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By S Bankoff

INCE1 proposed that electrostatic attraction between oppositely charged particles was responsible for slime-coating. Del Giudice2 postulated the metathetic formation of a cementing compound. Wark3 suggested that prevention of slime-coating was related to peptization of the slime. [ ] In the experiments of Table I the technique employed was essentially that of del Giudice, with the difference that the particle was examined under a film of water rather than dry.4 In general, the polished particle was agitated for 2 min. in a pulp consisting of 12.5 grams of the slime (-200 mesh) and 50 c.c. of distilled water, washed in three baths of distilled water, and examined at 220 diameters with the Leitz Ultropak. Observations of Brownian movement were made at 850 diameters with dark-field illumination. Several of these experiments do not jibe with the metathesis theory. According to published solubilities,5,6 the lead salts of the anions in experiments c through g are more insoluble than lead carbonate, there- [ ] fore should prevent the formation of lead carbonate on the galena surface. In experiment i the calcium oxalate, which presumably was on the calcite surfaces, should have permitted the formation of a lead carbonate cement by virtue of its greater solubility. Experiments j through m show that the addition of lime accelerates the deposition of quartz onto a galena surface. The writer is unable to postulate a satisfactory cementing compound, according to the metathesis theory, to explain this effect. These experiments led to the conclusion that the metathetic formation of a cement-

Jan 1, 1941

By M. S. Burton, B. W. Christ, G. V. Smith

Evidence of the effects which high-angle grain boundaries and veining subgrain boundaries have on the yield phenomenon of zone-refined iron is reported. Room-temperature tensile tests on 50-mil wive at several gram sizes produced upon recrystallization at diffevent temperatures below 910C (a-y phase-transfornzatzon temperature) show that upper and lower yield stress decrease with increasing grain size. The upper yield point effectively disappears at grain sizes of 81 and 102 u in samples of this diameter. However, samples of 129 p grain size. produced during recrys-tallization at 950°C, exhibit a pronounced upper yield point and an increased lower yield stress. Possible causes of the reversal in the grain-size dependence of yielding are discussed. Veining substructure, detected with picval-HC1 etchant, but not with 2 pct nital, is formed during the a-y transformation, and is believed to account for the observed effecls. The strengthening associated with high-angle boundaries in zone-refined tron is discussed in terms of: 1) the stress dependence of slzp multiplicity, and 2) the stress dependence of dislocation emission from grain boundaries. WIDE use of transmission electron microscopy and dislocation etch-pitting techniques has led to a growing awareness of the presence of dislocation substructures in annealed pure metals. Whereas much speculation'-4 has developed about the influence which subgrain structures have on the mechanical behavior of metals, particularly the yield strength, only limited experimental evidence correlating subgrain structures with lower yield strength has been presented. 2,3,5-7 It is the purpose of this note to present experimental evidence of the effects which grain boundaries and subgrain boundaries have on both the upper and lower yield strength of zone-refined iron. Effects due to high-angle boundaries formed upon recrystallization below the a-y phase transformation are compared with effects due to veining subgrain boundaries formed upon "recrystallization" above the a-y phase-transformation temperature. These effects are further compared with the reported influence 2,3,5-7 which low-angle boundaries have on the lower yield strength of bcc transition metals. EXPERIMENTAL PROCEDURE The starting material for these experiments was a 1-in.-diam zone-refined ingot prepared at Battelle Memorial Institute. Initial purification of electrolytic iron by vacuum-induction melting was improved by a floating zone-melting treatment in ultrapure hydrogen.' Chemical analysis of this zone-refined iron appears in Table I. Tensile samples of 50-mil wire were prepared by rolling and drawing portions of the ingot. An intermediate recrystallization anneal at 625°C after rolling to a reduction in area of 85 pct was carried out in an evacuated Vycor capsule (10-=5 mm Hg). Further reduction in area of 91 pct was followed by recrystallization in evacuated Vycor capsules at temperatures between 600" and 950°C, see Table 111. All samples

Jan 1, 1967

By J. H. Bowden

The shaft-plant here described was put in operation in September, 1895, and the No. 6 slope-motor was started in May, 1896. The plant comprises : One Norwalk three-stage compressor l21/2, 91/2 and 5 in. diameters of air- and 20 in. diameter of steam-cylinder, all 24 in. stroke; capacity at 100 revolutions, 296 cu. ft. of free air per minute, compressed to 600 Ibs. per sq. in. A main pipe, 5 in. diameter, 4380 ft. long, with five charging-stations in No. 6 Shaft, and a branch of 3 in. pipe, 3100 ft. long, with three charging stations, in No. 6 Slope. These pipes on each line charge a Porter compressed-air motor, with 7 by 14 in. cylinders, and four 24 in. drivers, weighing about eight tons, with a tank-capacity of 130 cu. ft. of air at 550 lbs. pressure in the main tank, reduced to 160 lbs. in the 8-in. auxiliary tank of 4.2 cu. ft. capacity, supplying the cylinders. The No. 6 shaft run averages 4000 ft. each way on grades of $ to 23/4 per cent., and averaging close to one per cent. in favor of the loaded cars. The No. 6 slope run averages 2100 ft. with nearly the same grades. The mine-cars weigh 2800 Ibs. empty, and about 9800 lbs. loaded, and are hauled in trips of 12 to 20, averaging about 15 cars. The shaft-motor now hauls about 355, and the slope-motor 320 cars per day of 10 hours, replacing in the shaft 17 mules, and

