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By N. R. Adsit

THE B-Ni system was chosen for this study because of the great interest being shown in boron-fiber-strengthened composite materials. Boron fibers were obtained from Texaco Experiment, Inc. They average 4.2 mils in diam with a 0.5-mil tungsten wire in the center. In order to make the diffusion couple, the fibers were included in the nickel matrix by electroforming. The samples were placed in a preheated furnace for the desired temperature and length of time. Sectioning and polishing the samples revealed concentric rings as shown in Fig. 1. The average penetration distance, X, was calculated by measuring the radius of the second phase (the white shell in Fig. 1) and subtracting the original radius. The second phase was identified as NiB by X-ray diffraction. This allows the kinetics of the formation of the phase NiB to be calculated by Eq. [I], which is taken from offman:"

Jan 1, 1967

By R. D. Pehlke, J. V. Gluck

AS a portion of a general study of liquid-metal thermodynamics, high-temperature galvanic cells were used to study the effect of added dilute solutes on the activity of zinc in dilute solution with molten bismuth in the range 450° to 650°C. 1,2 The cells were of the type The experimental procedures have been described previously.1 In the course of studies conducted in the bismuth-rich corner of the systems Bi-Zn-Au and Bi-Zn-Cu, marked discontinuities were observed in the electromotive force-temperature relations for a number of the experimental compositions. Above the discontinuity temperatures, the relations, which were linear, exhibited slopes similar to the binary alloy of the same mole fraction zinc, as shown in Figs. I and 2. Below the discontinuity temperatures, the slopes were markedly different, but the relations remained linear. In general, as the amount of the third eletnent was increased, the slope of the lower portion of the relations tended to become less positive. The slopes of electromotive force-temperature relations reflect the entropy of mixing of zinc and, therefore, the occurrence of a discontinuity marks the transition between two different equilibrium situations involving the solution of zinc. A number of other investigators3-5 have used such observations to determine liquidus boundaries in binary alloys. Since the upper portions of the ternary electromotive force-temperature relations of this study had the same slopes as the binary alloys, the discontinuities are interpreted as marking the transition between the single-phase liquid region and the underlying two- and three-phase regions. Reference to the Zn-Bi equilibrium diagram6 confirms that the binary alloys were single-phase liquids at the experimental temperatures. Fig. I shows the electromotive force-temperature relations for the alloys containing Bi-Zn-Au and Fig. 2 shows similar relations for the Bi-Zn-Cu alloys. In the lower portion of each figure, the temperature of the discontinuity is plotted vs the mole fraction of the added solute at the various levels of zinc concentra- tion. Cross-plots from these curves at constant temperature permitted the construction of the partial liquidus surface isotherms shown in Figs. 3 and 4.

Jan 1, 1967

By Bengt Helmerson

A new tankhouse was started in January 1959 at the Copper Refinery of the Boliden Co., Skelleftehamn, Sweden. In early 1961 a semiautomatic machine for looping and straightening of starting sheets was introduced to substitute previous manual operations. The machine as well as consequent, racking and handling is described. Finally, economic benefits achieved and new constructions for the future are discussed. HISTORY Tankhouse operations at the Boliden Co. 's Smelter in Skelleftehamn started in 1932 on a scale that since then has been gradually increasing. In order to rationalize the operations, a new tankhouse was erected. It went into production in January 1959 and was designed for a yearly production of 35,000 metric tons at a current density of 16 amps per sq ft. Already from the beginning, however, the tankhouse has been run with a current density of 21.5 amps per sq ft, corresponding to a maximum capacity of 50,000 tons a year. During the time of planning of the new tankhouse, due consideration was given to the possibilities of mechanizing the operations. New ideas could be and were actually tested on full or pilot plant scale in the old tankhouse. In that way we developed a system for the cathode handling including washing, weighing, and transportation. A system using forklift trucks in combination with trailers and overhead cranes has been developed for transportation and racking of anodes and also for handling of anode scrap. With respect to the electrolyte, circulation and temperature control are partly automatic. Special attention was paid to the production of starting sheets, which operation normally requires a great number of man hours, and it was made the object of a particular survey as to the best ways of straightening starting sheets, attaching loops to the sheets, and so forth. As a result, a machine was designed during 1957-58 and built in our own shops. After a period of tests, the new equipment was put in operation commercially on the 10th of April, 1961. Since this date the machine has produced about 2 million starting sheets without interruption and has been the only source of looped starting sheets for the tankhouse. GENERAL DESCRIPTION Fig. 1 shows all the major parts of the system. These parts are: slitting machine with feeding table (I), standard roller leveler, type Ungerer (2), tilting roller table (3), conveyors for sheets and suspension bars (4, 7), storage of suspension bars (51, punching and stitching machine (6), two lift-turn-tilt tables (8) for discharging the starting sheets, two rack conveyors (9) for sheet assemblies. Included are a hy-daulic pump station and panels for pneumatic and electric controls. SLITTING AND STRAIGHTENING The machine is fed by hand by a man sitting in front of the slitting-machine table, Fig. 2. This operator inserts one sheet at a time into the slitter. After being trimmed, the sheet is automatically conveyed to the following step of handling, straightening. The slitting machine cuts away about 8 mm of the upper and lower parts of the sheet (in relation to its original position in the stripper section) for two reasons. The first one is to give the machine sheets of uniform dimensions; the second one is a matter of quality. Normally the starting sheets as stripped have a thick edge at the bottom end. This part would collect anode slimes and might also cause short circuits when inserted in the cells without trimming. The straightener used is of German construction

