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US 4,152,143-Continuous precipitation of cement copper from an aqueous ore leach solution mixed with pieces of iron as the precipitant Copper depositing on the pieces of iron is loosened and removed therefrom by means of constant but regulated oscillating movement of the pieces of iron in a horizontal elongated chamber, and the loosened copper is separated and collected from the mixture E Kausel and R Nissen, assigned to Klockner-Humboldt-Deutz A G May 1, 1979 8 pp (75-100) Filed 1-12-78 (868,981) (Drawings below) [ ] US 4,156,711-Removal of metal impurities from an acidic zinc or cadmium solution prior to electrolysis. Impurities such as manganese, cobalt, nickel, and thallium are selectively precipitated by contacting the solution with persulfuric acid or an ammonium or alkali metal salt thereof while maintaining a pH value of from 1 5 to 4 5 This patent is a continuation-in-

Jan 1, 1980

By J. R. Ross, J. B. Rosenbaum

Bureau of Mines research has resulted in the development of fluid- bed ion-exchange columns for recovering uranium from slime pulps. In pilot plant tests, slime slurries containing up to 6 percent solids were processed at flow rates of 10 gallons per square foot per minute with high uranium recoveries and efficient resin loadings. Uranium was effectively eluted in a laboratory fluid-bed elution column at eluate-to-resin ratios of less than 5:1 and eluate flow rates of 3 gallons per square foot per minute. Construction costs of mills using these improved ion exchange techniques are estimated to be 25 percent less than for mills using solvent extraction of clear solutions. For mills having a capacity of 2,000 to 2,500 tons of ore per day, the saving would be in the range of $2.5 million. In addition, a saving of about $0.80 per ton of ore in total operating costs is indicated.

Jan 1, 1973

Single orders 2.5 c. Pamphlets 10. c. each in lots of three or more. Pamphlets 5 c. each in lots of fifty or more. These prices prevail for orders for pamphlet, of the same or different titles. The pamphlets listed on the following sheets are advance copies printed to facilitate discussion at the meetings of the Institute. They are offered for sale at the reduced prices given above as long as the supply, lasts. This list is published in the Bulletin in order that members may have the first opportunity to secure pamphlets, which sometimes are in such great demand that the supply is exhausted before the wants of members can be supplied. The following list includes only a fraction of the pamphlets that have been published by the Institute. Any other paper published by the Institute may be obtained for the price of $1, except those published in Volume XXXI, which are rare.

Jan 5, 1917

By Simon D. Strauss

The world appetite for minerals in the, third quarter of this century grew at a higher rate than had been anticipated. To illustrate, consider the experience of four, commodities. Excluding the Communist bloc, sometimes referred to as the centrally planned economies, demand for aluminum increased at a compound rate of 8.6% between 1950 and 1975,; copper rose by 4.4%; iron ore by 5.5%; and tin, the laggard in the group, by 2%. Except for tin, the figures are substantially greater than growth rates anticipated in 1950 in the Paley Commission report and other studies. The growth rate was not evenly distributed in geographical areas. Professor Wilfred Malenbaum of the University of Pennsylvania did an interesting study breaking these figures down as among three principal sources of demand -- the United States, other industrialized nations (which he referred to as the "rich lands"), and the developing world (which he referred to as the "poor lands").

Jan 1, 1982

By J. S. Browning

The pegmatites of the Kings Mountain-Lincolnton, N. C., area constitute the largest known domestic reserve of beryl and spodumene. The reserve is estimated to contain 90 million tons of pegmatic material with 1,280,000 tons of recoverable Li2O (lithia) as spodumene.1 The pegmatites also contain 0.4 to 0.5 pct beryl disseminated throughout the orebodies. The pegmatites may contain a potential reserve of 240,000 tons beryl, equivalent to approximately 34,000 tons of BeO. Different flotation methods for separating beryl from feldspar or quartz, or both, have been developed by various investigators.2,3,4,5,6,7 On the other hand, published information is limited on concentration of spodumene-beryl ores. As the response of beryl and spodumene to flotation is essentially the same, a successful separation of the two minerals depends upon use of a selective depressant or a selective collector for one of the minerals.

Jan 7, 1961

We did install one 100% brick bottom in our #33 furnace which is basically the same design as Inland's furnace. We had previously embarked on a program of replacing all bottoms in our 300 ton furnaces every 2nd campaign which would be about every 2000 - 2300 heats. This had been necessitated by the effect of our rather high oxygen blowing rates and our desire to maintain a minimum bottom interval level. This meant that we were able to compare bottom performance of various types of materials on a realistic bas is. Since furnace availability is critical to our operation, we are organized to employ every piece of equipment and all the necessary man power to complete a rebuild in the shortest possible time. A 300 ton furnace requires 7.5 days to rebuild. If a new bottom is to be installed an additional 2.5 days is added - 24 hours for tear out and 36 hours for bricklaying - making a total of 10 days.

