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By R. L. Stephenson

The effect of fabrication variables on the creep-rupture properties of TZM (Mo-0.5 pct Ti-0.08 pct Zr-0.03 pct C), Cb-TZM [columbium-modified TZM (7140-1.5 pct Nb-0.5 pct Ti-0.8 pct Zr-0.05 pct C)], and TZC (Mo-1.2 pct Ti-0.25 pct Zr-0.15 pct C) has been studied at 982º. 1093º, 1204º, and 1315°C for rupture times up to 1000 hr. The creep tests were performed in vacuum creep furnaces, employing cold-trapped oil-diffusion pumps, operating at pressures 2 X 10-7 tory. After-test chemical analyses showed no significant changes in interstitial content. The creep-rupture properties of TZM, fabricated according to current mill practice, were determined in the stress-relieved and in the re crystallized conditions to provide control data. Specimens of TZM, Cb-TZM, and TZC fabricated according to each of two experimental fabrication schedules were then tested. The schedules differed in terms of in-process annealing temperatures and warm -working temperatures. The data make several conclusions evident. Fabrication variables do indeed have a profound effect on the long-time creep-rupture properties of molybdenum alloys. Strengths of these alloys compare very favorably with those of other refractory metal alloys in the temperature range studied. FOR several years we have been engaged in the evaluation of the creep-rupture properties of promising refractory metal alloys. We consider the determination of these properties to 1000 hr at several temperatures necessary for a valid comparison. Such an evaluation indicated that the creep strengths of Mo-0.5 pct Ti and TZM (Mo-0.5 pct Ti-0.08 pct Zr-0.03 pct C) compare favorably with those of other refractory metal alloys. Tensile and recrystallization data of other investigators1,2 show an effect of fabrication variables. More specifically, those fabrication schedules which produce high strength through work hardening exhibit the least thermal stability. A similar conclusion was reported by perkins3 for Cb-TZM. This would lead one to expect that, in terms of creep, those materials showing higher strength at short times and low temperatures would exhibit lower strength at long times and high temperatures. If these expectations were fact, a substantial improvement could be made in these alloys by optimizing their fabrication schedule in terms of their anticipated service temperature. We therefore undertook a study of the effect of fabrication variables on the long-time creep properties of TZM, Cb-TZM (Mo-1.5 pct Cb-0.5 pct Ti-0.08 pct Zr-0.05pct C) and TZC (Mo-1.2 pct Ti-0.25 pct Zr-0.15 pct C). MATERIALS All materials used were supplied by the Climax Molybdenum Co. of Mich. Our original intention was to test the same heat of each alloy in different conditions. Fabrication difficulties prevented this; however, heats with nearly identical analysis were selected. The compositions of the materials used are listed in Table I. All materials were supplied in the

