts or oxides are added to give a density or behavior exactly suited to the particular melting practice. The successful handling of magnesium depends upon the proper use of the correct fluxes. There are four general methods of melting, summarized in the following paragraphs and treated in more detail in the section on Melting and Refining. Open-pot Method The open-pot method makes use of No. 230 flux.2 The flux provides protection during melting and a molten pool of flux into which the solid magnesium melts. It is stirred through the molten metal bath and agglomerates oxide or similar foreign bodies; then on quiet standing separates away, leaving the refined metal ball floating in an encircling layer of molten flux. It forms only a thin fluid film over the surface of the molten metal, which may be &apos; parted for hand-ladling processes and tends to cover the metal again after the ladle is removed. A very light dusting of the pot surface with fresh flux immediately after the ladle is removed is usually desirable. The open-pot method is used generally in the following processes: (I) alloying and secondary smelting in the production of ingot, (2) in sand foundries for premelting and to a smaller extent for the production of small castings requiring hand ladling, (3) in permanent-mold founding for premelting and also direct ladling to castings, (4) for continuous methods of preparing metal in the production of billets or ingots from which wrought products are fabricated, (5) in general scrap recovery. Crucible Process The crucible process makes use of No. 310 flux, which has the property of being thinly fluid at the start, to provide protection and refining qualities, and then drying out or thickening after a time, leaving a protecting crust on the pot surface until the time of casting. At that time it can be readily skimmed off or held back, thus allowing the contents of the crucible to be poured out directly into castings without fear of flux contamination. This flux is not

Jan 1, 1944

By D. W. Fuerstenau, D. A. Sullevan

In the experimental work for this comparison of wet and dry grinding, it was found that the size distributions for wet grinding operations are characterized by a constant value of the distribution modulus, (a; whereas, for dry grinding the distribution modulus decreases slightly with increased size reduction. Wet grindability seems independent of the weight of material in the mill while dry grindability depends on weight. Experimental data and eqmtions for each process are presented for noncleavable isotropic material, for cleavable or material in which there is some form of internal stress, and for energy consumption. The equation ED/EW=BK-? (where ED and Ew are, respectively, energy for wet and dry grinding, k is the size modulus, and B and ? are constants) was found to give the ratio of energy. Dry grinding is generally considered to require more energy than wet grinding. Taggart&apos; states that power consumption in wet grinding ranges from 60 to 90 pct of that required for dry grinding. Bond&apos; states that dry grinding requires one third more power than wet grinding. It is interesting that Rose and Sullivan&apos; note this same difference in power required for wet and dry grinding, but they state that on purely mechanical grounds it is difficult to see any great difference in fundamental principles between wet and dry milling, since dry milling may be regarded as wet milling with a fluid of low viscosity (i.e., air vs water). Yet it must be the viscosity of the fluid that is responsible for the differences between wet and dry grinding. Probably the most comprehensive investigation comparing wet and dry grinding has been that made by Coghill and Devaney. They compared the grind-ability of both chert and dolomite in a 19x36-in. batch ball mill under both wet and dry conditions. In these tests the weight of ore in the mill was varied from 35 to 200 lb and each grinding test was carried out for such period of time that the amount of -200-mesh material in the product was essentially the same for each test with a given material. Cog-hill and DeVaney&apos;s data for the grindability of dolomite, which are reproduced in Fig. 1, show that a comparison between wet and dry grinding is com- plex. The comminution of a material by a wet grinding method is characterized by a constant grindability over a wide range of mill loadings. Since grindability is the weight of material comminuted per unit of energy expended, it is equivalent to (w)/ (p)(t), where W is the weight of material being ground, P is the power, and t is the grinding time. In the case of wet grinding, the grindability of dolomite in the Coghill and DeVaney experiments was 0.546 * 0.009 ton per hp-hr when the load of dolomite in the mill ranged from 50 to 200 lb. On the other hand, for dry grinding no such simple relationship was found to exist between power, time, and weight of material in the mill. Dry grinding efficiency appears to depend greatly upon the amount of material within the mill. When the mill contained