Jan 1, 1901

By F. A. Schaufelberger

METAL can be recovered from a leach solution either indirectly by precipitation as a compound that is later reduced or directly by electrolysis, cementation, or chemical reduction, for example, with hydrogen. The widely used electrowinning processes suffer from the inefficiency of converting fuel to low voltage dc and from low current efficiency when complete recovery is attempted. With the batch hydrogen reduction methods outlined here, a unit of fuel converted to hydrogen in modern gas reform plants will make two to three times as much metal as can be obtained with electrolysis. With continuous hydrogen reduction, four to six times as much metal is obtained. Precipitation by reducing a metal salt solution with H, has been known for almost 100 years.' Commercial use of the process, however, awaited the research and development program initiated by Chemical Construction Corp. Within the last few years this program has brought about construction of commercial plants, listed on page 545. Ideal hydrogen reduction will precipitate a pure metal from a solution obtained by commercial leaching methods at a rapid rate without excessive temperatures and pressures. The metal precipitate will be of desired size and density, less than a percent left in the vessel being deposited on the wetted parts. The present discussion will outline Chemical Construction Corp.'s early development program and will discuss the chemistry and mechanics of reducing copper, nickel, cobalt, and cadmium from solution by H2. Work on selective reduction of nickel from cobalt has been described earlier.' The article is not concerned with precipitation of copper by disproportionation of cuprous solutions where yield is limited3 to 50 pet.* It does not discuss use of gaseous reducing agents other than hydrogen, such as SO2,4 which may lead to contamination with sulfur, or C0,5 which is considerably more expensive than hydrogen and produces a gaseous reaction product, CO2.† The article does not include use of other nongaseous reducing agents,7 which are far more expensive than CO. Also, notes on the history, engineering design, and performance of commercial plants have been given elsewhere.' It will be shown that a pure metal can be precipitated by reduction with hydrogen from solutions obtained by commercial leaching methods when the solution composition is controlled and proper acidity, proper metal ion concentration through controlled complex formation and hydrolysis, and adequate agitation for suspension of metal and for transfer of reducing gas are maintained. Reasonable temperatures and pressures are used which are less excessive than those used by previous workers, although they are maintained at above equilibrium values because of process kinetics.' It has also been found necessary to induce nuclea-tion and to control growth and agglomeration in order to get a powder product of suitable physical properties. Review of the Literature Muller, Schlecht, and Schubardt of I. G. Farben10 claimed a successive reduction of silver, copper, nickel, cobalt, and zinc from ammoniacal solution by applying progressively higher temperatures and hydrogen pressures. Metals produced by this technique were not pure, since no attempt was made to adjust the solution composition between the different reductions. It is doubtful that the zinc product contained any metallic zinc. The major contribution to the literature" was made by the Ipatiews,12 who prepared platinum, iridium, copper, nickel, cobalt, lead, tin, arsenic, antimony, and bismuth at often extreme conditions, up to the critical temperature of water (373ºC), at 1500 to 7500 psi, for as long as several days. Even cadmium and zinc were claimed to have been observed in trace quantities precipitated together with basic salts. In the early experiments solutions were not stirred. Extensive formation of oxides and basic salts occurred, probably long before sufficient hydrogen could be supplied in the unstirred liquid to decrease the metal concentration in solution by reduction. The importance of hydrogen pressure was

Jan 1, 1957

By J. J. Taber

The turbulent flow drag coefficients, or friction factors, have been experimentally determined for the cut-tings normally encountered in drilling operations. The gas law and average drag coefficients for characteristically flat particles (limestones and Shales) and for angular to sub-rounded particles (sandstones) were used to extend Newton's equation to a more useful form. The resulting equations are expressions for the slip velocity of a particle as a function of the particle size and shape, the bottom-hole injection Pressure, and the Bottom-hole temperature. The velocities necessary to lift actual rock cuttings as observed in the laboratory were compared with velocities predicted from the derived equations. Results indicate that there is no single correct circulating velocity and that the commonly used 3,000 ft/min linear velocity may he sufficient to lift only very mall particles. The advantage, in terms of horsepower requirements, of cycling high pressure air to obtain lower compression ratios was shown. INTRODUCTION A promising departure from standard rotary hydraulic drilling is air or gas drilling. In many instances the rate of penetration and bit life increases resulting from this method have been very substantial. Further the application of air drilling in areas of lost circulation or water sensitive pay zones has been highly successful. Purpose For the drilling contractor, the practical question remains, "How much air pressure and volume should I have?' lt is necessary to have a reasonable knowledge of the air velocities and pressures required in air drilling operations for the proper design and most advantageous use of surface equipment and for adequate removal of cuttings from the borehole. Eased on experience, most operators agree that at least 3,000 ft/min linear velocity is necessary for satisfactory hole cleaning.' It was the purpose of this investigation to evaluate the drag coefficients, or friction factors, for the cuttings normally encountered in drilling operations, i.e., sandstones, limestones and shales, and to utilize the values obtained to develop an expression for the minimum velocities and pressures (hence the volumes) necessary to lift these cuttings. THEORY Several investigators have done extensive work on the ability of drilling mud to lift bit cuttings. They conclude that the ability of a drilling mud to lift cuttings is dependent on the density difference between the rock being drilled and the drilling mud, the cutting size and shape, the mud flow constants, and the flow state (laminar, transitional or turbulent) of the mud. However, drilling muds are not true fluids but have a variation of viscosity with velocity in laminar flow and a constant apparent viscosity in turbulent flow. A survey of the literature revealed that no experimental work had been done to determine the velocities necessary to lift actual rock cuttings using a compressible fluid such as air or gas. In 1953, Nicolson6 stated that in air drilling fluid mechanics the particles could be assumed spherical in shape and that ; constant drag coefficient of 0.5 could be used due to the highly turbulent flow of the circulating air. By equating the turbulent resistance on the particle to the gravitational force on the particle, he obtained the expression, ^ = 2.67^y ,.......(1) where V, is slip velocity of spherical particle, ft/sec; D is particle diameter, in.; p, is particle density, 1b/ft8; and p, is fluid density, lb/ft3. However, as stated earlier, most operators seem to agree that adequate hole cleaning can be obtained by circulating a sufficient volume of air to give a linear velocity of 3,000 ft/rnin in the annular space. Basic Equation The velocity with which a solid particle freely falls through a fluid will increase until the accelerating force, gravity, is equal to the resisting forces, buoyancy due to the fluid displaced by the particle and friction due to the relative motion of the particle through the fluid. When the accelerating and resisting forces become equal,