Jan 1, 1967

Jan 1, 1967

By David W. James, Howard Jones, George M. Leak

Conditions are described for producing, by primary recrystallization, a matrix suitable for the growth of large grains near (110)[001] orientation in silicon iron strip by secondary recrystallizaliun in a steep temperature gradient. The orientation distribution of these large grains is expressed in terms of rotational deviations about the cross-rolling direction, the rolling direction, and the normal to the sheet, the deviational spread increasing in that order. With the aid of cowplenientary published data on the orientation dependence of growth rate, it is shown that this observation is consistent with the oriented-growth theory of recrystallization lextures. It is conclutled that growth-rate and orientation-distribution data obtained in a steep thermal gradient should be used with caution to account for isothermally Produced recrystallization textures. SEVERAL authors have reported methods of growing large grains by re crystallization of a small-grained matrix in silicon iron 1- B and pure a cr The present study was a preliminary in the growth of single crystals and bicrystals for surface relaxation," grain boundary mobility, and grain boundary diffusion studies. The method was to control the growth of a seed crystal into a suitable primary re crystallized matrix by feeding through a steep temperature gradient. The driving energy for growth derived from the grain boundary energy released as the seed crystals grew into the matrix. Thus, stability of the matrix against normal grain growth was considered to be essential for success. It was known that the manganese sulfide dispersion present in commercial silicon iron performs this function during secondary recrystallization to the (110)[001.] texture.12 Hence commercial, rather than high-purity, material was used throughout. The paper describes the growth conditions for grains large enough to be used as seed crystals for further growth into single crystals. The orientation distribution of the seed crystals is analyzed and its significance for the theory of recrystallization textures is discussed. EXPERIMENTAL PROCEDURE Strip material was supplied by the Steel Co. of Wales, Ltd. The chemical analysis in weight percent was Si, 2.90; C, 0.015; Mn, 0.059; P, 0.011; S, 0.027; Ni, 0.032; 0, 0.009; Fe, balance. A gradient furnace of similar design to one described previously4 was loaned from B.I.S.R.A. It consisted essentially of a vertical water-cooled copper slot projecting downwards into the hot zone of a molybdenum furnace. Hydrogen was passed through the furnace to protect both heating element and specimen from oxidation. Strip specimens up to 8 cm wide and 0.2 cm thick were sealed into the furnace at the mouth of the copper slot. A coating of light oil on the strip surface maintained the seal during translation of a specimen. The maximum temperature gradient in the region just below the copper slot was 500°C per cm over 1 cm, with the hottest point controlled at 1175°C. Several large grains would usually grow by secondary recrystallization from the primary matrix when a specimen was immersed in the hot zone for about 30 min. A back-reflection X-ray camera was constructed to facilitate rapid and accurate orientation determinations of the large grains produced. It was possible to reproduce a standard geometry, with regard to strip and camera, without the tedium of careful alignment on each occasion. Specimens, typically 4 cm wide and 75 cm long, were cut with the longitudinal axis parallel to the rolling direction of the original strip. The surfaces were cleaned by immersion alternately in a hot aqueous solution containing 2 pct hydrofluoric acid plus 10 pct sulfuric acid and in cold 10 pct nitric acid. The nitric acid etch was just sufficient to reveal the grain structure. Rolling and annealing treatments to prepare the matrix (discussed below) were followed by growth of seed crystals in the gradient furnace. The matrix was transformed to a single crystal by growth of a selected seed crystal connected to the matrix by a thin neck. 4,5 Growth was promoted by controlled feeding into the gradient furnace. Several single crystals of controlled orientation were grown successfully from seed crystals by twisting the interconnecting neck in a reorien-tation jig.4 EXPERIMENTAL RESULTS AND DISCUSSION Growth Conditions. A suitable matrix for growth of large grains was prepared starting from primary re-crystallized strip 1.9 mm thick. This was cold-rolled in two stages each being followed by a recrystallization anneal at 800°C for a few minutes. Such treatment gave the required growth matrix only if the two cold-reduction stages were each performed in several passes and in the following ranges: the first, 30 to 70 pct; the second, 10 to 50 pct. Immersion in the temperature gradient otherwise resulted in an equiaxed

