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By Robert A. Rapp, Ronald L. Pastorek

Solid-state electrochemical measurements by three alternative experimental procedures were made with the cell FeO, Fe3O4 |Zro.85Cao.15O1.85 |Cu| Zr0.85CaO.15O1.85 | FeO, Fe304 to establish the solubility and diffusivity of oxygen in solid copper in the temperature range 800" to 1030°C. The solubility of oxygen in solid copper and the diflusivity of oxygen in solid copper Dgu = 1.7 X 10-2 exp(-16,000/RT) Cm2/sec were determined and confirmed in alternative experiments. The enthalpy of solution of oxygen in solid copper equals —10,000 cal per mole; the partial excess entropy of the oxygen atoms in the Cu-O dilute solution is approximately the same as that found for interstitial atoms in other metals. The diffusivity of oxygen in solid copper is consistent with that expected for an interstitial atom. RELIABLE values for the saturation solubility N(s) and diffusivity DO of oxygen in solid copper have not been unambiguously established in the literature. Following three early determinations by others,1"3 Rhines and Mathewson4 reported that the solubility of oxygen in solid copper increased from 0.007 at. pct 0 at 600°C to about 0.015 pct at 1050°C. Phillips and skinner,, using essentiially the same analytical procedure, reported that the solid solubility increases from 0.0018 at. pct 0 at 550°C to about 0.0075 pct at 1050OC. The only previous value for the diffusivity of oxygen in solid copper was reported by Ransley.6 Ransley deoxidized Cu-Cu2O alloys in an atmosphere of carbon monoxide gas to yield a solubility-diffusivity product. He used the solubility data of Rhines and Mathewson to calculate the diffusivity values. Another method for obtaining the solubility-diffusivity product (N(s) DO) is by measuring the widths of internal-oxidation zones in copper alloys as reported by Verfurth and Rapp.7 However, the calculated N(S)Do products depend upon the alloy content of the specimen, so that the internal oxidation of copper alloys does not follow ideal internal oxidation kinetics. As a result, unequivocal values for the N(s) DO product were not obtained by this procedure. A solid-state coulometric titration technique similar to that employed in this work was introduced by C. Wagner8 to study the dependence on silver activity of the Ag/S ratio in silver sulfide in the temperature range of 160" to 300°C. Similar experiments have been carried out by C. Wagner and co-workers9-11 to study the stoichiometry range of silver and copper tellurides, cuprous sulfide, and cuprous selenide. Numerous authors have carried out electrochemical measurements with a solid oxygen-ion-conducting electrolyte to determine the solubility and/or diffusivity of dissolved oxygen in several liquid metals.12-l6 Rickert and Steiner17,18 have used solid-state electrochemical measurements to determine the diffusivity of oxygen in solid silver from 760" to 900°C. Two different cell geometries were used. In the cell of linear geometry Fe, FeO | ZrO2 + (CaO) | Ag + [0 (dissolved)] [1] oxygen diffused from the interior of the silver electrode to the silver/electrolyte interface where the oxygen activity had been lowered from a fixed initial value to practically zero by the application of voltage to the cell. The diffusivity of oxygen in solid silver was determined from the solution of the diffusion equation and the time dependence of the cell current. However, this determination of the diffusion coefficient depended upon a knowledge of the solubility of oxygen in solid silver. A cylindrical geometry was used for the cell Pt, O2(Po2 = 0.21 atm) | ZrO2 + (CaO) | Ag + [0 (dissolved)] [II] which also allowed the diffusivity of oxygen in solid silver to be determined. These values were in agreement with other available data.l9 Recently, Raleigh20,21 used a method involving the measurement of diffusion-limited currents in a cell involving the AgBr solid electrolyte to determine the diffusion coefficient of silver in Ag-Au alloys at 400°C. Diffusivity values on the order of l0-14 sq cm per sec were measured in the alloy composition range 10 to 60 at. pct Ag in a single experiment. From numerous electrical conductivity and galvanic cell measurements,9'22"26 the solid solution Zr0.85 Ca0.15 O1.85 has been established as an electrolyte with predominant oxygen ion conduction over a wide range of intermediate and high oxygen activities. For interrelating the thermodynamics and the kinetics of the dissolution of oxygen in solid copper in this investigation, a galvanic cell was constructed with FeO-Fe3O4 as the reversible reference electrode, the Zr0.85Ca0.15 O1.85 electrolyte, and a pure copper specimen under-saturated in oxygen as the other electrode. THEORETICAL ANALYSIS Three variations of a high-temperature electrochemical technique were used in this study to provide two determinations each of the solubility and diffusivity