By A. J. Sedriks

ALTHOUGH the occurrence of a readily visible tarnish on the stress-corrosion fracture surfaces of titanium alloys tested in oxygenated nitrogen tetrox-ide solutions has been reported,' the possibility that the formation of this tarnish is a requirement for cracking to proceed does not appear to have been considered. It has been proposed that failure occurs in this system as a result of some electrochemical-mechanical process.2 However, recent studies3-6 of the stress-corrosion cracking of a brass in certain ammoniacal solutions, which also cause visible tarnishing, have led to the view that failure occurs by the repeated formation and fracture of a brittle surface film of cuprous oxide. The purpose of this note is to point out the similarities which exist between the tarnish which forms on a brass and that found on titanium alloys failed in nitrogen tetroxide, and to suggest, by analogy, that a similar tarnish-rupture mechanism may be operative in the latter case. The titanium alloy selected for the present study contained 5.2 pct Al, 2.5 pct Sn, 0.025 pct C, 0.16 pct Fe, 0.014 pct N, 0.012 pct H, 0.07 pct 0, and 0.002 pct Mn by weight. Vacuum-annealed alloy strips measuring 4 by 0.25 by 0.04 in. were used to prepare self-stressed test specimens. Each specimen was made from two strips by bending the end portions and spot welding them together to produce curved sections of uniform bending stress. (The exact details of preparing such specimens have been described by Lisagor el al.7) The curvature in the strips determines the ma-magnitude of the outer fiber stress, which in the present specimens was 100,000 psi (yield stress = 120,000 psi). The specimen surface in the spot-welded end regions was shot-peened to induce compressive stresses and thereby eliminate the possibility of stress-corrosion cracking in these regions. The test environment was nitrogen tetroxide, initially containing 99.5 pct N2O4, 0.1 pct H2O, and 0.08 pct C1, through which oxygen had been bubbled for 30 min. During testing the tetroxide was subject to an oxygen pressure of 250 psi. The duration of the test was 96 hr, and during this time stress-corrosion cracks propagated through some 50 pct of the thickness of the specimens. After testing, the tarnish was liberated from the fracture surface by immersion in a methanol-5 pct bromine solution, and then examined by electron dif- fraction and transmission electron microscopy using a JEM-7 electron microscope. The possibility that the bromine solution had affected the structure of the tarnish was investigated by an "in silu" examination of the stress-corrosion fracture surface using a reflection electron diffraction attachment designed for handling bulk specimens. Typical areas of the tarnish liberated by the me-thanol-bromine solution are shown in Fig. 1. Fig. l(a) reveals that the tarnish consists of individual platelets, and from Fig. l(b) it can be seen that the platelets are joined together to form a semicontinuous film, the boundaries of the titanium substrate grains being retained in the tarnish. Electron-diffraction patterns taken from these areas exhibited diffraction spots typical of a monocrystal. The diffraction pattern shown in Fig. 2 was taken from the central area in Fig. l(n). Monocrystal patterns obtained from areas containing numerous individual platelets can only be explained by assuming that their growth is governed by the titanium substrate (i.e., their growth is epitaxial). In other areas, the tarnish had folded over or became mechanically damaged, and these areas gave diffraction patterns consisting of "spotted" rings, enabling interplanar spacings of the tarnish lattice to be determined. These spacings, measured using a

Jan 1, 1968

By S. A. LoPilato, J. T. Smith

SEVERAL techniques have been evaluated for cooling the throat area of rocket-nozzle inserts to prevent erosion or fracture of the inserts during exposure to high operating temperatures and pressures. Self-cooled composites, such as infiltrated tungsten, have shown considerable promise for these applications. These composites can be fabricated by infiltrating the refractory matrix with a lower-melting metal or non-metal which is insoluable in tungsten. During firing, the lower-melting substance undergoes a series of continuous endothermic phase changes which absorb sufficient heat to maintain the nozzle matrix material at or below a safe operating temperature. At present, the state-of-the-art has reached a point where the refractory matrix density and microstruc-ture have been established as the critical parameters to be controlled for optimum self-cooled performance.'" Nondestructive testing has been utilized to ensure that porous tungsten billets were of uniform density and free from cracks or other defects prior to fabrication into rocket nozzle inserts. Ultrasonic-velocity techniques have been employed because of their reliability and reproducibility. The purpose of this note is to present and interpret the test data developed for porous tungsten matrices. For evaluation purposes, tungsten powders with Fisher subsieve sizes of approximately 4 and 18 p have been obtained for study from four commercial sources: the General Electric Co., Wah Chang Corp., Fansteel Metallurgical Corp., and Kennametal, Inc. Porous tungsten matrices were fabricated from the powders by hot pressing in induction-heated graphite die assemblies. Typical billets ranged from 3 in. diam, 2 in, high to 5 in. diam, 5 in. high. The ultrasonic-velocity measurement technique employed was through transmission, pulse echo at a frequency of 1.0 mc using matched barium titanate crystal transducers. The testing equipment included a pulsed ultrasonic generator, an amplifier, a specimen holder, and an oscilloscope, as shown in Fig. 1. The porous tungsten thickness was measured to i 0.0005 in, with precision micrometers while the oscilloscope achieved 0.02 psec time measurement accuracy. The time for a sound wave to pass through the billet, the bulk wave velocity, was calculated to 0.5 pct using Eq. [l]: V-} where V = bulk wave velocity, in. per psec, T = specimen thickness, in., and / = time, psec. To develop inspection standards, the bulk density of a porous tungsten billet was determined by the ASTM water-immersion technique.3 The ultrasonic-velocity measurements were completed at seventeen positions for each billet and averaged to develop a characteristic standard velocity for a particular tungsten powder at several density levels. A plot of ultrasonic velocity vs density is presented in Fig. 2 for six different tungsten powders. This graph has been established as