Jan 1, 1961

Abbey. Robert Graham, District Mgr.. The W. W. Sly Mfg. Co., 50 Church St., New York, N. Y. &apos;21 Abbott, Clarence E., V.P., Charge of Raw Materials, Tenn. Coal, Iron & R. R. Co., 1242 Brown-Marx Bldg., Birmingham, Ala. &apos;04 Abbott, Louis Benjamin, Chief Engr., Consolidation Coal Co., Watson Bldg., Fairmont, W. Va. &apos;15 Abeel, George H., Jr., Cons. Min. Engr 12S1, S. Canon Dr., Beverly Hills, Cal. &apos;18 4 -Abel, Raymond L., Asst. Prof., Dept. of Pet. Refin.. Univ. of Pittsburgh. Pittsburgh, Pa. &apos;28 Abel, Walter D., Cons. Engr 650 S. Grand Ave., Los Angeles, Cal. &apos;82 Abele. Louis T., Min, & Met. Engr., Supt., Texas Hill Mine Coulterville, Cal. &apos;31 Abell, Leo M Sullivan Concentrator, Chapman Camp, B. C., Canada &apos;31 Abernathy, George Elmer, Prof. of Geol. & Min., Kansas State Teachers College. Pittsburg, Kan. &apos;20 Aborn, Robert H., Asst. Met., Research Lab., U. S. Steel Corp., Lincoln Highway, Kearny, N. J. &apos;19 Abraham, W. E. V., Member, Geological Staff of Burmah Oil Co., Ltd., Nyaunghla, Upper Burma, India. &apos;28 Abstein, Henry T., Engr. & Mgr., Profile-Tamarack Mines Co Yellow Pine, Idaho &apos;27 Acker, E. O&apos;C., Met 128 East Washington Lane, Germantown, Philadelphia, Pa. &apos;86 Ackerman, D. E., Met., Research Lab., International Nickel Co., Inc Bayonne, N: J. &apos;24 Ackerman, George F., Engr., Real del Monte y Pachuca Min. Co., Apt. 3, Pachuca, Hgo., Mexico &apos;29 *Acres. T. H.. Geol. Dept., Valuation & Pet. Engrg., Richfield Oil Co., 555 S. Flower St., Los Angeles, Cal. &apos;29 Adachi, Jinzoo Address Wanted &apos;88

Jan 1, 1934

By C. E. Birchenall, R. H. Condit

THREE surface activity procedures are in com--L mon use for the determination of diffusion coefficients in solids. In the oldest of these&apos; the activity observed at the original surface is compared before and after diffusion, where all the activity is in a thin, plated layer on the surface before diffusion. Partial absorption of the radiations from active atoms which have diffused below the surface reduces the effective activity after diffusion. The formula employed to calculate the diffusion coefficient is where F, is the ratio of final to initial activity at the surface, measured with identical counting geometry; Z=u3Dt, where D is the diffusion coefficient; t is the diffusion time; and u is the absorption coefficient for the radiation in the solid as defined by Lambert&apos;s law. This absorption law implies that all the rays are parallel to each other and normal to the specimen surface. This assumption of a collimated beam used by Steigman, Shockley, and Nix has been adopted by all other investigators and, although it gives results which are approximately correct under restricted physical conditions, it does not represent many actual circumstances. It is the purpose of this paper to show the importance of the divergent rays and to indicate a procedure for taking them into account. In the residual activity method the activity is determined on a series of surfaces ground on the specimen at progressively greater depths in the diffusion layer parallel to the initial surface. Gruzin2 has de- rived a formula for this procedure, which may be put in the form where I is the ratio of the activity measured at a newly ground surface at distance k below the initial surface to the activity at the initial surface measured after diffusion, and K= k/2p Dt. A third procedure involves the autoradio-graphic determination of activity on a plane ground at a small angle to the initial interface through the penetration zone. Aut oradiography can be particularly sensitive to the oblique rays. Unlike most counters which detect essentially all ß particles or X-rays which enter the active volume as a single event, the photographic emulsion may be thin enough so that oblique rays with longer path length in the emulsion produce more darkening than rays which move normal to the film plane. Consider a plane containing a source of radiation uniformly spread over a circle and a point counter located on the perpendicular through the center of the circle. As the counter moves along this line, the total angle 6, at the counter subtended by the specimen will vary. For a fixed counter distance, let 6 be angle between the counter axis and the line connecting the counter to a point P on the active plane. If an absorber of thickness X is interposed parallel to the source between counter and source, the ray from point P to the counter will pass through an absorber thickness X secant 6. Exponential absorption is assumed to hold for all rays. If r, is the ratio of intensity at the counter with absorber to the intensity without absorber and a = pX, 1 00 The behavior of this integral, evaluated numerically,

Jan 1, 1957

By A. M. STROKG

Discussion of the paper of Charles R. Keyes, presented at the Spokane meeting. Bulletin o. 34, October, 1909, pp. 867 to 903. A. M. STRONG, Bishop, Cal: (communication to the Secretary*) The paper of Mr. Keyes gives us the most complete account of the geology of the borax-deposits in the Death Valley region that has yet been published, and is a valuable addition to the geological literature of a very interesting though little-known territory. During the past ten years I have been over much of the northern part of the country described by Mr. Keyes and the region immediately north of it. Mr. Keyes seems to give the impression that Furnace creek is the northern end of these borate-bearing deposits, but such is not the case. Of the seven principal marsh-deposits which for years furnished the greater part of the borax supply in the manner described by him, four are north of the boundary-line as given on his map. The entire territory immediately east of the Sierra Nevada is composed of a series of sinks, each with a well-defined drainage-area.. Of these, Death valley is the deepest, and its drainage-area one of the greatest. The section given in the paper is typical of any line drawn eastward from the Sierra Nevada. At the lowest point of each of these sinks is a marsh, which, in times of heavy rain-fall in the mountains, is converted into a lake. These marshes always contain borax, which is now considered to have been derived from the washing of the Tertiary lake-beds in the surrounding mountains, of which they form a considerable part. Additional territory which I have studied shows that the boundaries given on Mr. Keyes&apos;s map should be considerably extended to the north. Just how far these borate-beds extend I am not prepared to say. J. E. Spurr says of them : 1

Feb 1, 1910