Jan 1, 1970

By H. Y. Hunsicker

A graphic method has been devised for three-di-mensional analysis of hot deformation and for correlating the amount and directionality of the deformation with resulting directional properties. Deformation is evaluated in terms of dimensional change ratios referred to three orthogonal axes. Since all combinations of the three ratios can be represented in a triangular coordinate field with logarithmic scales, a two-dimensional chart of extent of deformation and degree of asymetry is possible. The entire gamut of shape changes from upsetting through flat-rolling to rod-rolling is accommodated. The resulting coordinate system is a base upon which can be represented the properties of the wrought products measured in the directions of the axes employed fir evaluating the deformation. When property data are available for many types and amounts of deformation, a three-dimensional figure can be constructed, and the projection of this figure is referred to as a ''3d'' chart. Experience in using such charts to plan fabricating operations for a variety of thick-section forged and rolled products of heat-treated aluminum alloys has verified its practical value for optimizing directionality relationships. MechANICAL anisotropy of thick section products of heat-treatable aluminum alloys is recognized by producers and users of these products, and the extent of the directional differences is apparent in property tabulations included in handbooks, standards, and specifications.' Attention has also been directed to the existence of important directional differences in the resistance of these products to stress-corrosion cracking. Metallurgical structure factors responsible for these directional differences include, among other possibilities, shape and alignment of grains, voids and nonmetallic inclusions (when present), volume fraction and spatial distribution of secondary phase particles and solid-state precipitates, crystal-lographic textures, and Bauschinger effect. The contributions of the individual factors vary with alloy composition, heat-treated temper, type of working process (forging, rolling, extrusion), and the amount and directional nature of the deformation. In general, the cast ingot used as the starting material for producing these wrought products exhibits only a modest degree of directionality. A monotonic and continuous transition from this nearly isotropic state with progressive hot deformation would appear probable, assuming that the working temperature is sufficiently high to cause continuous dynamic recovery. Several years ago a project was undertaken to evaluate the effects of hot deformation and metallurgical structures on the directionality of thick wrought aluminum alloy products, and the method to be described was developed as an analytical tool in this investigation. DIRECTION NOMENCLATURE The nomenclature system adopted by industry for the three mutually perpendicular directions employed in testing aluminum alloy products includes four terms: "longitudinal", "transverse", "long transverse", and "short transverse". These terms are conventionally related to the external geometry of the product but also by implication to the deformation and resulting metallurgical structure. Occasions arise in which through use of unusual fabricating methods, intentional or otherwise, the structure does not have the usual relationship to external geometry or may be very complex because of inhomogeneity of deformation throughout the piece. The longitudinal direction is generally parallel to the primary rolling direction or to the direction of extrusion. In the case of forging, it is parallel to the direction of maximum extension (not maximum "working" or "flow", as frequently stated). The term transverse is applied to any direction perpendicular to the longitudinal direction in a product having symmetry about the longitudinal axis, and generally, although not always, the deformation to produce these forms is nearly symmetrical in the transverse plane. This term then may be applied to a round, square, hexagon, or other polygonal, symmetrical shape produced by extrusion or rolling or by forging, if produced by a simple, symmetrical drawing procedure. The type of microstructure generally associated

Jan 1, 1970

By A. G. Darnley

"The Geological Survey of Canada is devoting consider-able effort to finding ways to make airborne radiometric measurements both quantitative and reproducible. Equipment has been designed by Atomic Energy of Canada Ltd. to provide high count rates in order to minimize statistical uncertainty, this being essential to justify applying terrain clearance and Compton scattering corrections to the data. Correction factors have been determined experimentally and can be applied automatically. Considerable ground work has been undertaken in parallel with equip-ment development in order to determine field parameters.Two airborne gamma-ray spectrometers are described. One is based on three 5-by 5-inch Nal(Tl) detector crystals and is used in a helicopter; the other employs twelve 9-by 9-inch detectors and is used from a Skyvan aircraft. The former is being used to investigate the range of radiometric response from specific rock types, and for the correlation of ground and air measurements; the latter has completed initial trials and will be commencing experimental surveys during 1969.Results are given to show the comparative sensitivities of the various detector sizes, and operational requirements for a gamma-ray spectrometer survey are discussed briefly."