Jan 1, 1970

By J. R. Cahoon, H. W. Paxton

The possibility of using unidirectionally solidified, two-phase alloys as an approximation to fiber composite materials is investigated. The short-term me.chanical properties and failure modes of unidirectionully solidified A1 (rich)-Cu alloys containing ap -Proximately 0, 17.5, and 27.7 vol pct of 0 phase 'fibers" are determined at temperatures from 25" to 500" and compared with those obtained for conventionul SAP alloys. In a previous publication,' hereafter referred to as I, the possibility of understanding some of the room-temperature mechanical properties of unidirectionally solidified castings was explored. For Al(rich)-Cu and Al(rich)-Mg two-phase alloys over a substantial range of compositions, the yield and ultimate strengths and common ductility measures were very adequately predicted from the principles of fiber strengthening4 and the analysis of ductility outlined by Gurland and Plateau." The results obtained in I suggest the possibility of using unidirectionally solidified, two-phase alloys to simulate fiber composite materials where the inter-dendritic second phase or constituent acts as the reinforcing material. Recent attempts concerning the fabrication of fiber conlposites have concentrated on producing composites with a good bond between fiber and matrix and with very long fibers so that their maximum contribution to the strength of the composite may be realized. However, these objectives are difficult to attain in practice and present fabrication processes are either extremely laborious or costly.13 The slow, unidirectional solidification of eutectics has received considerable attention as a method for producing composite materials. 5,6 This method can fulfill both of the above objectives but it is currently laborious, expensive, and has the additional disadvantage that the volume fraction of reinforcing phase cannot be easily varied. On the other hand, unidirectionally solidified, two-phase alloys, also with a good bond between the phases, are relatively easy to make and the volume fraction of reinforcing "fibers" can be easily varied by changing the average composition of the alloy. The disadvantage of the cast alloys is that the mechanical effectiveness of the "elongated interdendritic reinforcements" (EIR)* may be reduced due to their rela- tively short lengths, the w factor in Eq. [2] of I. However, if the EIR have a high strength their contribution can be considerable. For composite materials containing discontinuous cylindrical fibers of various lengths the ultimate strength is given by1 where it is assumed that the composite fractures when the fibers fail. In Eq. [I], a, is the stress in the matrix just prior to failure of the composite, Vf is the total volume fraction of fiber reinforcing constituent, Vf(l+) is the volume fraction of fibers whose lengths exceed the critical length, I,, which is defined as the shortest length of fiber in which the stress can build up sufficiently to break the fiber. af is the fracture strength of the fiber material, w is a factor accounting for the discontinuity of those fibers whose lengths exceed I,, 1-/d is the average aspect ratio of those fibers whose lengths are shorter than I,, and t is the shear stress in the matrix at the fiber-matrix interface. The factor w is dependent on the length of the fibers and also on whether deformation of the matrix occurs plastically or elastically. However, for a given length of fiber, w is smaller when elastic deformation of the matrix is assumed.' It is of interest to consider the properties of simple unidirectionally solidified, two-phase alloys at elevated temperatures in view of the possibility of using suitable modifications for high temperature service. Knowledge of the creep behavior of these materials is still rudimentary (although under active investigation) and the present paper concerns itself with short time tensile properties of some alloys similar to those investigated in I (i.e., unidirectionally solidified Al(rich)-Cu alloys). Unidirectionally solidified alloys containing 5.6, 17, and 23 wt pct Cu were tested parallel to the direction of solidification at temperatures from 25" to 500°C. In the present investigation, the alloys were homogenized for 2 days at 535°C giving a matrix of homogeneous a phase (5.2 wt pct Cu) and an interdendritic constituent (EIR) which was completely Q phase (53 wt pct Cu). EXPERIMENTAL Alloys of nominal composition 5.6, 17, and 23 wt pct Cu (containing approximately 0, 17.5, and 27.7 vol pct 8 phase, respectively, after homogenization at 535°C) were prepared by melting 1200 g of A1 (99.99 pct) in a high purity graphite crucible and adding the appropriate amount of freshly cleaned copper chips (99.9 pct). The molten alloy (at 700°C) was poured into a preheated graphite mold (also at 700°C) and the ingot unidirectionally solidified by impinging water on the steel baseplate of the mold. The alloy was degassed immediately

Jan 1, 1970

By W. S. Sanner

Pyrolysis (destructive distillation) techniques developed at the Bureau of Mines to determine the yield and quality of the products from coal were used to convert municipal (household) and industrial refuse into potentially useful solids, liquids, and gases without adding to environmental pollution. The tests demonstrated that a ton of municipal refuse can be converted into 154 to 424 pounds of solid residue, 0.5 to 6 gallons of tar, 1 to 4 gallons of light oil, 97 to 133 gallons of liquor, 16 to 32 pounds of ammonium sulfate, and 7,380 to 18,058 cubic feet of gas. A ton of industrial refuse, consisting of paper, rags, and cardboard, can be converted to 618 to 838 pounds of residue, 1.5 to 3 gallons of light oil, 68 to 75 gallons of liquor, 12 to 23 pounds of ammonium sulfate, and 9,270 to 14,065 cubic feet of gas. The energy from the gas is more than sufficient to provide the heat for the pyrolysis.

Jan 1, 1970

By George C. Coupland

Ecstall Mining Limited, a wholly owned subsidiary of Texas Gulf Sulphur Company, is the owner and operator of the Kidd Creek Mine including the concentrator complex located near Timmins, Ontario. Canada, approximately 450 miles north of Toronto. The mine, concentrator and Timmins form a triangular arrangement with a 17-mile rail link connecting the mine and concentrator and both of these facilities 18 and 14 miles respectively by road from Timmins. A core drilling program in the spring of 1964 established the presence of a large massive sulphide orebody which was to become the Kidd Creek Mine. Texas Gulf Sulphur had been conducting an intensive search for base metal in various parts of Northern Ontario and Quebec since 1957. Of several thousand anomalies detected in airborne electromagnetic surveys, several hundred warranted ground inspection, but only one of more than sixty drilled became a commercial orebody, the Kidd Creek Mine. The geophysical exploration work has been well covered in a paper written and presented by Van Donohoo, presently a Vice-President of T.G.S., at the American Mining Congress in San Francisco in October 1969. GEOLOGY The orebody lies within a series of overturned rhyolitic flows and pyroelastics with a major peridotite intrusive to the east. The hangingwall and footwall are composed chiefly of intermediate volcanics, andesite and dacite. The southern end of the orebody appears to terminate abruptly against greywacke while the north end is bifurcated and the structure obscured.