Jan 1, 1967

By K. A. Jackson, J. D. Hunt

A new classification of eutectics is proposed, based on tlze entvopies of wzelting of the tuio eutectic phases. The clnssification was used to predict suitable tvansparent analogs of the metallic systems. Experimental confir?nation loas obtained for the theovetical shape of the lamellar solid-liquid interface, fov the fault mechanisms of lanzellar spacing changes, and for the development of low-energy solid-solid boundaries between the lamellae. An explanation is presented to account jov the irvegular and coinplex regular structures zrhich are found in some eritectic systems. FrOM experimental observations, single-phase materials can be divided into two groups according to their solidification characteristics, those that grow as faceted crystals and those that do not. acksonl' showed from thermodynamic reasoning that the type of growth depended on a factor a which was almost thg entropy of melting. Most nonmetals have high entropies of melting (a greater than 2) and grow with crystalline facets. Most metals have low entropies of melting (CY less than 2) and grow almost isotropically with no facets. The authors propose that eutectics may be classified in a similar manner. There are three groups of eutectics, those in which both phases have low entropies of melting, those in which one phase has a high and the other phase has a low entropy of melting, and those in which both phases have high entropies of melting. Lamellar or rodlike structures are formed in systems in which both phases have low entropies of melting. In these alloys dendrites of either phase may be formed, when the alloy is rich in the relevant component. Examples are Pb-Sn, Sn-Cd, Pb-Cd, Sn-Zn, Al-Zn. Irregular, Fig. 14((), or complex regular, Fig. 14(b), structures are formed in alloys in which one phase has a high entropy of melting and the other has a low entropy of melting. Examples are A1-Si, Zn-MgzZnll, Pb-Bi, Sn-Bi. When the alloys are rich in the low entropy of melting phase, dendrites are formed; when the alloys are rich in the high entropy of melting phase, faceted primary crystals are produced. These crystals are sometimes called hoppers or pseudodendrites. In this work the term dendrite will only be used to describe nonfaceted primary crystals. Dendrites are not formed during solidification in high entropy of melting single-phase materials. The third group of eutectics includes alloys in which both phases have high entropies of melting. Each phase grows with a faceted solid-liquid interface. Since most metals do not have high entropies of melting, metallic examples in this eutectic group are rare. However they may occur between some intermetallics and semiconductors or semimetals such as silicon, germanium, and bismuth. Attempts have been made to study eutectic solidification visually by watching the growth process.374 Since metals are not transparent, the observations had to be made on external surfaces. This difficulty can be overcome by using transparent analogs of the metallic systems. As was mentioned earlier, most single-phase compounds have entropies of melting greater than 2 and so grow as faceted crystals. Recently organic materials with entropies of melting less than 2 were investigated.' These materials grow in exactly the same way as the low entropy of melting metals. When the materials are pure, they grow with a solid-liquid interface parallel to an isotherm; when they are impure, cells or dendrites are formed. Since these materials are transparent, have low melting points, and even have cubic structures, they should be ideal for making up transparent analogs of the metallic eutectics. The purpose of the present work was to investigate these organic eutectics and to see whether this quite different series of eutectics could be classified in the same way as the metallic systems. The observations made on the organic alloys are also discussed with reference to the current theories of lamellar growth. Explanations are proposed to account for the structures formed in the other eutectic groups. EXPERIMENTAL Thin cells containing the organic alloys were uni-direction ally solidified on a specially constructed microscope stage.' Uniform growth rates were obtained by moving the cells, with a motor drive, through a fixed temperature gradient, so that the solid-liquid interface remained stationary with respect to the microscope objective lens. The cells were made by fusing two microscope cover slides 7/8 by 7/8 by 1/100 in. together on three sides, leaving a gap of 1 to 3 mils between the slides, and these were filled by surface tension. A preliminary investigation of the phase diagram between two components could be made very rapidly. One side of the cell was filled with component A and the other side with component B. Since only a small amount of mixing could occur every composition from pure A to pure B was present in the cell. When the cell was placed in the temperature gradient a pictorial representation of the phase diagram was obtained. Eutectics, peritectics, "interorganics", and solid -solid transformations could be readily detected. Fig. 1 shows part of a eutectic phase diagram. The Sample was first grown slowly then stopped. The two

Jan 1, 1967

By R. J. De Angelis, J. B. Cohen, A. Nelson

In this note several recent results on twinning in copper shock-loaded with planar shock waves will be presented and the role of the twins in recrystalliza-tion will be discussed. The twinlike markings first observed in shock-loaded copper by smith1 were identified as twins by De Angelis and Cohen.2 This identification has been confirmed by others.3 In Ref. 2 it was also shown that there is an orientation dependence for twinning at low shock pressures, such that twins in a crystal loaded in [lll] form in the rarefaction or tensile wave but in