Jan 1, 1970

"In response to needs created by intensive exploration and accelerating expansion of coal mining in the Western provinces, Canadian R & D on coal is progressively widening its scope. Principal interests continue to lie in coal geology, preparation and processing, carbonization, combustion and transportation, but much active work is also in progress with respect to mine environments, mined-land reclamation, and environmental consequences of coal mining, processing and use. Long-range 'basic' research, which characterized much of the R & D pattern in the fifties and early sixties and which was often no more than an attempt to prevent total extinction of a dying industry, has been somewhat de-emphasized, except insofar as it relates to 'safe' coal storage and to coal-based carbons (which are beginning to command attention as pollution control media).In this review, recent exploration, mine development and new preparation facilities are noted, and current R & D in transportation, processing, handling, carbonization and combustion is summarized. Reference is also made to investigations bearing on non-fuel uses of coal (notably as source-materials for carbons and agrobiological products)."

Jan 1, 1970

Jan 1, 1970

By H. J. Heinen

Malononitrile [CH2(CN)2J, which forms a carbanion in basic solutions, was investigated as a potential leachant for gold and was shown to be an effective extractant in alkaline pulps. Malononitrile was comparable to equal molar quantities of sodium cyanide (NaCN) in leaching gold from an oxide ore and yielded 10 to 20 percent higher recovery in leaching a refractory carbonaceous ore, although dissolution was slower with malononitrile than with cyanide. Complete recovery of the gold from the pregnant solutions was achieved by coprecipitation with a lead salt on zinc dust; the leachant was shown to be capable of regeneration and recycling a limited number of times. Addition of an anion-exchange resin to the carbonaceous pulp containing malononitri1e increased gold recovery from 67 to 95 percent. Some malononitrile derivatives were also shown to be gold solvents.

Jan 1, 1970

By F. Daniel Rosenkranz, Peter L. Silveston

Experiments investigating the treatment of a ground wood white water waste from an Ontario pulp and paper mill by an HVCB coal are reported. Adsorption capacity for the waste, with a soluble COD contribution of 2,100 mg/I, amounted to 0.17 per cent, by weight, of the Nova Scotia coal used. Percolation of the white water waste through a coal bed indicated that soluble COD is removed. For finely ground coals, over 90 per cent of the suspended solids in the waste are retained on the coal. Plugging of the coal bed is rapid, so that any treating process using filtration would have to renew the surface of the bed frequently.

Jan 1, 1970

The main orebody of the Bodangora mine is a metalliferous quartz reef within a major fault plane in the strongly folded and faulted volcanic rocks of the Ordovician-Silurian Oakdale Formation. The similarity of the type of mineralization to that of other pyrometasomatic deposits in this area suggests that the mineralizing fluids originated in the nearby Wuuluman Granite.The associated Mitchell's Creek West or Dick's reef is discussed briefly.

Jan 1, 1970

By John Nagy

Large-scale tests in the U.S. Bureau of Mines Experimental Coal Mine show that the explosion hazard of coal dust on shuttle-car roadways can be con-trolled by proper application of water, dry rock dust, a saturated solution of ammonium phosphate, or mixtures of water or the water-phosphate solution with rock dust. The experiments were made with loadings of 1.0 and 5.0 pounds of mine size coal dust per linear foot of entry, and with a 3-or 4-inch-thick layer of coal rubble on the floor, The data from the tests with mine-size coal and rubble are comparable. The water contents of the dust loading were determined from samples collected just prior to initiation of a gas-air mixture in an ignition zone at the face Dust samples were collected 1 inch deep from the coal-rubble deposit. One experiment was made with the dust in the coal rubble bound with latex applied as a water solution by spray. The binding action was inadequate and explosion propagation was obtained.