Jan 1, 1967

By A. E. Deruyttere, J. Van der Planken, M. Laurent, Van den Bergen

FahRENHORST and schmid1 observed that zinc single crystals work hardened less rapidly when strained in liquid air (- 185°C)than in a bath at -82°C, whereas at higher temperatures the rate of work hardening decreased with increasing temperature, as would be expected. Cadmium and magnesium showed no such decrease at -185°C. At that time the observed anomaly for zinc at liquid air temperature probably seemed insignificant. However it later was confirmed2 by experiments in liquid nitrogen (-196°C) and in the mixture solid carbon dioxide-acetone (-77"C) and therefore appeared to be real. seeger3 then suggested that the anomaly might be due to the different wetting of the zinc crystals by the cooling media. Recently a new confirmation was obtained,4 however the cooling media again were different: the rate of strain hardening was found to be lower in liquid nitrogen and liquid oxygen than in pentane cooled to various temperatures down to -126°C. Ekperiments will now be reported in which the medium surrounding the specimen at the different temperatures was the same, namely gaseous air. The single crystals were made from "Overcor 99.99" zinc. They were grown in a vertical traveling furnace on seeds of nearly the same orientations. The diameter of the crystals was 5 mm and the length between shoulders 140 mm. The brass shoulders were stuck to the crystals by means of araldite. A thin steel wire was fixed to each shoulder and served to fasten the specimen to a Houns-field tensile testing machine. The crystals with the shoulders and part of the wires were surrounded by two concentric cylindrical containers. The coolant. either liquid air or ground solid carbon dioxide, was poured into the outer container only. During cooling the containers rested on a support which was removed when the straining was started. In order to check the temperature which the crystals would attain inside the inner container, a hollow bar of zinc in which a thermocouple was fitted was first mounted in the apparatus as a substitute for a crystal. It appeared that a constant temperature, respectively - 183° and -72°C, was attained inside the bar, if a soaking time of the order of 1 hr was allowed and if the outer container was constantly kept filled. Accordingly, this procedure was adopted for every tensile test. To take account of the large scatter, fourteen tensile tests were performed with liquid air and seven with solid carbon dioxide. The orientation of the crystals and the results are presented in the table, in which the symbols have the following meaning: 1 : temperature x : initial angle between basal plane and specimen axis : initial angle between slip direction and specimen axis a : shear strain at fracture 0: average rate of strain hardening = —-——- 100 t0 and Te representing respectively the critical shear stress and the shear stress at fracture. Despite the scatter of the a- and 8— values which is of the same order of magnitude as in the work reported by Seeger and Trzuble,4 it is evident that the strain hardening rate is significantly lower at -183°C thanat-72°C. The table also contains the average values calculated from Seeger and Trauble's results at the corresponding temperatures: z.e., four results at -183oC and two at-70°, -71°C. These authors calculated 9 in a slightly different way, but this is unimportant. The agreement between the a-values shows that both sets of experiments are comparable despite the differences in experimental techniques. The rates of strain hardening also agree and it may therefore be concluded that the anomaly is not

Jan 1, 1962

By R. J. Jackson, D. E. Williams, W. L. Larsen

The phase diagram of the Ta-Zr system is presented with a discussion of the methods used in its determination. The solidus contains a minimum at 1820°C near 25 wt pet Ta. A complete solid solution exists at elevated temperatures between tantalum and ß zirconium. This solid solution decomposes monotectoidally at 800°C and 12 wt pet Ta. The maximum solubility of tantalum in a zirconium is slightly less than 2 wt pet, and decreases with decreasing temperature. The solubility of zirconium in tantalum is 5 wt pet at the monotectoid temperature and about 2 wt pet at room temperature. THIS investigation was part of a program of research on refractory metal alloy systems having potential application in nuclear reactor technology. Preliminary prop-ess has been reported in the Ames Laboratory annual research reports.l Most of the previously reported work on the Ta-Zr alloy system consisted of partial phase diagram investigations and the determination of the mechanical properties of the zirconium-rich alloys. Anderson eta1.2 studied alloys containing up to 30 wt pet Ta as part of an investigation of several zirconium alloy systems. These investigators also determined some of the mechanical properties of the alloys at room temperature and 650°C. In a discussion of Anderson's work, Pfei13 suggested that the bright phase in the microstructures of the intermediate alloys is a tantalum-rich solid solution or an intermediate phase in a matrix of ß zirconium solid solution. Litton,4 Keeler,5 and Chubb6 determined the mechanical properties of zirconium-rich alloys at ambient and elevated temperatures. Van Thyne and McPherson7 reported the tensile properties

Jan 1, 1962

By W. Hodge, A. F. Haskins, R. M. Evans

Refractory boron compounds are shown to resist corrosion by molten zinc. Coatings were made from ferroboron and manganese boron by several methods: welding, hard facing, and pack diffusion; and techniques of coatings are very important. Mechanical failure of the diffusion coatings can be partially eliminated by applying them to type 416 chromium steels rather than carbon steels. Welded coatings made with a tungsten arc are better than those made by other welding methods. Sintered compacts of mixtures of iron and chromium borides developed strengths of about 30,000 psi. They resisted corrosion of zinc at 600°C and oxidation at higher temperatures. MOLTEN zinc rapidly attacks common metals of construction. The rate of attack is greatly amplified at temperatures over 500°C. However, there are many applications where it is necessary, or at least advantageous, to use metal construction, such as for galvanizing pots and zinc smelter equipment. Condensers and agitator linings used in continuous zinc smelting processes are eroded and corroded by violently agitated molten zinc. Pumps, tubing, and other parts to permit transfer of molten zinc would be desirable in many zinc handling operations. The development of metallic materials which are resistant to molten zinc also might permit its use as a heat-transfer medium in modern high efficiency power plants. In reviewing previous work on zinc-resistant metals, it was evident that most of the available data refer to corrosion at temperatures just above the melting point. Tungsten and high Mo-Fe alloys containing more than 80 pct Mo resist corrosion by molten zinc.', ' Imhoff states that because chromium is not attacked by zinc, chromium plating improves galvanizing pot life." Nitrided cast iron has been used in die-casting machines' where the molten alloy is 96 pct Zn and 4 pct Al. Other metals that have been suggested as of possible value for zinc resistance are columbium, tantalum, and titanium.V he corrosion of steel by zinc has been discussed by many authors,z, "2 None of these materials resisted corrosion by molten zinc at the temperatures used in this investigation, i.e., 600" to 700°C. I. Exploratory and Resistant-Coating Tests To make a study of zinc-resistant metals, exploratory tests were conducted to sort out roughly those materials which seemed most worthy of further development. This preliminary study included both solid metals and surface coatings. Exploratory Corrosion Tests in Molten Zinc—In initiating a study of this problem, numerous samples of metals and alloys were evaluated by dynamic corrosion tests made at 440 °C. Each metal was tested in its most readily available form, which, because of shape and size, was often unsuited for standard corrosion testing. The equipment used for dynamic corrosion testing of all materials, except in a few initial experiments, is shown in Fig. 1. Samples were tied to tungsten rods with tungsten wire, immersed in the zinc, and revolved at 12 rpm about the circumference of a 4 in. diam circle. Speed of travel was about 12.5 fpm. The molten zinc was protected from oxidation by an atmosphere of carbon monoxide, or, at a later period in the program, by a 9:1 mixture of nitrogen and hydrogen. When the effect of both molten metal and atmosphere was desired, the zinc level was lowered. Special high grade zinc was used in all of the corrosion tests. Corrosion losses for materials tested are shown in Tables I and 11. Whenever the materials were available in suitable form, the losses are reported in mils per year. It was recognized that weight losses on irregularly shaped specimens did not show the corrosion rate but the important consideration—poor resistance to corrosion—could be determined readily.