Jan 1, 1972

By Robert Longyear

IN, diamond-drill work, a true sample consists of all the material cut by the bit-both core and cuttings. As the recovery of this sample is the object of diamond drilling, the utmost care should be taken to secure it. Speed of drilling and low costs are of little value if an inaccurate sample is obtained. The engineer in charge must study his material and lay out the plan of sampling, and then see that the drill runner follows his instructions; for the runner may be more interested in obtaining a large footage than in developing accurate methods of sampling. FIG. 1.-CORE BOX. When the core has been removed from the core barrel, it should be placed in a core box in the exact order in which it is taken from the ground. This box, Fig. 1, is usually a shallow tray 4 or 5 ft. (1.2 or 1.5 m.) long, with partitions running lengthwise between which the core

Jan 12, 1921

By L. W. Bahney

Many methods for the determination of gold or silver, or both, in cyanide solutions have been published, which with care in manipulation, and modification in some cases, will give results that are satisfactory. It is possible to classify or group these methods as follows: 1. Evaporating the solution in a porcelain or agate-ware dish containing litharge,l or in a "boat" made of lead foil. 2. Forming a lead sponge containing the precious metals by means of zinc shavings,2 zinc dust,3 or a piece of aluminum.4 3. Decomposing the cyanide solution with an acid and precipitating the precious metals by the use of one or a combination of some of the following: Copper sulphate,5 sodium sulphite,6 hydrogen sulphide,' cement copper.ll 4. Precipitating the silver by zinc dust held in a Gooch crucible and determination with a standard solution of sulphocyanate.9 5. Electrolysis.l0 . 6. Colorimetry.ll

Jan 1, 1915

F. G. SMITH.-Probably someone will ask whether I discovered why the bottoms of the large shells broke out. I did not, as a result of this investigation. An experiment was made along the lines indicated in this paper, to determine whether abnormal grains greatly affected the physical properties of brass. Two ordinary test bars were annealed for 1/2 hr. at 750° C. and physical properties determined on one. The other was covered with indentations made with a peen hammer and then reannealed. for 5 hr. at 750° C. It was found in the tensile test to be made up of large grains 1/4 to 1/2 in. in diameter. The physical properties, however, differed from those of the first bar only as much as might be expected after a 5 hr. anneal under normal conditions. It appears then that the large grains produced in this manner do not ruin the physical qualities of the brass.

Jan 12, 1919

Michigan State Department of Conservation, Lansing, Mich The Department of Conservation has two divisions issuing publications which should be listed in this directory. Geological Survey Division. R. A Smith, State Geologist Land Economic Survey Division L R Schoenmann, Head. A price list of publications of either division will be sent upon request to that division Geological Survey Division.-Citizens of Michigan may obtain publications of this Division on payment of forwarding charges Prices to others for available publications are given below: Vol 5 (1881-1884): Pt 1, Geological report of the Upper Peninsula of Michigan, by L L Hubbard, pt 2, Geology of Lower Michigan with reference to deep borings, by A C Lane, $125. Annual Report for 1908. Pt b, Geological section of Michigan, by A C. Lane and A E Seaman, 50 cents. Publication No 5, The Late Glacial and Post Glacial Uplift of the Michigan Basin, and earthquakes in Michigan, by W. H

Jan 1, 1933

By R. A. MacGregor

The Stanrock mine of Stanrock Uranium Mines Ltd. is located on Quirke Lake in the Elliot Lake area of northern Ontario, about 25 miles north of Lake Huron. The property was developed and brought into production at a rate of 3000 tons of ore per day during the uranium boom of the mid-1950's. The mine workings are from 1200 to 2100 ft below sea level. Mining was done by the room-and-pillar method with 65 to 80% extraction. The plant is located at an elevation of 1400 ft above sea level. The orebodies are conglomeratic beds, 6 to 40 ft in thickness and dipping 5º to 40º. The ore is a quartz pebble conglomerate with a pyritized sericitic matrix. The ore minerals are brannerite, frequently intergrown with anatase or rutile, uraninite, and some monazite and minor coffinite and thucolite. Sulfides constitute 5 to 10% of the ore as pyrite with minor amounts of pyrrhotite, chalcopyrite and galena.