Jan 1, 1970

By William T. Barrett

It is said that Thales of Miletus, 600 B.C.,1 was aware of the attraction of lodestone toward iron and highly magnetic minerals. However, the birth of magnetic concentration followed shortly after the invention of the first electromagnet by Sturgeon in 1825. Sturgeon's magnet was described in the annals of electricity.2 The first attempts to concentrate minerals by the use of magnets date back to about 18473 but the first commercial drum-concentrator was apparently invented by R. Cook in 1849. Credit must also be given to the invention of P. Righter's machine in 1867,5 and to the highly successful Wenström separator devised in Sweden in 1883.8 Since the advent of these early separators there have been virtually hundreds of patents granted covering minor modifications of drum-type magnetic separators. The more important advances from a technological viewpoint have been the design of stable power supplies for d.c. magnets, the advent of ceramic permanent magnets which are now replacing electromagnets for the concentration of ferromagnetic minerals, and advances in general magnet and machine configurations.7 One of the problems facing both the designer and the user of magnetic separators is the evaluation of the body forces acting on particles in the magnetic field of the separator. Perhaps the most elegant method of evaluating the body force associated with a drum-type magnetic separator is that recently suggested by W. F. Brown.8 Brown measures the radial component of the field intensity one-half inch from the drum surface and fits a Fourier series in the angle about the drum axis (Figure 1). Once the coefficients of the series are known, it is then possible to calculate [ ]

Jan 1, 1970

By William E. Bruce

Percussive drill calibration experiments performed by the Bureau of Mines on two drills are described. The use of a linear velocity transducer to determine piston velocity, blow frequency, and piston stroke length is discussed. Data are presented on the relationships between maximum work rate and feed air pressure. Penetration rates in nine rock types were measured for the same two drills. Physical properties of the nine rock types are presented in tabular and graphical form to show relationships between penetration rates and physical properties. Finally, conclusions are drawn as to the potential use of these data to predict percussive drilling rates.

Jan 1, 1970

By Wendell H. Nielson

Flotation processes contain disturbances which make material balance closures difficult to achieve. Lack of closure also arises from instrument errors. A portion of these problems can be overcome by proper equipment selection; the primary measurement installation and methods of initial data filtering are discussed below. The problem of data adjustment has been considered before (2). The technique described here is essentially that of Ripps (2). The technique was expanded to include linearization of non-linear material balance equations. An additional large error detection portion was also added to Ripp's formulation. Ripp's technique is based on a Lagrange-Multiplier optimization method. The Lagrange-Multiplier technique is generally applied when there are equality constraints on the variables. Steady-state material balance equations fit in this category. The basic Lagrange-Multiplier method is described. It is followed by a description of the modified material balance data adjustment technique. An example is presented to illustrate the use of this method.

Jan 1, 1970

By Eugene F. Casey

An immersed tube tunnel is one which is composed of elements that are prefabricated in a dry dock or on shipways, usually away from the actual tunnel site, floated into position and then lowered into a preexcavated and graded trench below a body of water. The elements or segments are then connected to each other under water, and the entire immersed tube tunnel covered with a protective blanket. Because water is essential, this method of construction offers advantages in a relatively limited field. By the very nature of the method, lowering elements to the bottom of an underwater trench, immersed tube tunnels are primarily used for crossing bodies of water, such as rivers, bays, straits, canals, etc. Although this method of construction was first used for a subaqueous railway crossing under the Detroit River in 1906-1910 and again in 1912-1915, for a four track subway tunnel under the Harlem River in New York, the reason immersed tube tunnels construction has not been used more extensively is simply a matter of economics. Bridges, compressed air tunnels and similar structures could be constructed at a lower cost.

Jan 1, 1970

By R. B. Schluter, M. M. Fine

Development of a process for winning copper from pelletized chalcocite concentrate is underway at the Bureau of Mines, Twin Cities Metallurgy Research Center. The new route from concentrate to metal by which the Bureau seeks to eliminate matte smelting and converting includes a two-stage fluid bed treatment. In the first stage, pelletized concentrate containing 32%Cu and 7% S is first desulfurized to less than 1.0% S in an oxidizing atmosphere. In the second stage, the calcine is metallized by reduction with hydrogen. Thereafter, the reduced product plus 10% CaO is routed to a smelting furnace which separates metallic copper from the gangue. Recovery and Cu content at this point are in the 97-98% range. This product must be refined to remove sulfur and iron so the metal is suitable for making wirebar copper. An important feature of the process is fine concentrate pelletization prior to fluid-bed treatment. This permits a shorter reaction time, a decrease in dusting and easier subsequent processing. In a broad sense, sulfide copper pyrometallurgy is a batch sequence in three separate vessels, i.e., a reverberatory furnace to yield matte copper, a converter to produce blister copper and another reverberatory furnace to produce fire-refined copper. Matte-smelting has remained relatively unchanged since it became a universal practice some 50 to 60 years ago. It is now serving a wide range of smelter feed materials, but many concentrates are not immediately amenable to the process. There are abundant copper resources which lack sufficient sulfur and other elements lo sustain the full chemistry involved in matte-smelting. This necessitates adding sulfur to make the product fit the process, and usually none of the sulfur is recovered. From the standpoint of pollution alone, the development of a smelting technique for low-sulfur concentrates not requiring the addition of sulfur would be a significant gain.