Jan 1, 1956

By Leon W. Dupuy

A brief elemental discussion of the fundamental factors involved in diamond drilling often fills a need, particularly when a mine operator is contemplating for the first time an exploratory drilling campaign. Mr. James A. Barr, of the Mining Methods Committee of the Institute, has suggested that many engineers must undertake a drilling program of one kid or another and, in the case of diamond drilling, sometimes even are at a loss as to how to start correspondence. The Bureau of Mines has acquired much experience in managing exploratory diamond-drilling activities. Its activities in diamond drilling included exploring for potash in Texas, Utah and New Mexico1-' during the 1920's. The Strategic Minerals Exploration program was started in 1939 and was materially expanded during the war to include critical and essential minerals. At the peak of its war-time activity more than 200 engineers were employed, a majority of whom supervised diamond drilling. Many of them had little experience with such work prior to their employment with the Bureau, and it was necessary to instruct them in their duties. The purpose of this paper, therefore, is to present the fundamentals of exploratory diamond drilling from the viewpoint of management in such a way that they will Serve as a basis on which those beginning exploratory diamond drilling may build an experience and acquire ability to direct exploration as they gain that experience. Selection of Method of Drilling Selection of the method of drilling is governed by the type of material to be penetrated and by the type of sample needed to determine the quality and importance of a deposit. Types of drills that might be used for a given job include diamond drills, churn drills, hand auger drills, power auger drills, bucket drills, and rotary drills (sometimes called "seismograph rigs"). Each type has a specific field in which it is most useful. While the Bureau of Mines utilized all the types of drilling mentioned, diamond drilling was used on a majority of its exploratory projects. Factors Governing Selection of Diamond Drilling The prime consideration in selecting a method of drilling is first to determine what results are desired and then to choose a method that will furnish reliable data in the ground to be penetrated. Use of diamond drills permits recovery of a core as well as sludge at a comparatively low cost. The core provides an excellent means of studying the formation being drilled and furnishes much information that would be difficult to obtain otherwise. Diamond drills will recover a satis-

Jan 1, 1948

By Leon W. Dupuy

A brief elemental discussion of the fundamental factors involved in diamond drilling often fills a need, particularly when a mine operator is contemplating for the first time an exploratory drilling campaign. Mr. James A. Barr, of the Mining Methods Committee of the Institute, has suggested that many engineers must undertake a drilling program of one kid or another and, in the case of diamond drilling, sometimes even are at a loss as to how to start correspondence. The Bureau of Mines has acquired much experience in managing exploratory diamond-drilling activities. Its activities in diamond drilling included exploring for potash in Texas, Utah and New Mexico1-' during the 1920's. The Strategic Minerals Exploration program was started in 1939 and was materially expanded during the war to include critical and essential minerals. At the peak of its war-time activity more than 200 engineers were employed, a majority of whom supervised diamond drilling. Many of them had little experience with such work prior to their employment with the Bureau, and it was necessary to instruct them in their duties. The purpose of this paper, therefore, is to present the fundamentals of exploratory diamond drilling from the viewpoint of management in such a way that they will Serve as a basis on which those beginning exploratory diamond drilling may build an experience and acquire ability to direct exploration as they gain that experience. Selection of Method of Drilling Selection of the method of drilling is governed by the type of material to be penetrated and by the type of sample needed to determine the quality and importance of a deposit. Types of drills that might be used for a given job include diamond drills, churn drills, hand auger drills, power auger drills, bucket drills, and rotary drills (sometimes called "seismograph rigs"). Each type has a specific field in which it is most useful. While the Bureau of Mines utilized all the types of drilling mentioned, diamond drilling was used on a majority of its exploratory projects. Factors Governing Selection of Diamond Drilling The prime consideration in selecting a method of drilling is first to determine what results are desired and then to choose a method that will furnish reliable data in the ground to be penetrated. Use of diamond drills permits recovery of a core as well as sludge at a comparatively low cost. The core provides an excellent means of studying the formation being drilled and furnishes much information that would be difficult to obtain otherwise. Diamond drills will recover a satis-

Jan 1, 1948

By Maurice Lacasse, Pierre Legast

GENERAL OUTLINE For more than one hundred years, asbestos ore has been mined on Les Mines d’Amiante Bell's property at Thetford-Mines , Quebec, Canada. In 1878, the first tons of fibre were produced. The mine operated as an open pit until 1951 at a yearly production of about 330 000 mt of ore. Since 1951, the mine has operated underground using a block caving method. The mine produced 725 000 mt per year until 1978, when the rate of production was increased to 1 100 000 mt. The ore was produced entirely fm the first lift on 650 level until 1976. Then, a second lift on 950 level was put into operation to replace production facilities fm the first lift which is now exhausted. Annual fibre production is 72 500 mt with grades £ran 3 to 7. The total work force is 600 people. The host rock is a peridotite partially serpentinized. The asbestos fibre seams occur as stockwork deposit structurally controlled by talcose shear zone. The geological rock formations are heavily jointed and have a wide range of competence. Asbestos ore bodies have an heterogeneous nature which des difficult geological interpretation. THE GRIZZLY METHODS A full gravity method was used on the first level where the caved ore was drawn from finger raises onto grizzly bars spaced at 480 mn. Oversize blocks were reduced by secondary blasting. The ore fell by gravity in- to the ore pass below the grizzly chamber and was loaded into 5.7 mt haulage cars through a 1.2 m wide chute. Access to the undercut drift was fm the grizzly drift through finger raises. The undercut trough was drilled and blasted in a 1.2 m interval ring sequence into a slot situated at the end of each panel. The undercut stope was emptied through the finger raises. The undercut retreated from South to North at blast interval determined by the finger raises spacing. Fig. 1 represents the various steps involved with the grizzly method. Extraction drift dimensions were opened 1.8 m wide x 2.4 m high with anchor rock bolts and wire mesh where safety required them during excavation. Grizzly chambers were excavated at 2.4 x 2.4 x 4.6 m long on a 7.6 x 7.6 m grid spacing. Ore passes with dimensions of 1.5 x 1.5 m were developed from the haulage drift. On the extraction level, headings were drilled with jacklegs and cleaned by slusher into ore passes to the haulage chutes. The support used in the grizzly chambers was square concrete structure with 150 mn H beam reinforcement. The H beam was partially buried in the concrete and had one free face to allow for difference frequency of blast vibration between concrete and steel. The supported brow of the chamber had an opening 1.5 x 2.1 m. Ore passes were ring concreted 150 mn thick without any reinforcement. A 24 MPa compressive strength concrete was pumped and poured in pre-assembled forms. Based on the success of this method on the first level, the same layout was repeated on the second level. With the start of undercutting on the second lift, signs of deterioration were noticed in extraction drifts. At first, there was great concern as the operators were confident that standard repair techniques could cope with such a situation. An intensive program of support repair and a reduction of draw resulted. The following method of repairs were used: 1) Steel square sets of 150 mn H beam at 0.6 m intervals were installed. 2) This was reduced later to 0.3 m interval and eventually to a skin to skin steel structure. 3) Yieldable arches were introduced spaced at 0.9 m intervals, linked laterally with 150 m. H beam. 4) The yieldable arches spacing was then reduced to 0.46 m and eventually installed skin to skin. However, this support was not successful.