Jan 1, 1970

By L. R. Raymond

With the trend toward deeper and consequently hotter holes, measurements of drilling mud properties at atmospheric temperatures are becoming increasingly inadequate.' Both the prediction and control of down-hole mud properties depend in part upon our knowledge of temperatures in the wellbore. Consequently, a better understanding of factors that affect temperatures during circulation and trips could improve drilling operations. It was toward the goal of obtaining this understanding that this study was directed. Other investigators2 have studied the response of fluid temperature in the borehole during trips. However, all of these studies have used an assumed formation temperature profile at the conclusion of circulation and have provided no means to calculate this profile directly. In this study, the formation profile during circulation was calculated. Other investiga-tors3-5 have also studied bottom-hole temperature during circulation. However, they have developed neither general techniques for calculating the entire temperature profile in the system nor generalized methods for predicting bottom-hole fluid temperatures during circulation. Such techniques and methods have been developed and are discussed briefly in the following pages. Temperature Behavior During Circulation Circulation of fluid during the drilling operation is represented schematically in Fig. 1. The process of circulation has three distinct phases: (1) fluid enters the drill pipe at the surface and passes down the drill pipe; (2) fluid exits the drill pipe through the bit and enters the annulus at the bottom; and (3) fluid passes up the annulus and exits the annulus at the surface. To simulate the thermal behavior of the fluid in the system, each of the phases of circulation must be described mathematically. In Phase 1, the fluid enters the drill pipe at a specified temperature, TDo. As the fluid passes down the pipe, its temperature is determined by the rate of heat convection down the drill pipe, the rate of heat exchange between the drill pipe and the annulus, and time. Phase 2 of the circulating process merely requires that the fluid temperature at the exit of the drill pipe be the same as the fluid temperature at the entrance of the annulus; i.e., TD(L,t) = TA(L,l). Thus in Phase 3, the fluid enters the annulus at TD(L, t). As the fluid flows up the annulus, its temperature is determined by the rate of heat convection up the annulus, the rate of heat exchange between the annulus and the drill pipe, the rate of heat exchange between the formation adjacent to the annulus and the fluid in the annulus, and time. These rates of heat exchange and the time dependency of mud temperature are described by well known heat-flow equation.6 Consequently, as shown in the Appendix, the temperature profiles in the drill pipe, annulus, and formation can be obtained by solving Eqs. 1 through

Jan 1, 1970

By H. J. Levinstein, H. J. Guggenheim

RbFeF3 is a transparent ferromagnet with a large faraday rotation which permits the direct observation of magnetic domain structures in bulk crystals. If the position of dislocations within the crystal were known a study of domain wall dislocation interactions would be possible. In this paper an etch pitting solution is described which gives a one-one correspondent between the etch pits and the dislocations intersecting the (100) surfaces of RbFeF3 crystals. In addition, RbFeF3 is shown to have sufficient plasticity so that known arrays of dislocaticms can be put into the crystal. It is concluded that RbFeF, is an ideal material for the investigation of domain wall dislocation interactions. THE influence of lattice defects on the motion of domain walls in ferromagnetic materials has been studied extensively both theoretically and experimentally.4 The experimental data obtained has been qualitative in nature due to the lack either of a quantitative knowledge of the magnetic domain array in the material or of the nature of the dislocation configuration in the material. At room temperature RbFeFJ has the cubic perovskite structure. It is ferromagnetic below 86°K.5,6 It is also transparent and has a large faraday rotation in the magnetic state.7 The domain structure of this material is observable in three dimensions in crystals which are millimeters in thickness.' Since RbFeF3 satisfies the requirements of having an easily visible three-dimensional magnetic domain structure, it was of interest to determine if the dislocation structure of the material could be determined and if the material was sufficiently plastic so that dislocations could be introduced into the as grown crystals. This is a report of the results of that investigation. EXPERIMENTAL PROCEDURE The crystals of RbFeFs used in this experiment were grown by a technique described elsewhere.5 In order to obtain flat strain-free surfaces, the samples were first cut to the crystal orientation desired and the surfaces were polished by employing standard metallographic techniques. The samples were then immersed in a solution of 1 to 3 g of KOH in 100 ml of water. This solution removes the damaged surface layers uniformly leaving a film on the surface of the sample. Etch pits are obtained by immersing the sample in an approximately 50-50 solution of 30 pct peroxide and concentrated acetic acid. The film formed during the KOH treatment turns deep red in color in the etching solution and flakes off the sample. The etching time required depends upon the pit size desired and