Jan 1, 1967

By P. K. Weimer

Coinpletely integrated thin-film circuits inco?,porating more than 1000 active and passive elements have been fabricated reproducibly in the laboratory by evaporation of- all components. A 180-stage modified shift register comprising 540 CdSe TFT's, 360 resistovs, and 180 capacitors was deposited upon a glass substrate during one pump-down of the vacuum systeitl. Experimental units have been operated for more than 5000 hr at temperatures uP to 85°C without failure of any slages. The present pupper reviews the charvactevistics of evaporated thin-film transistors (TFT's) and discusses their application to integrnted circuils. INTEGRATED circuits most widely used today are based upon silicon technology, with the circuits formed on the surface of a block of single-crystal silicon1 or on a block of sapphire 2,3 upon which a thin layer of silicon has been deposited. Transistor patterns and interconnections are defined by photographic procedures using photoresist masking. Large groups of transistors are produced in batches which undergo many processing steps, some of which are carried out at elevated temperatures. Passive elements are formed by treatment of the semiconductor surface or are deposited by evaporation alongside the active elements. The size and complexity of the circuits are limited by defects in the devices and by the size of the available single-crystal chips. Capacitative coupling to the semiconducting substrate may also limit useful size and frequency response of the circuits. An alternative approach to integrated circuits is based upon the deposition by evaporation of all circuit components upon a noncrystalline, insulating substrate such as glass.4 Thin-film field-effect transistors,1'6 known as TFT's, can be deposited in large arrays on glass or plastic substrates at the same time the associated passive elements are being deposited. Although still in the research stage the all-evaporated approach is expected to offer certain advantages for many applications. In particular, the use of thin films upon a noncrystalline substrate offers the prospect of producing complex, large-area circuits not now feasible with single-crystal silicon. Important applications of this type include memory arrays for computers and imaging devices for television. The ease with which the evaporated TFT's can be deposited may permit continuous, automated production methods not possible with high-temperature batch processing. Recent advances7'8 in the fabrication of thin-film transistors have led to greatly improved reproduci-bility and life of the TFT's. Experimental circuits having over 1000 active and passive elements deposited upon a common glass substrate are currently being produced in the laboratory. The present paper reviews recent progress in the development of the TFT and in its application to integrated circuits. I) DESCRIPTION OF THE THIN-FILM FIELD-EFFECT TRANSISTOR The TFT is a field-effect transistor of the type having the control gate separated from the semiconductor by a thin insulating spacer. Although its operation resembles that of the silicon MOS transistorg its construction is based entirely on thin-film techniques. Fig. 1 shows a cross-sectional view of an evaporated TFT deposited upon a glass substrate compared with a silicon MOS transistor deposited upon single-crystal sapphire.3 The semiconductor in the TFT is a poly crystal line layer, of a material which can be readily evaporated, such as cadmium sulfide, cadmium selenide,l0 or tellurium." Silicon monoxide layers have usually served as the gate insulator, but other oxides, sulfides, and fluorides may be used. Film thicknesses range from a few hundred to a few thousand angstroms. The source, drain, and gate electrodes in the TFT are of metal. Qpical source-drain gap dimensions are 0.0003 x 0.030 in., with a gate strip whose width slightly overlaps the source and drain. The source and drain electrodes should make low impedance contacts to the semiconductor. With cadmium sulfide films, gold is a satisfactory material for underlying electrodes, while aluminum is preferable for overlying electrodes.12 Considerable variation in design of the TFT is permissible, with the electrodes being

Jan 1, 1967

By D. L. Archer, W. W. Owens

Conventional waterflooding often is uneconomic in highly fractured reservoirs because of the gross bypassing of the reservoir oil by injected water. Imbibition and pressure pulse flooding have been used in at least one fractured reservoir in an attempt to achieve better oil recovery performance. This paper presents the results of laboratory flow tests conducted on large cores to evaluate the possible applicability of these methods (particularly pressure pulse flooding) to different types of reservoir systems. Test data were obtained on both water-wet and oil-wet systems, and on systems having two widely different levels of compressibility and flow capacity. Results indicate that pressure pulse recoveries from fractured reservoirs will likely not exceed 5 to 10 per cent pore space with maximum response achieved during the first pulse cycle. Improved recovery by this method is possible from both oil-wet and water-wet reservoirs. Comparable saturation distributions during imbibition and pressure pulse production suggest that an initial pressure pulse cycle to speed production response would not interfere with subsequent imbibition flooding in water-wet reservoirs. INTRODUCTION There is a steady increase in the number of fluid injection projects being initiated each year to improve oil and gas recovery over that obtained by primary production mechanisms. Experience gained in different geographical areas and with different recovery methods is teaching that reservoir anatomy is one of the more important factors controlling the success or failure of such projects. Fractured formations appear to be the rule rather than the exception, especially in carbonate reservoirs. Conventional methods of fluid injection, whether it is waterflooding, gas injection or miscible flooding, have limited applicability to highly fractured reservoirs because of the severe bypassing of reservoir fluids. The result is early breakthrough of the injected fluid and rapidly increasing ratios of injected to in-place fluid with an undesirable effect on return on investment. Thus, innovations to conventional methods must be developed if recovery from fractured reservoirs is to be optimized. One new method proposed for application to highly fractured reservoirs is pressure pulse waterflooding. Although pressure pulsing with gas has been suggested' and rested in at least one reservoir; the Sohio Oil Co. is generally credited with the development and testing of pressure pulsing in conjunction with waterflooding. Publications" of Sohio's waterflood operations in the Spra-berry Trend indicate that the idea for pressure pulse flooding evolved from a critical analysis of the disappointing early performance of their flood initiated in a portion of the trend in April, 1961. This flood was planned to take advtantage of imbibiltion and high pressure gradients across the reservoir matrix blocks (unfractured Mocks of the reservoir rock which are visualized to be generally surrounded 'by the fracture system) evaluated in pilot tests by the Atlantic Richfield Co.5 and Humble Oil & Refining Co.' However, the early recovery and pressure performance of this flood indicalted that high pressure gradients induced between the fracture system and the centers of the matrix blocks were forcing water into the periphery of the blocks and temporarily interfering with the counter-current flow of oil due to imbibition. Fill-up in the blocks was occurring with re-solution of the free gas phase as pressures climbed above the original reservoir bubble point. It appeared that cessation of water injection to permit the capillary forces to become dominant and that expansion of the rock and its contained fluids during pressure reduction might aid in expulsion of oil from the rock matrix into the fractures. Subsequent production performance. aflter cessation of injection, proved this hypotheslis correct. Thus, pressure pulse waterflooding was born. Pressure pulse flooding appears to have several advan'tages over imbibition type flooding in highly fractured reservoirs. First, all wells may be used for water injection which should hasten fill-up and achieve a more rapid increase in reservoir pressure. Second, because of increased injection pressures and rates, flooding gradients will force water into the reservoir matrix more rapidly than would be achieved by imbibition alone. Third, during the pressure depletion cycle of the flood, the compressibility of the system, which has been increased by resolution of the free gas phase, provides energy for the displacement of oil at a rate greater than would correspond to countercurrent flow during imbibition. Fourth, during depletion all wells may be put on production, thus contributing to higher oil withdrawal rates on a reservoir-wide basis. One possible disadvantage of pressure pulse flooding as compared to imbibition floodling, however, is that the outer periphery of each matrix block is flooded to a residual or near residual oil saturation during the Water lnjection stage. This zone of reduced permeability to oil m'ay offer greater restriction to the production of