Jan 1, 1970

By E. I. Gordon

The electronic pickup tube is the image-to-video signal-converter or transducer in tele vision-like systems. Images may relate to visible light or IR excitation as in conventional TV systems, X-ray excitation as in some medical and production control applications, or electron excitation as in electron microscopy. The latter process is also important in some forms of light or X-ray sensitive pickup tubes as an intermediate step. In virtually all of these devices the image ends up as a stored charge pattern on a suitable target electrode and the video signal is created by periodically scanning the target with a low energy electron beam and removing the stored charge. In a major group of tubes radiation induced conductivity creates the charge pattern. In others, photoemission is used. In this paper an attempt is made to illuminate some of the device requirements placed on materials exhibiting radiation induced conductivity, some of the materials and techniques that are used, and the problems. The emphasis will be on visible light and IR sensitive targets although some attention will be given to X-ray and electron imaging. Photoconducting films as well as diode arrays will be discussed. ELECTRONIC pickup tubes find their greatest use in commercial, entertainment television, and in industrial and educational closed-circuit television. Video telephone systems, such as AT&T's PICTURE-PHONE System will become eventually the greatest user. Military use is also very important. Nevertheless the use of electronic pickup tubes in technology, science, and medicine is assuming ever greater relevance and demands the greatest diversity and perfection in the pickup tube art. Commercial television and closed-circuit television use requires visible light response, high resolution, low lag, and uniform response. Video telephone use requires the same plus extreme reliability, stability, and low cost. Military use emphasizes, in addition, sensitivity, IR response, and ruggedness. (Devices for far IR response will not be considered here.) The use of pickup tubes in medicine and biology emphasizes UV response for microscopy, X-ray response for radiology, and energetic electron response for electron microscopy. Astronomy and nuclear physics demands low light level response, storage ability, and resolution (here the tube is a successful replacement for film). The interested reader might profitably read Advances in Electronics and Electron Physics, vol. 12,' 16,2 and 22A3 and 22B4 for detailed discussion of the use, properties, and technology of electronic pickup tubes. In general, because of the importance of these uses, none of the above properties will be ignored. Nevertheless attention will be restricted to only those imaging devices, called pickup tubes, using a scanning electron beam to dissect the image with a resulting video signal for conventional CRT display. However pickup tubes have become so complex that many of them include components such as image in-tensifiers which would be normally excluded by this restriction. Thus some of the other imaging devices will not be ignored entirely. We will first review the fundamental elements and physical phenomena involved in modern electronic pickup tubes, then the relevant materials and some of the material problems and then an interesting goal yet to be achieved. REVIEW OF PICKUP TUBE PRINCIPLES In all modern television systems using pickup tubes there is an interval called the frame interval, during which the incoming radiation flux is allowed to produce a cumulative effect in the form of a stored charge pattern which is a replica of the radiation image, and a scan interval during which the stored charge pattern is converted into a video signal. The frame interval bears no fixed relation to the scan interval and may be shorter or longer. In conventional, real time television the scan interval including retrace is identical to the frame interval. Integration and storage is the key to the sensitivity of modern pickup tubes, in contrast to earlier tubes such as the image dissector. At equivalent light levels and without integration, the number of photons contributing to the video signal in the image dissector is lower by a factor approximating the number of picture elements in the displayed image, a number of order 10. Statistical fluctuations in the number of contributing photons represent a serious limitation to the attainable signal to noise ratio, resolution and contrast. As a result considerably greater light levels have to be used then in targets which integrate over the full frame period. Thus the crucial elements, common to all modern pickup tubes, are the charge storage surface and the scanning electron beam which is incident on the charge storage surface at very low energy. These are shown in Fig. 1(a). The charge storage insulator is generally very thin with a thickness of several microns or less. The surface of the insulator is held near cathode potential. The backplate potential is held at cathode potential or at a small positive voltage relative to cathode. The combination of storage insulator and backplate electrode is commonly called the "target". In the absence of incident radiation flux the electron beam scans over the storage surface depositing negative charge uniformly over the scanned part of the surface by virtue of the fact that the effective secondary

Jan 1, 1970

By J. Winter, W. C. Setzer, A. J. Goldman

ANISOTROPY in cold worked tempers of commercial aluminum alloys is manifested in deep drawn products as protuberances or ears 45 deg to the rolling direction. This reflects the {123}(412) rolling texture.' In fully annealed material, 0 to 90 deg ears in and per-