Jan 1, 1970

By Dipl. -Ing. Mertens

Gentlemen: I am pleased and regard it as a priviledge to give you a report on rapid roadheading with heading machines in the coal mining industry of Western Germany. Importance of Heading Operations in the West German Coal Mining Industry Every year about 770 km of headings are driven In the seams of the West German coal mines, most of them gate roads, the rest rise headings, to open new faces. In thick seams the heading operations are carried out entirely in the coal, in thin seams the country rock has to be ripped. The total length of 770 km corresponds to a rock volume of roughly 9.5 million m3; this figure underlines the importance of the heading operations in the coal mining industry of our country.

Jan 1, 1970

Jan 1, 1970

By Stewart WJ

Australia's first offshsore well was spudded in on 27th December 1964 and resulted in the discovery of the Barracouta gas field. Further exploratory drilling led to the discovery of the Marlin gas field in December 1965, the Kingfish oil field in April 1967 and the Hblibut oil field in June. 1967. In September 1968, a small oil reservoir was found in a sand below the main Barracouta'gas reservoir. The Snapper gas field was discovered in May, 1968 Information on exploration activities associated with the discovery of oil and gas in the Bass Strait area may be found in the paper, "Exploration in the Gippsland, Bass and Otway Basins, Australia" by B. M. Hopkins. _ Development of the commercial fields is being undertaken on an equal participation basis by Hematite Petroleum Pty. Ltd. and Esso Exploration and Production Australia Inc. Esso Standard Oil (Australia) Ltd. is responsible for the design, construction and operation of the production facilities.

Jan 1, 1970

By C. E. Capes

The spherical agglomeration process provides an attractive method for the cleaning and recovery of fine coals in the form of compact oil-bonded pellets. In treating a washery effluent containing 50% minus 20 micron material by this technique, the slurry was first mixed under vigorous agitation with oil to deash and dewater the fine coal. The flocculated coal pulp was then formed into larger agglomerates on a modified balling disc. The operation of a semi-pilot scale process is described and an analysis of some of the operating and system variables is given. A semi-theoretical expression to predict the final agglomerate size under various conditions is derived and compared with the experimental data. Coal producers are faced with a growing requirement to clean and recover fine mesh coals. Greater mechanization of the extractive and preparation processes has resulted in finer-sized products containing larger quantities of associated foreign matter and preparation plant effluents contain quantities of fine coals which are potentially valuable. These losses will probably increase with the expansion of production and will require the development of effective disposal and utilization processes under pressure of the lack of adequate disposal areas, the enforcement of air and stream pollution laws, and the economic need to obtain the maximum yield of salable product(1)

Jan 1, 1970

By M. A. Bergougnou, I. Inculet, K. I. Burgess

This paper describes the electrostatic methods of separating various minerals, reviews the principles of fluidization and outlines the technique of electrostatic sorting in fluidized beds. The application of the method to the benefication of coal is emphasized.