Jan 1, 1981

By M. van Swaay, C. E. Birchenall

A. S. lBrling (Johnson, Matthey & Co. Ltd., Laboratories)— Because of its initial emphasis upon the production of membranes by powder metallurgy and by normal casting and rolling techniques, this paper is of considerable interest to those concerned with the design and application of industrial diffusion units. As the subsequent performances of the three grades of palladium were not compared in detail, it can perhaps be concluded that specific permeabilities were very similar. A short table in which the absolute diffusion rates obtained by the Authors with their three grades of palladium were compared with those of other investigators18-25 would, however, have been of particular value in view of the very variable results obtained with this membrane material. The Authors state early in the paper that the permeability of the thoriated samples decreased in much the same way as that of the nonthoriated samples. Later, they emphasize that sintered palladium without thoria was very susceptible to poisoning and did not respond as well as the other materials to the decontamination treatment. These results, which suggest that sintered membranes are less effective than those produced by normal methods, have considerable industrial implications, and amplified experimental details would be very welcome. The results of the Authors differ in one important respect from those of other investigators. Thus, no "bleeding" was required to maintain a constant rate of diffusion, although Davis, Darling, and De Rosset found this to be necessary. Davisz3 found that "bleeding" was necessary even when the hydrogen had already been purified by diffusion through a palladium tube, and it would be of value to know the purity of the gas stream emerging from the purification train shown on Fig. 1 of the Authors' paper. The Authors show that diffusion rates varied according to the square root of the pressure difference providing that the palladium membrane was not contaminated in any way. This finding is in agreement with the results of those workers2,18,19,23,24 who diffused their hydrogen through the membrane into a partly or completely evacuated system.Those workers who did not find this square-root law dependence did not have a partial vacuum on the downstream-side of the membrane.'' The difference between the two experimental con- ditions appears to be significant, as the absolute diffusion rates per sq cm of diffusion area are lower when the square-root law dependence is not observed. While the effect could be attributable to poisoning of the membrane it is conceivable that a positive pressure on the downstream side of the membrane might influence the mechanism of diffusion. In view of the capricious behavior of palladium, factors of this type, which are likely to influence its industrial significance, should be carefully considered. M. van Swaay and C. E. Birchenall (authors' 9-eply) — Our Eq. 191 may be compared with several others for hydrogen diffusion in palladium: D = 5.95 x exp (-5770/1)' D = 3.55 x 10"3 exp (-5550/)' D = 4.3 x 10"3 exp (-5620/1')' Other values are given in the literature, but in many cases surface poisoning may have affected the results. No analysis was performed on the hydrogen gas stream after purification. It should be noted that the presence of liquid nitrogen traps near the heated membranes may have set up convection currents and provided the equivalent of "bleeding." The question of whether a partial vacuum existed on the downstream side of the membrane is not clear. Does it imply that there is something unique about the permeability measured near one atmosphere pressure? We do not believe that there is. When square root pressure dependence is not observed, diffusion rates are not measured. Is "absolute diffusion rate per sq. cm. of diffusion area" equivalent to permeability? The terminology is new to us. In any case we doubt very much that pressures of the order of several atmospheres can affect the mechanism of diffusion.

Jan 1, 1962

By Pol Duwez

The effect of the rate of cooling on titanium, zirconium, and thallium has been measured. For titanium-molybdenum alloys, it has been shown that for molybdenum concentration up to 8 pct the rate of cooling has no effect on the transformation temperature, but this temperature decreases progressively with increasing molybdenum content. HIGH strength to weight ratio and remarkable corrosion resistance have often been advanced as the main reasons for the present widespread interest in titanium. For the physical metallurgist, the existence of an allotropic transformation in titanium is another important factor. As in the case of iron, an allotropic transformation may be the fundamental property upon which the response of Ti-base alloys to heat treatment will depend. It is therefore important to study the mechanism of the allotropic transformation in pure titanium and the effect of alloying elements on this transformation. The existence of an allotropic transformation in titanium was reported in 1931 by Schulze.' Later, De Boer et al.' determined the transformation temperature from a discontinuity in the electrical resistivity at 882"42O°C. According to recent work," the transformation temperature is 882.5"&1°C. The crystal structure of the room temperature a phase is hexagonal close-packed and the high temperature fi phase is body-centered cubic.' It is well known that the high temperature /3 phase of pure titanium cannot be retained by quenching to room temperature. Several investigators'-' have shown that in alloys of titanium with metals which are soluble in the @ phase (for example, nickel, molybdenum, chromium, or manganese), the /3 structure can be retained, providing the concentration of the alloying element is greater than a certain critical value. Below this critical value, the alloys transform during quenching, at least partially, into a supersaturated solid solution having the a. structure. This behavior is very similar to that found in some iron binary alloys (Fe-Ni and Fe-Mh, for example) and is an indication that the transformation might occur by means of a shear mechanism analogous to that observed in the austenite-martensite reaction. The present investigation is mostly concerned with the effect of the rate of cooling on the /3 to a transformation. In the first portion of this paper, the results obtained on pure titanium are described. Two other pure metals, zirconium and thallium, were also investigated, because they both have an allotropic transformation like titanium, from an hexagonal close-packed to a body-centered cubic structure. For purposes of comparison, the effect of rate of cooling of the y to a transformation of iron was included in the experimental program. The second part of this paper deals with Ti-Mo alloys. The equilibrium phase boundaries involving the solid state reactions on the Ti-rich side of the system were determined and a study was made of the effect of the rate of cooling on the transformation of the high temperature /3 solid solution. Experimental Procedure Since the main object of the present investigation was the determination of the effect of the rate of cooling on a transformation temperature, the best technique available was that used by Greninger" in his study of the martensite arrest in carbon steels. This method consists of heating a very small sample of metal to which fine thermocouple wires are .attached, cooling the sample rapidly by means of a blast of helium, and recording the temperature vs. time curve on an oscillograph. The apparatus used in the present experiments was very similar to that described by Greninger, except that the heating coil was made of molybdenum wire (0.040 in. in diam) and the assembly was placed in a bell jar under vacuum of 10" mm Hg or less. The specimen con-