Jan 1, 1970

By R. M. Rose, K. A. Jones

Resistive measurements ulere made on superconducting niobium single crystals in transverse magnetic fields. Crystals were grouln in both high and ulfrahigh vacua, doped with stnall quantities of oxygen, and annealed in ultrahigh vacua at temperatures from 900' to 1350°C. Maxima in the fluxoid pinr~ir~g force were observedfor the [100] and [210] directions. The increase of the critical current density with dissoved oxygen was seen to saturate at relatively low concentration. This behavior, and the variation of J, and residual resistivity (as a function of oxygen content and annealing) of both clean and dirty gassy) crystals, is seen as a consequence of the formation of clusters with (210)~b habit planes and (200)ffo common boundaries. These suboxide clusters are apparenlly stable at high temperatures and very low oxygen concentrations. It is generally known that dissolved oxygen at concentrations well below the solubility limit sharply increases the critical current density of superconducting niobium.' Such a result would not be expected if Nb-0 solutions were random, not even as the result of segregation on the scale usually encountered in solid solutions. According to the Kim-Anderson theory of flux creep,' the critical transport current density is determined by the pinning force Fp associated with some feature of the microstructure. As the Lorentz force. a or (J X R), of the transport current in the magnetic field approaches Fp, flux creep and then flux flow occur. The pinning force is expected to be quite small if the heterogeneity involved is significantly smaller than tte range of coherency which for niobium is circa 250~.~ Although the strain field of an individual oxygen atom in the niobium lattice is relatively large, it does not seem plausible that individual atoms could be so effective as to account for the data. Also, ~ramer~ found that straining and strain aging specimens containing small amounts of oxygen on occasion decreased the residual resistivity. A possible explanation for the above behavior may be found in the work of van Ooijen and van der Goot,= who found that annealing changed J, for niobium foils containing oxygen, and they attributed the changes to ordering of the oxygen atoms. This phenomenon has been observed by other investigators using X-ray and PROCEDURE Cylindrical 4-in.-diam niobium single crystals with axial orientations [ill], [110], [112], and [oo~] were grown from pure niobium, see Table I for analysis, in an ion-pumped ultrahigh-vacuum system using the electron beam floating zone technique. Total pressure during growth was lo-'9 torr: the oxygen partial pressure was less than lo-" torr, as determined by a mass spectrometer. These crystals will be referred to as the "clean" crystals. Similar crystals were also grown in another system at a pressure of 5 X 10"6 torr. These crystals will be referred to as the "dirty" crystals. Specimens 14 in. long were cut from the as-grown crystals and one end was polished down to no. 600 carbide paper smoothness. A back-reflection Laue photograph was then taken in order to fix the crystallo-graphic directions transverse to the crystal. The critical current density J,, the current density necessary to produce a voltage drop of 1.0 pv between voltage leads placed a in. apart, was determined as a function of the magnitude and direction of the transverse magnetic field and of the oxygen concentration. The technique and experimental arrangement was essentially similar to that of Tedmon et al.' In the remainder of this paper, the azjmuthal angle $ for the field H is referenced to the [ I101 direction in all four crystals, and oxygen was added in small equal increments by anodization and annealing.7 The resistivity ratio, RR, of the resistance at room ternperature to that at 4.2"K (H =7.00 kG) was determined as well.

Jan 1, 1970

By Harold A. Watson

A method for measuring leakage of vapors into a chemical-cartridge half-mask facepiece during simulated use is described. The respirator, fitted with high efficiency cartridges, is worn in a dichlorodifluoromethane (CC12F2)--air test mixture while a series of timed activities (facial movements, varied breathing, exercise, etc.) is performed. Complementing other tightness tests, this method is useful particularly for studying face fit and the effect of facial movements on leakage. The concentration of CC12F2 within the facepiece is monitored continuously to observe the immediate effect of physical activity on leakage. A composite sample is collected simultaneously in a plastic bag as a measure of average leakage during the 18-minute test period. Leakage, reported as percent, is calculated from the concentrations of CC12F2 within the facepiece and in the test atmosphere.