Jan 1, 1970

By D. R. Parrish, F. F. Craig

In some respects, forward combustion (alias: fie-flooding, underground combustion, in-situ combustion, dry combustion) is an efficient oil recovery method. For example, its displacement efficiency (as much as 95 percent in reservoirs with high porosity and high oil saturation) is good. In its use of heat, however, forward combustion is grossly inefficient. Most of the heat generated during forward combustion is wasted. About one-fifth of the heat is picked up by the incoming air and re-used (regenerated); the remainder is left behind the combustion zone and ultimately is lost. Compressed air is expensive, and heat generated from compressed air via underground combustion is too valuable to be thrown away. Improvement is needed. Since the early 1950's, improvements in forward combustion by addition of water injection have been discussed, particularly in the patent literature, with increasing frequency.'-'' These concepts are based on the fact that relatively inexpensive water can be used to pick up much of the heat that is ordinarily wasted during forward combustion, and transport it forward to a more useful place, thereby reducing the amount of air required to move a heat front through the reservoir. Several approaches have been proposed. Merriam and Squires1 taught that a combustible (fuel) gas should be injected along with the air and water. This, however, would give at least a tendency toward reverse combustion instead of forward combustion, and would reduce the velocity of the heat bank, defeating the primary purpose of the water injection. Pelzer2 described primarily a batchwise method of forward combustion and water flooding. He advocated burning part way through a reservoir with forward combustion, then switching from air to water injection alone to push the heat toward the producing wells. Though possible, this method has serious disadvantages, the major one being that, by the time water injection is started, much of the heat has been irretrievably lost to the overlying and underlying formations. We have described what is considered a practical Combination Of Forward Combustion And Water-flooding (COFCAW).3,4 Air and water are injected simultaneously (or alternately) after a small heat bank has been formed by forward combustion. Some of the injected fluid fills up the region behind the heat bank; the rest enters the heat bank. Upon encountering heated rock, the water is converted into steam, which then flows ahead of the combustion zone and displaces much of the oil in place. Only enough air is injected to provide heat for vaporization of the water and to compensate for reservoir heat losses. Since the size of the heat bank is minimized, heat losses also are minimized. Because of more efficient oil displacement ahead of the combustion zone, fuel consumption is reduced. Too, unlike a forward combustion zone that cannot move until all fuel at a point has been consumed, COFCAW leaves some

Jan 1, 1970

By R. P. Harvey, J. E. Walstrom, A. A. Brown

In view of the large number of wells directionally drilled from offshore platforms and urban drillsites, greater interest is being focused on the directional survey and on the uncertainty inherent in calculating the position of the bottom of the hole, or other benchmarks in the wellbore. Of the two methods presented here for evaluating this uncertainty, the first is analytical and uses the principles of probability and statistics. The second method uses Monte Carlo simulation to generate a pattern of the scatter of possible bottom-hole locations. Both methods are based on a model for which the usual assumption is made that the curvilinear axis of the wellbore is adequately represented by a large number, M, of linear segments joined end to end from the top to the bottom of the hole and closely following the course of the hole. The errors due to this approximation are assumed to be negligible and are not studied here. One form of the model is to consider that for a given hole there exists a perfect set of data describing it, of the above form. Each linear segment has an angle of inclination with the vertical 7, in radians, an azimuthal angle from true north xi in radians, and a length Si, in feet. The subscript variable, i, extends from 1 to M. Each of the M linear segments representing the axis of the wellbore has three components in the X, Y, and Z directions. These components are calculated from the equations: The bottom-hole coordinates as determined from the reference set of data for the wellbore are given by the following for i = 1 to M: X=SX, Y = Sy, Z=SZ; . (2) A directional survey instrument, lowered into the wellbore to the M segments, or stations, measures the values of the 7; and the 3,. In general, because of errors from various sources, the resulting angular measurements will not be precisely equal to the 7" and xi. Random variables l, and Ai are therefore considered with associated probability density functions fi(li) and gi(Ai), respectively, which represent the distributions of potential survey measurements for this hole. Since it is assumed that the values Si are accurately measured they are treated deterministically. The random variables corresponding to the surveyed bottom-hole coordinates are given, for i = 1 to M, by:

Jan 1, 1970

By R. S. Kinasevich

As part of other work related to the studies of kinetic factors that influence the flotation of specific sulphide minerals, specially designed kinetic flotation experiments at Cominco included work done on -65 + 100 mesh and -100 + 150 mesh, high purity galena. The flotation collector used was sodium isopropyl xanthate containing radioactive sulphur-35. Radiation monitoring of the galena fractions from stage flotation tests indicated that the adsorbed radioactive xanthate was uniformly distributed among the floated fractions and the non-floated, or residual portion of the galena. This anomalous behaviour could not be correlated to changes in Seebeck coefficients, to lattice distortions, or to the nature of the mineral surface as revealed by infrared spectroscopy and by microscopic measurements.