Jan 1, 1967

By Alexander Coucoulas

FABRICATION of thin-film circuits deposited on glass substrates requires the formation of permanent electrical contacts. Since thin films are in the order of a few thousand angstroms thick and are deposited on nonconductive surfaces such as glass, new methods of lead attachment are being pursued in the microelectronics industry. Ultrasonic welding is being considered in thin-film technology since joining can be accomplished between a wide variety of dissimilar materials.l,' Ultrasonic welding is accomplished by a transducer-coupling-tip system which converts high-frequency electrical energy into mechanical vibrations and delivers it into the weld region. During the process the tip oscillates in a direction parallel to the surface of the weldments, inducing shear stresses in the work pieces which are clamped between the tip and anvil. Though the basic bonding mechanism is not clearly understood, it has been described as closely akin to friction welding. In the course of an investigation concerned with ultrasonic we!ding of aluminum wires to tantalum thin films (1400A) deposited on glass, low weld strengths were related to glass failure. Upon investigating this condition, an improved method of bonding was developed where the aluminum was held at a temperature where a minimum amount of strain hardening occurred during the introduction of ultrasonic energy. Experimental Procedure. Aluminum wires (0.015 in,) were bonded to tantalum thin films with an optimized set of welding parameters (power, time, clamping force) employing a commercial 100-w 60-kc ultrasonic welder. Forty-five degree shear-peel tests, where the lead is pulled at a 45-deg angle with respect to the substrate at 0.2 in. per min, produced a large variation from zero to the strength of the wire, Table I. Inspection of the weld region generally revealed: glass cracking before and after testing; the removal of glass nuggets from the substrate by the lead during testing, Table I; thin-film penetration. In an effort to improve the shear-peel strength, the aluminum between the tip and substrate was heated above ambient temperature through an argon gas media prior to and during welding with the same parameters employed above. With the addition of heat: wire deformation was increased; shear-peel tests all failed at the weld-wire junction, leaving the bonded portion undisturbed; no evidence of glass cracking or film penetration prior to or after testing was observed. In order to prevent failure at the weld-wire junction due to excessive wire deformation, 0.035-in. aluminum wires were welded to tantalum thin films with an optimized set of welding and heating parameters. As