Jan 1, 1970

By R. W. Regehr, R. A. Burmeister

Epitaxial growth of GaAs 1-xPx on germanium substrates was achieved using an open tube vapor transport system. The compositional range of 0.3 < x < 0.4 was examined. The best results were obtained with (311) orientation of the germanium substrate. The physical and chemical properties of the resulting layers were investigated using several techniques. Spectrographic analyses of the layers indicate substantial incorporation of germanium into the GaAs t-X Px layer. Evidence is presented which indicates that this incorporation occurs via a vapor phase transport process rather than by solid phase dijfu-sion. Electrical measurements suggest that the germanium thus incorporated behaves predominantly as a deep donor in the compositional range of 0.33 < x * 0.40 and has a deleterious effect upon the luminescent properties of GaAs1-x Px. The increasing technological importance of GaAs1-xPx for use in light-emitting devices has led to an evaluation of several aspects of existing growth processes. The method most commonly used to prepare GaAs1-xPx for electroluminescent device applications is vapor phase epitaxial growth on GaAs substrates.&apos;-4 In a typical electroluminescent diode structure the active region of the diode is entirely within the epitaxial layer and thus the electrical properties of the substrate are relatively unimportant since it is effectively a simple series resistance (assuming hetero-junction effects to be negligible). The use of germanium rather than GaAs as the substrate material is of interest for several reasons. First, GaAs of reasonable structural quality has been epitaxially grown on germanium4-2 and it is reasonable to expect that GaAs1-xPx could subsequently be deposited on the GaAs layer. Second, germanium substrates are readily available with both lower dislocation densities and larger areas than GaAs. Finally, single crystals of germanium are more economical than GaAs single crystals. The principal objective of the present investigation was to test the feasibility of growing GaAs1-xPx epi-taxially on germanium substrates, and to evaluate the properties of such layers with regard to electroluminescent device requirements. The approach used was to a) demonstrate epitaxial growth of GaAs1-xPx on germanium, and b) characterize the relevant structural, electrical, and optical properties of the GaAs1-xPx layers. The possibility of germanium incorporation into the grown layers was of special interest since there was some indication of this in previous studies of GaAs growth on germanium.5&apos;11,12 Although a study of the electrical properties of germanium in GaAs1-xPx was not an intent of this investigation, several features of the electrical properties of the layers grown in the present study which appear to be due to germanium are described. EXPERIMENTAL PROCEDURE The open-tube vapor transport system used for the epitaxial growth of GaAs1-xPx is illustrated in Fig. 1. This system utilizes the GaC1-GaC13 transport reaction and is similar in most respects to the larger system described elsewhere.&apos; The germanium substrates were n-type, with a resistivity of 40 ohm-cm (Eagle-Picher Co.). These were cut to the orientations of {100), {111), and (3111, and were mechanically polished and chemically etched in CP-4 (5 min at 0°C) prior to growth. In some cases, a GaAs substrate was employed in addition to the germanium. The orientation of the latter was {loo}, and they were also mechanically polished and chemically etched prior to growth. The initial composition of the deposited layer was pure GaAs. After approximately 10 microns of GaAs was deposited on the germanium substrate, the phosphorus content of the layer was gradually increased over a distance of approximately 15 microns to the desired concentration and maintained at this value throughout the remainder of the growth. Typical operating parameters used during growth are given in Table I. Selenium was used as a n-type dopant in several runs to facilitate comparison of the electrical properties of the layers grown on germanium with those of layers grown on GaAs substrates, which are usually doped with selenium. The concentration of H2Se in the gas phase was adjusted to a value which would normally yield a carrier density of 1 to 5 x 101 7 at room temperature in layers grown on GaAs substrates. The terminal surfaces of the epitaxial layers were examined by optical microscopy for structural characteristics. Laue back-reflection photographs (Cu radi-ation) were also made on the terminal surface to verify the epitaxial nature of the deposit. After these steps

Jan 1, 1970

By H. M. Howard

"The subject of Grinding Media is perhaps still quite controversial. Many people will state today that the spherical ball is the only way, and also will state that this was settled long ago others are not so sure, and I am in this second category. Over the years there have been many changes in grinding and in our evaluation of grinding media we should always be ready to review the overall situation at regular intervals. There is quite a lot of inertia in all branches of Hineral Dressing and this is particularly true of grinding or, more correctly, comminution.In order to understand some of the things which are done today, and to understand some of the thinking on grinding, it is desirable to go back some sixty years and trace the developments in comminution. In doing this we should consider perhaps three general categories with respect to daily tonnage. An arbitrary division would be under 500 T.P.D., 500-5000 T.P.D., and large operations which might have several parallel units, each with a capacity of about 5000 T.P.D. For the future, in the broad picture, this last category will be the important one because we will be more and more dependent on large-tonnage low-grade operations for most of the metals of the future. Some such division is necessary because the daily tonnage will have a very great effect on what we can and cannot do. It is also necessary to consider the entire flowsheet, and to remember in particular that grinding is not merely to make small particles but is also a conditioning process, to prepare the materi.al for the process which follows. The relationship of crushing to grinding must also be considered. It is logical to include the liners as part of the grinding media and we should try to distinguish between the wear of grinding media and the consumption of media by corrosion. Finally, the whole question of grinding media should be examined in relation to the possibilities of using some form of autogenous grinding."

Jan 1, 1970

By Rees D. Groves

Cement copper is ordinarily converted to marketable metal by processing in a conventional smelter and refinery. Because of rapidly increasing cement copper production and limited excess smelting capacity, other techniques were investigated for preparing marketable copper products. One route was to make copper powder for industrial use. The process scheme employed flotation for rejecting the bulk of the impurities, acid leaching to remove residual iron and aluminum, reduction sintering to eliminate oxygen, and grinding to obtain powder. Another route was to sinter the floated and leached copper into the form of anodes and electrolyze these to yield refined copper cathodes. At a current density of 30 amperes per square foot, power consumption for electrorefining was 185 kwhr per ton of copper. The feasibility of preparing commercial-size anodes by sintering is still to be assessed.