Jan 1, 1952

By Herbert H. Kellogg

Graphs representing the standard free-energy of formation as a function of temperature for 21 fluorides are presented, along with estimated values for the standard free-energy of formation of 20 atedadditional fluorides. A few of the many possible uses of these data in metallurgical calculations are discussed, including the fluorination of oxides, sulphides, metallurgicaland chlorides, and the reduction of metal fluorides. RECENT papers which have presented free-energy data for oxides, sulphides, chlorides, carbonates, sulphates, and silicates in the form of free energy vs. temperature plots,1-5 have found important uses in teaching and metallurgical development work. This method of presentation of thermo-dynamic data serves to make available in readily usable form thermodynamic constants which are scattered throughout the literature, and to show by graphical means the stability relations which exist between the compounds of a given type. It is certainly desirable to have these free-energy-temperature diagrams for as many types of compounds as are of present or potential use in metallurgical processes. Thus, even though there are but few uses of metallic fluorides in extractive metallurgy today, the potential uses of fluorine processes are of great importance and serve as the principal justification of this paper. Recent developments in the production of fluoro-carbons have resulted in vastly improved methods for the production and handling of fluorine and corrosive fluorides, with consequent reduction in costs.".' The extractive metallurgist should no longer overlook possible fluorine processes when development of a new process for a relatively high unit-price metal is being considered. In a previous paperv he author outlined in some detail the importance and use of free-energy data in metallurgical calculations and also discussed the properties of a standard free-energy vs. temperature diagram. The same method of presentation is adopted in this paper, and the reader is referred to the earlier work for explanations of the use of free-energy data. Thermodynamic Data This paper presents standard free-energy vs. temperature diagrams, Figs. 1 and 2, for those fluorides for which the major thermodynamic constants are known. In the calculations of the standard free-energy of formation (AGO), values of the enthalpy of formation at 298°K (?Ho,) were taken from "Selected Values of Thermodynamic Constants"8 most of the values of standard entropy at 298°K (S°298) were taken from "Selected Values"," but in a few cases the values given by Kelley9 ere preferred; data for the Phase changes came from "selected Values" and several of Kellley's publics- tions;0-12 and most of the specific-heat data were taken from Kelley.l0 The appendix gives a detailed list of the sources of the data. As explained in an earlier paper,6 he accuracy of some of the standard free-energy relationships is not high. An error of +1 kcal at 1000°C is expected in most of the curves of Figs. 1 and 2. The error may be as high as +3 kcal in some of the curves. Rather than attempt to estimate the reliability of each curve, the source of the data used is reported in the appendix, and the reader may compare these data with newer values as they become available. Figs. 1 and 2 fail to show values for the fluorides of many important metals. In most cases this is because the entropy of the metallic fluoride is unknown. For preliminary calculations it is often useful to have available the best estimate of an unknown datum, rather than no information at all. With this in mind, Table I lists estimated standard free-energy values for a number of important metallic fluorides not included in Figs. 1 and 2. The values reported in Table I were, calculated by Brewer et al.13 and are based on estimated entropy values. The estimated uncertainty of the values for each fluoride were calculated from the uncertainty values given by Brewer1' for ?H°, and the entropy function.

Jan 1, 1952

Charles Catlett, Staunton, Virginia (communication to the Secretary*): I have had occasion to examine a few of the irondeposits in the immediate section of which Mr. Watson speaks, but have not had an opportunity to visit any of the well-known manganese-deposits. I find the former can be very safely read in light of the information which it is possible to get from the same measnres farther. north, where they are less completely decomposed. In the same way all of his conclusions in regard to the geology of the manganese-deposits bear out their occurrence in Virginia, when we allow for the far more complete decomposition in the section he has so carefully studied. Judging from the same measures farther north, I think he will be safe in agreeing even further with Penrose as to the origin of these ores. Some years ago I carried on prospecting work in these measures in Virginia, in which the iron-ore and manganese-ore were followed down to undecomposed material, and in which their occurrence along a definite line of stratification, and apparently a part of the original bedding, was plainly shown. This is unusual, however, even in the section of which I speak. At Crimora, Virginia, the decomposition is quite complete; at the same time the results of some hydraulic work, which has been done there, disclosed, at the time of my last visit, the manganese interbedded in the residual clay along a definite and distinct plane parallel to the bedding of the underlying quartzite, and which, as is shown at other points, corresponds with the plane of the original material. In view of the phosphorus reported by Mr. Watson as existing in the Cartersville ores, and the not uncommonly prohibitive amount in southern ores, I am interested to know whether

Jan 1, 1904

JESSE L. JONES,* Pittsburgh, Pa. (written discussion?).-As the die-casting process is so very different in character from the process of making sand molds, it is often considered that entirely different methods of pouring, gating, venting, etc. should be used. There is really, however, no essential difference in the making of (lie castings and sand castings, and similar methods should be used in each process. In the matter of gating, the metal should be introduced at a central point, as nearly as possible, so that it will have an equal distance to flow from the point of entrance to the most distant points of the mold. This will cause a uniform rate of congealing of the casting and prevent streaks and cold shuts. The venting should be done in such a way that a free exit of the air in the molds can occur. It should be less difficult to take care of the venting of a die-casting mold than to vent an ordinary sand mold. In the case of a sand mold, the venting is left, to a considerable extent, to the judgment of the molder, and it is possible that no two molds will be vented in a similar manner. Further than this, after a vent has been made in a sand mold, it may become clogged by the sand and for this reason be inefficient. There is also quite a variation in the pressure of the metal entering a sand mold, due to varying heights of the pouring gate. In a die-casting mold these factors can be controlled more closely. The vents should be so disposed that the air in the mold compressed by the entrance of the metal may be able to leave the mold at a uniform rate and by exits located symmetrically. These exits are made quite small on molds at first, as they can he easily enlarged if necessary, and they are tapered so that a free flow is guaranteed without danger of the metal spurting out from the die. Uniformity of pressure of the metal as it enters the mold is very important and, as the pressure is mechanically applied, its control is not difficult. It is true that a sand mold has much less of a chilling effect on the metal poured into it than has the die-casting mold, but, outside of this point, there is a great similarity between the die-casting process and the process of making castings in sand folds. It is suggested that much would be gained by regarding these two processes as not essentially different.