Jan 1, 1967

S. Tandanand, Twin Cities Mining Research Center, U. S. Bureau of Mines As an addition to the fine reviews on drilling presented in the foregoing papers, we feel it would be appropriate to mention briefly some work in this area by the U. S. Bureau of Mines. The Bureau has had under way for several years at its Twin Cities Mining Research Center studies directed toward a better understanding of basic drilling mechanisms. The work includes drillability investigations with diamond rotary, and with percussive drilling systems, as well as fundamental studies of rock behavior under drill bit types of loading. Results of our work to date have contributed the following to the state of the art. MECHANISM OF ROCK FAILURE-Rock fragmentation through use of mechanical energy systems, including drilling systems, consists of two major components-machine and rock. The two components are related to each other by their functional behavior and their resultant motion which the components mutually influence. Forces in the systems are transmitted directly to the bit which in turn induces stresses in the rock. When the induced stresses exceed the strength of the rock, the rock fails resulting in penetration. Rock strength is a function of the forces applied to the rock. Stresses under a drill bit, regardless of bit configurations, are essentially compressive, resulting in a condition where the rock has the highest resistance to failure. The ratio of principal stresses induced under drill bits is an indication of the mode of failure in the rocks. Initially, compressive stresses under the drill bit cause rock to undergo inelastic deformation. The impression observed at the first stage of crater formation under the drill bit shows that rock is no longer elastic. Associated subsurface failure at this stage precedes total rupture which subsequently appears at the rock surface. Thus, explanation of crater formation, by applying theory of elasticity alone, is likely to be over-simplified. ENERGY VERSUS VOLUME OF ROCK REMOVED-Experimental results show that energy per unit volume of rock removed is constant for a particular rock and bit type. Rock offers a definite resistance to penetration, depending on the method of the energy application; this may be defined as the drilling strength of a rock. Energy consumption in a drilling system may be divided into two components: 1) Energy required to move the machine parts; and 2) energy consumption in breaking rock. Component 1 is dependent on the type of the machine. Component 2 is dependent on the strength properties of rock and the efficiency of the bit in rock cutting. The sum of the energy required in both components determines the total energy required in breaking rock. Our work in this area has included consideration of both diamond and percussive drilling systems. PENETRATION RATE-For a drilling rate expression to be useful in predicting field performance, it should include the operating characteristics of the drilling machine. Eq. 37, for example, is simply a statement of the fact that the drilling rate is determined by the power output of the machine (2pNT) and the power requirements to break the rock in the hole (AER). In order to predict the performance of a particular drill and the effect, for example, of the rotary speed, on the drilling rate, R, Eq. 37 must be modified to include the

Jan 1, 1967

Jan 1, 1967

By C. A. Wert, M. G. Coleman

The Zener relaxation in alloys in the a! solid-solution region of the Cu-Ni-Zn ternary system has bear investigated. Of the binary solid solutions that bound this region, Cu-Zn and Ni-Zn exhibit measurable Zener peaks whereas Cu-Ni does not. At constant atomic percent copper, the Peak height drops uni.forinly from the value in the Cu-ZTL binary to zero in CIA-Ali. The cariation of peak ternperatuve with composition is linear. At constant atomic percent zinc, the peak height in the ternary alloys goes through a large maximum as compared with the binary values. The temperature of these peaks varies smoothly with composition. The half-width of the peaks in the ter nary alloys, however, are much larger than those in the binaries. A large enhancement of the relaxation strength of the Zener relaxation in ternary Au-Ag-Zn alloys as compared to the relaxation strengths in Au-Zn and Ag-Zn binary alloys was observed by Firson and ert.' Since this effect was unexpected, the present study was devised to investigate whether enhancement of the Zener relaxation in ternary alloys is a general feature or is particular to the Au-Ag-Zn system. We have chosen the Cu-Ni-Zn alloy system for this investigation. Measurable Zener relaxations are observed in both the Cu-Zn and the Ni-Zn binary systems, but not in the Cu-Ni binary system. A large solid-solution region extends to large concentrations of zinc, making it possible to vary composition of the alloys over a wide range without crossing phase boundaries. EXPERIMENTAL PROCEDURE Two series of alloys were prepared. the first at constant atomic percent copper, the second at constant atomic percent zinc. The compositions of these alloys are shown by the circles in Fig. 1. The alloys were prepared by melting the individual components, each of which had previously been vacuum-melted, in an evacuated quartz capsule in an induction furnace at 1500 C. The capsules containing the molten alloys were quenched in water to reduce coring. Any individual melt which exceeded 0.001 pct weight loss was discarded. The ingots were swaged to a 50 pct reduction of area and annealed for 1 week in an evacuated quartz capsule to aid homogenization. The alloys were then

Jan 1, 1967

By J. G. Eberhort

ThE literature of surface phenomena shows that, except for most of the rare-earth elements, surface tensions have now been determined for almost every liquid metal. The situation for liquid metal oxides is, in contrast, characterized by a great scarcity of surface-tension data. A surface-tension correlation between these two classes of substances has been found which provides a means of estimating unknown liquid-oxide surface tensions from the corresponding known liquid-metal surface tension. Lf the surface tension of the liquid metal is a(M) and that of the liquid metal oxide is o(M,Oy), then oxides of all stoichiometries can be brought into one correlation if is plotted against with the surface tensions taken at the respective melting points. The available data is displayed in this fashion in Fig. 1 where the relationship between the surface tensions of the two classes of liquids is found to be The correlation in Fig. 1 is based on data found for nine liquid metal oxides and the corre- sponding liquid metals In cases where several sur-face-tension determinations were available on the same substance, higher values were generally favored over lower ones because they usually indicate greater Sample purity. All of the metal-metal oxide pairs are in good agreement with Eq. [I] except for B-Bz03. The reason for the departure of this pair from the correlation is not understood. To estimate the surface tension of other liquid metal oxides the corresponding liquid-metal surface tension must be found. A nearly complete bibliography of the surface tension of liauid elements is available in the 46th edition of the Handbook of Chemistry and physics. Some additional references on metals are included here for convenience Se,26Sr,'?ThanduZ5). It is also possible to estimate the surface tension of a solid metal oxide or metal from the corresponding liquid-state data. As a liquid material is cooled through its melting point the surface tension increases abruptly by an amount Ao. bondi' has estimated that the maximum value of Aa at the melting point is Ao = Ahf/A [2] where Alzf is the heat of fusion per atom and A is the area per atom in the interface. Thus with heat of fusion and crystallographic data the surface tension of a solid at the melting point can be estimated as o + Ao.