Jan 1, 1970

By R. D. Hossack

"The selection of a site for plant facilities is a function of several factors and has as its objective the maximization of profits, given fixed markets and sources of raw material locations. In practice there are several sites, any one of which or a combination of two or more would be suitable to meet the basic requirements of source of supply of raw material and labour and still fulfill market demands. The model used to select the optimum profit combination utilizes both computer programs and traditional financial analysis techniques. Of the three computer programs used in the mode), one is a linear program and another is a transportation simulator. Basic cost and price data are required. In examining costs, three levels are used: (a) distribution costs of raw material to the plant and finished goods to the market; (b) direct production costs at the plant, such as labour and locally supplied material; and (c) capital and overhead costs at the plant, such as construction costs, taxes, insurance, and federal and provincial cost allowances. The direct costs generally depend on the scale of operations, so that a large plant in one location may have a lower unit cost than two smaller plants. This, of course, must be balanced against distribution costs. In examining profit, it is necessary to think in terms of the price and volume of sales at each of the market locations. Given basic data and relationships, the model can be used to optimally locate production facilities or, alter-natively, optimally structure a transportation network given existing locations of plants and markets. It is dynamic to the extent that it can react to changes in volume, price and cost to optimally locate an additional plant, the expansion of existing plants, the shutting down or cutting back of plants, or the restructuring of distribution networks."

Jan 1, 1970

By L. Leibowitz, M. G. Chasanov, L. W. Mishler

A drop calorimeter system is described for use in measuring enthalpies to 3600°K. Data are presented for tungsten between 2800" and 3600°K. The enthalpy of tungsten in cal per mole between 2000° and 3600°K can be represented by the equation HºT- Hº298 = - 1.7622 X 103 + 5.7772T + 8.9861 where T is in degrees Kelvin. A tabulation of com -puted values is presented for heat capacity, entropy, and free energy function. A drop calorimeter has been constructed to carry out enthalpy measurements at temperatures to 3600°K. Samples are heated by induction1 and dropped into a commercial adiabatic calorimeter, modified for this purpose. The experimental temperature is limited by the melting point of container materials and compatibility of the container and its contents. Several high-temperature drop calorimeters have been described in the literature1-5 but none has been used at temperatures as high as those in the present work; our measurements of the enthalpy of tungsten range from 2800" to 3600°K. DESCRIPTION OF EQUIPMENT An overall schematic view of the equipment is shown in Fig. 1. Power for the induction coil is supplied by a 25-kw 250 kHz Ther-Monic generator coupled to an iron core RF transformer. The Sample capsule is suspended in the work coil by 10-mil diam tungsten wires which are wrapped around a horizontal 5-mil diam tungsten wire. The horizontal suspension wire is clamped between two massive copper electrodes which are fixed in an x-y motion device that allows adjustment of the position of the heated capsule from outside the vacuum chamber. The copper electrodes are connected by flexible copper straps to a 1250-joule (5 kv, 100 pfarad) condenser bank. When it is desired to release the capsule, the condensers are discharged through the horizontal suspension wire causing it to vaporize rapidly. Very reliable and precise release of the capsule is achieved in this manner. Experiments have shown that no heat correction is required for this discharge energy. As part of the temperature measuring system, two prism holders have been incorporated in the apparatus. The upper prism holder is in the main vacuum chamber itself, whereas the lower one is in a side arm attached to the drop tube below the gate valve. The upper prism is mounted on a rotary vacuum feed-through, and may be moved under a protective shield when not in use. This prevents deposition of vapors on the prism surfaces when temperature measurements are not being made. Similarly, the lower prism is mounted on a push-pull vacuum feed-through, and when not in use may be pulled into its side tube. The prism mountings are fitted with guides and stops so that they may be moved precisely into the desired position. The aim throughout is to minimize the time the prisms are exposed to vapors from the hot samples. At the high temperatures reported in this paper, only the lower prism was used. The upper prism holder in these cases was fitted with an additional radiation shield. By using a prism and viewport, the lower surface of the samples can be observed by an optical pyrometer. The measurements discussed in this paper were obtained with a Leeds and Northrup 8622-C-S series manual pyrometer which is estimated to be accurate to 0.5 pct. Pyrometer calibrations and prism and window corrections were carried out in the conventional manner6 using tungsten strip lamps calibrated by the National Physical Laboratory, Teddington, England. Prism corrections were rechecked after each use. All work to date has been done in vacuum, and no measurable change has been observed in the prism correction below -2300°K for the upper prism and below -2800°K for the lower one. The total time of exposure of the prisms is about 50 sec per run. At high temperature, the final temperature reading is corrected by using the final A value for the prism; see Ref. 6 for details of this procedure. The calorimeter is a modified Parr Instrument Co. (Moline, lll.), Series 1230 adiabatic calorimeter with automatic jacket control. Other authors5 have used a similar calorimeter with good results. The calorimeter jacket cover and calorimeter cover are attached to the drop tube which contains a radiation shield. This shield is a gold-plated copper disc which can be operated manually from outside the calorimeter. The receiver is attached below the radiation shield and is lined with tungsten. In a typical experiment, the calorimeter and its jacket water temperatures were adjusted to 0.000°K temperature difference. The sample was allowed to equilibrate in the furnace at the desired temperature for about 20 min. The initial calorimeter temperature was then recorded, the sample dropped, and appropriate shutters closed. After about 3 min, the drop tube and receiver were filled with helium to 60 torr. The final calorimeter temperature was recorded after it had remained constant over a 5-min period. The equilibration time in the calorimeter was about 25 min. Thermistor probes are used to operate a hot and cold water supply system to maintain the jacket temperature equal to the calorimeter temperature. For actual measurements of the calorimeter temperatures, a quartz thermometer was used (Hewlett Packard Dymec Thermometer, Model #2801A). This thermome-