Jan 1, 1970

By Å. Sterten, R. Tunold, J. Brun, K. Dalatun

c axis compression behavior of beryllium single crystals at three purity levels under hydrostatic pressures up to 27 kbars was determined. Extensive non-basal slip, observed by two-surface trace analysis and transmission electron microscopy, occurred under a hydrostatic pressure of about 12 kbars (175 ksi) for the high-purity (twelve-zone pass) material and at about 19 kbar (275 ksi) for the lower-purity (zone-leveled) material. Prismatic loops with a (c + a) Burgers vector were observed in association with second-phase parti- A principal factor limiting the use of beryllium is its brittle behavior when tested at the usual strain rates (E = 10-4 sec- 1) at temperatures below about 200°C and under impact conditions at temperatures in excess of 200°C. It has been proposed' that the brittle-ness of beryllium is associated with the lack of a sufficient number of independent slip modes and the absence of a slip mode with a Burgers vector out of the basal plane [presumably (c + a) pyramidal slip mode] and to the ease with which beryllium cleaves on the basal and second-order prism planes. The absence of pyramidal slip has been attributed to a high Peierls-Nabarro stress associated with the motion of dislocations with a (c + a) vector and the ease with which cleavage occurs on the basal and second-order prism planes. The experimental evidence in support of the proposed explanation for the brittleness of beryllium is far from complete; for example, that the ductile-to-brittle transition in polycrystalline beryllium is associated with the operation of profuse (C + a) slip has not been unequivocally established. The occurrence of (c + a) slip ({1122}(1123)) has been experimentally established2-5 under conditions where basal and prism cleavage are restricted in a c axis compression test. In these investigations (C +a) slip was found in high-purity beryllium single crystals tested in c axis compression* at 200°C and in Be-4.4 pct Cu and Be-5.2 pct cles in the lower-purity materials tested. The loops were related to surface "extrusions" observed on many of these same specimens. Nonbasal dislocations operating on (1122) planes with a (c + a) Burgers vector were observed. The presence of c and a dislocations together with (c + a) dislocations suggests that the (c + a) dislocations dissociate presumably on unloading or after failure of the test crystals to c and a dislocations. terial, (c + a) slip has only been observed near the the fracture4 surface in room-temperature c axis compression tests. Fracture in these tests occurs without measurable plastic flow, as determined with a strain sensitivity of 10"6. Since it has been shown for many metals that the application of hydrostatic pressure suppresses fracture,?-' it was felt that studying the behavior of unalloyed beryllium single crystals stressed in c axis compression under a hydrostatic pressure would reveal whether (c + a) can occur if fracture was prevented, and that it might elucidate the role of (c + a) slip in the ductile to brittle transition. Evidence that (C + a) slip is associated with increased ductility in a high-pressure environment has been found in stress-strain tests on poly crystalline beryllium.10 The present paper describes a study on the influence of a hydrostatic pressure environment on the occurrence of (c + a) slip in beryllium single crystals. Material of two purity levels was tested in c axis compression over the pressure range ambient to about 27.5 kbars.* 1) MATERIAL PREPARATION AND CHARACTERIZATION Two lots of low-purity single-crystal beryllium were used. The first lot was "ingot secondary refined grade" and designated lot A. The second lot (lot B) was produced by a two floating zone pass zone-leveling operation in an argon-filled sealed quartz apparatus on a 1-in.-diam by 12-in.-long bar of Pechiney secondary refined-grade vacuum-cast and hot-extruded material. The high-purity material (lot C) was made by traversing twelve floating zone passes through a similar bar of Pechiney secondary refined-grade vacuum-cast and hot-extruded material. In a series of spark cutting and lapping procedures,11 single-. crystal specimens some 0.12 in. sq by 0.30 in. high were made with the sides Parallel to the first- and second-order prism planes and the basal plane within 3' of arc of the top and bottom surfaces of the specimen. Such an accurate orientation is necessary because of the large difference in resolved shear stress

Jan 1, 1970