Jan 4, 1919

By H. E. Cline, T. H. Alden

A study zvas made of rate-sensitive plastic deformation and superplasticity in alloys of lead and tin. These alloys (lead, PO-19 pct Sn, Sn-38 pct Pb, Sn-2 pct Pb, tin) were extruded, aged at room temperature, or melted and resolidified to produce a variety of ~nicrostrnctures. Flow stress us strain rate data were obtained frorn tension tests for strain rates between 10-6 and 1 min-1. The curve log o .us log £ was S-shaped jor fine-grained materials and approxinzately linear for coarse-grained nzaterials. At constant grain size, the behavior was relatively insensitive to conposition. High rate sensitivity (d log o/d log k) and superplasticity occurred at intermediate strain rates in fine-grained materials and are believed to be associated with a transition with strain rate in the mode of plastic flow. This transition was shifted to higher strain rates with increasing temperataire or decrensing grain size. The high rate rneclzanisrn is presunzed to be slip, while rnetallographic evidence sug-gests that the low rate lnechanism is pain boundary sliding. PEARSON' discovered that extruded eutectic alloys of Pb-Sn and Bi-Sn could be elongated as much as 2000 pct in tension. The ability for stretching decreased with aging time or annealing to increase the grain size. At high strain rates, or if the material was in the cast condition, normal ductility was observed. Following deformation of the extruded Pb-Sn eutectic at low rates, Pearson observed an equiaxed granular structure on an initially flat surface, while rapid straining produced elongated grains. He attributed the large deformation in the extruded alloys to the persistence of extremely small grains to a temperature sufficiently high for inter granular flow. Avery and backofen2 measured the strain rate sensitivity of the flow stress, m = d In old In 6, in the Pb-Sn eutectic and established a correlation between m and the tensile elongation. In the extruded eutectic alloy the strain rate sensitivity was 0.1 to 0.2 at rapid rates and the elongation was small, while at low rates m increased to 0.4 to 0.6 and superplastic elongation was observed. They also noted a grain size effect. In the case of the cast Pb-Sn eutectic the strain rate sensitivity remained at 0.1 over the range of strain rates of their experiment (3 x 10"3 to 2 min-I). These authors suggested that diffusional (Nabarro-Herring) creep was the mechanism by which deformation occurred at low strain rates, while climb-controlled creep occurred at high rates. Two predictions of this model are that, at low strain rates, the strain rate sensitivity approaches 1, i.e., Newtonian viscosity, and that the strain rate at constant stress varies as D/L2, where D is the coefficient of self-diffusion and L the grain size. More recently, a mechanical and microstructural investigation of the dilute superplastic alloy, Sn-5 pct Bi, has been done.3 The results show that the high strain rate sensitivity is associated with a transition with strain rate of the mechanism of plastic flow. At low strain rates, grain boundary sliding and its associated accommodation processes were evident, while at high strain rates quasi-uniform slip was concluded to be the dominant deformation process. The following experiments were performed to extend our knowledge of the phenomena of superplasticity to a larger range of strain rates, compositions, temperatures, and microstructures in the Pb-Sn alloy system. The question of why a cast structure does not exhibit viscous behavior although it appears to have a fine microstructure2 was investigated.

Jan 1, 1968

By T. B. Massalski, C. S. Barett

THAT metals and alloys of the body-centered-cubic structure tend to become unstable at low temperatures is so nearly universal that any exceptions are worthy of special attention. Studies of the exceptions may disclose unrecognized examples of metastability or may shed light on the nature of some of the factors that stabilize the body-centered-cubic phase. Among the structurally analogous body-centered-cubic 3/2 electron compounds, the ß-phase in the Cu-Zn system deserves further attention for, although this phase is known to undergo partial mar-tensitic transformation on cooling below room temperature to the temperature of liquid nitrogen when the composition is less than about 42 wt pct Zn, it does not transform on cooling .when there is more than this amount of zinc present.1-4 The present authors recently found that an alloy containing 48.35 wt pct Zn could be transformed, however, if deformed severely at room temperature or lower temperatures.V his discovery led to the suggestion that the jerky flow of ß-brass single crystals6 and some of the unusual temperature variations of the yield strength and hardness are due to strain-induced transformation during the tensile tests. The present investigation is an extension of that work to cover the entire available range of compositions of Cu-Zn ß-phase alloys and certain interesting compositions of the ß-phase in the Cu-Zn-Ga system. Particular attention is given to the structure of the transformation product resulting from cold work, which is found to vary with alloy composition, and to the temperature range in which transformation can be induced in the various alloys. The composition limits of the body-centered-cubic phase in the Cu-Zn system, based on a recent review by Raynor7 and the precision determinations of Beck and Smith: are shown in Fig. la; in the ß region the alloys are disordered and in the ß region they are ordered. The rate of ordering is so rapid that a high degree of order is found in any of these alloys immediately after quenching. Experimental The nine binary and four ternary alloys of this investigation were prepared from cathode copper (99.99 pct purity), electrolytic zinc (99.99+ pct), and gallium (99.98+ pct). All alloys were cast in transparent Vycor tubing, homogenized at temperatures between 800° and 890°C, and quenched in water. Ternary alloys were cast in small amounts (-5 g) to predetermined compositions to fall along a line of constant electron concentration in the ternary system. Changes of weight during the casting operation of the ternary alloys were not greater than 1 part in 2500 from the intended nominal weights and therefore their compositions were accepted without chemical analyses. All binary alloys were cast in larger amounts (100 to 150 g), homogenized, and hot rolled after preheating to 800°C. The central portion of the rolled strip of each alloy was annealed for eight days and quenched in brine. All binary alloys were analyzed chemically. The compositions, heat treatments, and metallographic appearances of all alloys are tabulated in Table I. Various samples were subjected to heat treatment or cold work at several temperatures and were then examined metallographically or by means of X-rays. Specimens about 6x6x3 mm in size were examined metallographic ally to confirm the presence of the ß-phase after quenching. Cold work was introduced by fastening each sample between two pieces of steel, cooling the assembly to the desired temperature, and transfering it rapidly to a vise where moderate or severe compression was immediately applied. Cold working at liquid helium temperature was done by a chisel-shaped tool mounted on an X-ray spectrometer, described elsewhere.% A!! metal-

Jan 1, 1958