Jan 1, 1970

By S. Feuerstein

THE influence of environment on the mechanical properties of metals has been extensively studied and documented.&apos; Most investigations have dealt with an interaction between a particular environment and a specific metal surface and the concomitant change in bulk mechanical behavior. Typical contributing media are oxide and metal film:;, electrolytes, and other surface-active agents. In the last category fall controlled gaseous environs (i.e., pressure or vacuum). Most vacuum exposure experiments prior to 1963 were conducted at pressures s>10-6 torr and elevated temperatures, or in such a manner as to prolong the exposure (e.g., by stress-rupture, creep, and fatigue). Little attention has been given to vacuum environment effects on the mechanical behavior of metals subjected to simple uniaxial deformation at room temperature. Test times and temperatures were assumed too ineffective as far as bulk changes were concerned. Further, the contribution of surface effects to the bulk mechanical behavior of metals was considered minimal. Under vacuums of the order of 1.0- 8torr and higher, molecular densities and, consequently, the rate of monolayer formation are such that exposures from seconds to days would be required for complete gas coverage. Thus, atomically clean surfaces created under ultra-high vacuum could conceivably maintain their cleanliness for time intervals orders of magnitude greater than at higher pressures. The influence of this unusual type of environmental surface phenomenon on the short-term bulk mechanical behavior of aluminum was first observed by Krame and Podlaseck in 1963.&apos; kin equivalent effect was reported for magnesium by Williams and Nelson.3 It was concluded from these studies2,3 that vacuum and, consequently, the monolayer formation rate of the oxide, were responsible for the described changes in flow behavior. The presence of an oxide layer impedes dis- I) EXPERIMENTAL DATA: MOLYBDENUM The tensile behavior of molybdenum was investigated by the author4-6 at ambient temperature over a range of pressures from 760 to 10-10 torr. These studies revealed that the flow behavior of the bulk specimens (0.200 in. diam by 2 in. gage length) was independent of pressure on sintered (0.062 mm grain size) and arc-cast polycrystals (0.012 to 0.149 mm grain sizes) and single crystals. Since the specimens were relatively large in size, it was assumed that any flow behavior effect would be surface-limited because of the short-term deformation procedure. Strain-rate-change experiments performed to determine the activation volumes for individual specimens at 760 to 10- 10 torr further indicated that the surface flow contribution was either minimal or zero, contrary to the findings of Shen el a1.7 on aluminum. Although the flow behaviors did not change, specimen ductility did change. For the sintered material at a strain rate of 4.2 x 10-4, specimen ductility was -9 pct higher at l0- 10 torr than at atmospheric pressure (dry nitrogen). A more comprehensive investigations on this same material revealed a distinct pressure dependence, Fig. 1. Intermediate and atmospheric pressure tests were obtained by backfilling the system from l0- 10 torr with extra dry, prepurified nitrogen. Other environments (air and purified argon) were also utilized for the 760 torr experiments; the results were essentially the same as those for dry nitrogen atmospheres. Departure from the fracture strain values obtained at 760 torr takes place in the vicinity of l0-6 torr, as indicated by the scatter band; a noticeable ductility increase is apparent at l0-8 and 10-10 torr.

Jan 1, 1970

By M. C. Irani

This study is a survey of supply and demand for minerals, metals, alloys, and compounds used by the chemical industries in the Ohio River Basin (ORB) area of Ohio, Pennsylvania, and West Virginia during 1967. Data for the study were obtained from completed questionnaires received from chemical manufacturers and from interviews with officials of chemical companies and mineral producers and distributors. The information includes kind, quality, quantity, values, sources, specifications, uses, and methods of transportation. Results of the study show that of the total value of mineral materials consumed by the chemical industry, manufacture of inorganic chemicals consumed 46 percent; fertilizers, 22 percent; and soaps and detergents, 19 percent. Fifteen commodities accounted for 91 percent of the total value of mineral materials consumed. Five of these--phosphates, potash, salt, sulfur, and titanium dioxide--accounted for 59 percent of the total.

Jan 1, 1970