Jan 1, 1967

Jan 1, 1967

By W. Buchanan, O. Johari

STEREOGRAPHIC projection has been one of the most useful aids in crystal-structure studies. With the increasing use of electron microscopy in metallurgy and other fields, stereographic projection is being used in many ways1 to interpret the results from electron diffraction patterns and transmission micrographs. For many of these applications, e.g., trace analysis, twinning, and so forth standard projections of various indices are required.

Jan 1, 1967

By L. K. Borrett ond C. S. Yusi

The authors have made extensive use of a modern field of mathematics, topology, to give a new approach to the study of sintering. They present a topological model for the sinter body and the void space, and establish a relationship between them. However, in an interdisciplinary paper of this nature it is important that the material be presented, insofar as possible, in

Jan 1, 1967

By R. T. Torgerson, W. A. Baginski

Alloying studies were conducted on modifications of Cb-10W-1OHf (C-129) alloy as part of a cooperative alloy development effort between The Boeing Co. and the Wah Chang Corp. The purpose of these studies was to develop a fabricable, high- strength columbium alloy with superior melding properties. The initial investigations of alloy modifications were conducted using laboratory-melted button ingots. An alloy with the composition exhibited excellent veld ductility, elevated-ternpevature strength, and fabricability. The yttrium-modified alloy was desigrzated C-129Y and was selected for further developrnetzt. Three prodziction heats of C-129Y weve processed into sheet. Welding, forming, and tensile proper-lies are presented for this material. Tungsten-are welds of. C-129Y exhibited a minimum bend radius of 1/2T in the as-welded conditioti compared to 8T for C-129 alloy. An investigation was conducted on Disil coating of C-129Y and test data are presented on oxidation resistance and effects of re-entry environments. The excellent combination of strength, fabricability, weldability, and low transition temperature of C-129Y alloy offers potential design advantages for use of this alloy in structures of aerospace vehicles. It is atiticipated that C-129Y will rapidly supplant C-129 and similar alloys clue to the versatility provided by its impvoved welditzg properties. COLUMBIUM alloys with improved properties are required to achieve better performance and efficiency of radiation-cooled structures for re-entry vehicles and recoverable launch systems. Cooperative work by The Boeing Co. and the Wah Chang Corp. resulted in the development several years ago of C-129 alloy, a high-strength Cb-W-Hf alloy.' This alloy has received favorable consideration for many advanced designs of high-temperature structures due to its excellent combination of properties. However, this alloy exhibits low weld ductility unless given a high-temperature stress-relief treatment. For this reason the development effort was directed towards modification of the C-129 alloy composition (Cb-1OW-1OHf) to eliminate the need for post-weld heat treatment. This paper describes the successful development of an alloy meeting this requirement. This new alloy was designated C-129Y and has a nominal composition of EXPERIMENTAL PROCEDURES Alloying Studies. Various Cb-W-Hf compositions were investigated using are-melted button ingots. These buttons were hot-forged using a protective glass coating and rolled into sheet specimens. Metal-lographic examination: tensile testing, and welding studies were conducted to evaluate properties of the experimental alloys. Sheet Fabrication. Three pilot production heats of C-129Y were fabricated into sheet to establish processing techniques and to determine sheet properties. The three heats consisted of 6-in.-diam ingots weighing from 140 to 250 lb. The ingots were prepared by electron-be am melting followed by vacuum-arc melting. The hafnium and yttrium additions were made during the are-melting operation by tack welding alloy strip additions to the Cb-W master-alloy electrode. The final ingots were machined into billets with samples of the machine turnings collected for chemical analysis. Ingot breakdown methods for the three heats are as follows: Ingot Ingot Heat Size Weiaht___Breakdown Method A 6 in. 250 lb Hot extrusion B 6 in. 140 lb Hot forging C 6 in. 250 lb Hot extrusion Sheet bars from the extrusion and forging operations were conditioned, recrystallized, and rolled into sheet. Initial rolling was conducted at elevated temperatures and final rolling was conducted at room temperature.

Jan 1, 1967

By E. Buehler, R. H. Willens

A Hew melting technique has hem adapted to the rapid quenching of- alloys from the liquid state. The inelting method has no limitations on the alloys investigated for there is no reaction with crucible materials and the most refractory materials are easily melted. The vate of heating is so rapid that alloys which have a high vapor pressure constituent can be melted with a minimal loss in material. Several new superconductovs have been discoveved by vapid quenching of lolten alloys. THE rapid quenching of alloys from the liquid state has led to the discovery of many new metastable phases. The methods initially used were limited to alloys which did not react with crucible materials.1,2 There was also the unmentioned limitation in tem- perature. Alloys with melting points much greater than 2000°C could not be melted in the rapid-quench apparatus. Recently, there have been successful attempts to rapidly quench reactive alloys by Moss et at. and Matthias Moss et al. injected powdered material (325 mesh) into a high-temperature plasma and the high-velocity molten droplets impinged on a cooled copper plate. The technique innovated by Matthias was to melt the alloy in an arc furnace and splatter it against a copper plate by means of a high-velocity gas jet aimed at the melt. I) FAST COOLING APPARATUS The creation of a metastable phase in a given alloy system by rapid cooling from the melt is contingent on the quenching rate. Some alloys require very slow rates while other alloys require the ultimate in quenching rate. At the present time, the vertical-gun technique of Duwez and willens' has demonstrated, in practice, the highest quenching rates and thus the best

Jan 1, 1967

By Nicholas J. Grant, John S. Benjamin

A series of composite alloys containing a high volume of NiAl, Ni3Ah or CoAl, bonded with 0 to 40 vol pct of a ductile metal phase, were prepared by powder blending and hot extrusion. The binder metals were of four types: pure nickel or cobalt, near saturated solid solutions of aluminum in nickel and cobalt, type 316 stainless steel, and niobium. Sound extrusions were obtained in almost all instances. Studied or measured were the following: interaction between the alunzinides and the binders, room-temperature modulus of rupture values, 1500° and 1800°F stress rupture properties, hardness, structure, and oxidation resistance. Stable structures can be produced for 1800°F exposure, with interesting high-temperature strength and good high-temperature ductility. Oxidation resistance was excellent. A large number of experimental investigations have been made of the role of structure on the properties of cermets and composite materials. Gurland,1 Kreimer et al.,2 and Gurland and Bardzil3 have indicated the preferred particle size in carbide base cermets to be about 1 µ, with a hard phase content of 60 to 80 vol pct. The optimum ductile binder thickness was noted to be 0.3 to 0.6 µ.1 Complete separation of the hard phase particles by the binder is important in reducing the severity of brittle fracture.' The purpose of the present study was to produce structures comparable to the conventional cermets, using a series of relatively close-packed intermetal-lic compounds rather than carbides as the refractory hard phase, and to study the effects of binder content and composition on both high- and low-temperature properties. The selected intermetallic compounds were particularly of interest because of the potential they offered in yielding room-temperature ductility. The highly symmetrical structures are known to possess high-temperature ductility and room-temperature toughness. Based on a ductile binder, the alloys were prepared by the powder-metallurgy route to avoid melting and subsequent alloying of the matrix, and were extruded at relatively low temperatures. It was expected that the composite alloy would retain useful ductility. In contrast, infiltration and high-temperature sintering led to alloying of the matrix and to decreased ductility. The systems Ni-A1 and Co-A1 were selected for this study. In the Ni-A1 system the compounds NiA1, having an ordered bcc B2 structure, and Ni3Al(?1), having an ordered fcc L12 structure, were chosen. In the system Co-A1 the intermetallic compound CoAl with an ordered bcc B2 structure was used. ALLOY PREPARATION The intermetallic compounds, see Table I, were prepared by using master alloys of Ni-A1 and CO-A1, with additions of either cobalt or nickel to achieve the desired compositions. The master alloy in crushed, homogenized form, was melted with pure nickel or cobalt in an inert atmosphere, cold copper crucible, nonconsumable tungsten arc furnace. The resultant intermetallic compounds were homogenized at 2192°C in argon, crushed, and dry ball-milled in a stainless mill to -100 and -325 mesh for the Ni-A1 compounds and to -325 mesh for the CoAl compound. Finer fractions were separated for some of the composite alloys. Several ductile binders were utilized. These included Inco B nickel, 5µ ; pure cobalt, 5 µ, from Sher-ritt Gordon Mines, Ltd.; fine (-325 mesh) niobium hydride powder; fine (15 µ) type 316 stainless-steel powder; and near-saturated Ni-A1 and Co-A1 solid-solution alloys, also in fine powder form. The niobium hydride was decomposed above about 700°C in processing of the compacts in vacuum to produce niobium powder. The Ni-7.1 pct A1 and the Co-5.3 pct A1 solid-solution alloys were prepared from pure nickel or cobalt and pure aluminum by nonconsumable tungsten arc melting under an inert atmosphere. The ingots were homogenized, lathe-turned to fine chips, and dry ball-milled in air to -325 mesh powder. These solid-solution alloys are designated NiSS and CoSS; see Table I. Subsequently the hard and ductile phases were dry ball-milled as a blend. Experiments clearly established the need to coat the hard particles with the ductile binder to optimize subsequent hot compaction by extrusion. Ordinary dry mixing usually resulted in nonhomogeneous alloys which were quite brittle. Conventional cermets are consolidated by liquid phase sinteiing or infiltration, which resulis in undesirable and uncontrolled alloying of the binder phase. For this study, a loose (unsintered) powder-extrusion process was emploved, minimizing reactions between binder and hard particle, thereby permitting much greater control of composition and structure. The constituent powders were first mixed in the desired

Jan 1, 1967