Jan 3, 1969

By J. C. Donnell, O&apos

Sinking an inclined ventilation shaft at the Never Sweat mine of The Anaconda Co. has required a unique underground hoisting arrangement because the shaft changes direction from vertical to 71.5º. Access to the project is made through the High Ore shaft to the 2800-ft level, then by crosscut to the bottom of the vertical Never Sweat shaft. The 71.5º incline shaft starts at this point, which makes an unusual operation as the 60-cu ft sinking skip coming up the incline changes into a vertical position above the 2800-ft level before going into the dump scrolls. This requires both rollers and guide shoes on the skip. Coming up the incline to the collar of the shaft the loaded skip enters into a guard before reaching the vertical section. The tendency of the surface- mounted Never Sweat hoist is to lift the front wheels of the skip off the track, so the guard keeps the skip on the rails during the transition.

Jan 11, 1965

We would like to thank Mr. Mandolesi for his informative paper on rails from strand cast steel. The chemical and structural properties of the strand cast steel were of particular interest to us. We would like to supplement his excellent report with some of Inland's findings from our Caster with submerged nozzles and strands reduced in line from 7" x 7" to 5-5/8" square cross section. Inland has conducted extensive segregation studies on AISI 1049 steel - Fine Grain 0.50% carbon and 0.75% manganese. Based on approximately 80 heats, our normal segregation pattern results in analyses of .49% carbon in the center, and 0.50% carbon at the midway and edge position. The sulfur analysis averages .025% in the center, .027% midway, and .026% at the edge. Note the slight negative segregation between the center and midway position. This steel, being lower carbon and probably cast nearer the liquidus, resulted in less segregation than the 0.80% carbon rail steel.

Jan 1, 1972

By Robert Glass Cleland

[PHELPS DODGE COPPER PRODUCTS CORPORATION OFFICE, 40 WALL STREET, NEW YORK 5, N. Y. OFFICERS Whipple Jacobs President Howard T. Brinton Vice-President Edgar P. Dunlaevy Vice-President Weightman Edwards Vice-President S. Allan Jacobs Vice-President]

Jan 1, 1952

By David J. Mack

A SURVEY and critical appraisal of published information about Young's modulus was originally made by the writer because of a complete lack of information about this very important quantity in works on mechanics, physical metallurgy, physics, and other sciences. It was felt that a comprehensive summary of such information about Young's modulus might be of general interest and may suggest new problems or lines of attack on other problems that involve E. Hence this paper has been prepared even though it is only a review, with no new ideas or experimental data. The references are only those used in assembling the paper. No attempt was made to compile a complete bibliography on the subject of Young's modulus. CALCULATION OF YOUNG'S MODULUS FROM THEORETICAL OR EMPIRICAL CONSIDERATIONS Many attempts have been made to compute E from theoretical considerations. The earliest calculations were probably those of Tomlenson (1883) and Southerland (1891), but Fessenden 41,42 made extensive calculations a few years later and arrived at the relationship: [2E = 78. 101 (_L V] where V is the atomic volume. In 1923, Peczalski,43 working from the same stand-point but with more information available on atomic structure, arrived at an identical relationship, which he expressed as: [E=B(m) 2] where B is a constant of value about 8 • 10 7, p is density and m is atomic weight; the atomic volume, of course, being m/p. Portevin44 immediately pointed out that while the equations of Fessenden and Peczalski were true of the common metals, they gave low values for the refractory metals with high moduli (Fig. I). He showed (Fig. 2) that much better concordance was obtained by means of an empirical equation of the form: [E _ KT'Vb] where K is a constant; T the absolute melting point; V, atomic volume, and a and b constants of value approximately I and 2 respectively. This constant K in the Portevin equation is not necessarily the same for all elements, as shown by Thompson.45 Other equations for E based upon theoretical considerations have been derived by Honda and Yamada49 and Lasareff. 50 The most recent calculations of elastic moduli based upon quantum mechanics are probably those of Fuchs.46-48 He extended the method of Wigner and Seitz for calculating the lattice energy and compressibility of monovalent metals and computed the elastic constants of lithium,

Jan 1, 1945

By Roger A. Gregg, Barry J. Piearcey

MANY of the nickel-base superalloys developed recently for use in the as-cast condition exhibit a massive "white-etching" constituent1 in the inter-dendritic regions. Commercial alloys in this category are SM 200,* IN 100, INCO 713, and Nicrotung. The appearance of a similar microconstituent in nickel-rich Ni-A1-B alloys has been reported by Schijbel and Stadelmaier. Their investigation revealed that this constituent was the binary eutectic of the terminal nickel-base solid solution and the inter metallic based on Ni3A1. This binary eutectic is degenerate and NhA1 is the major phase. At lower temperatures the eutectic composition lies within the NkA1 phase field and under equilibrium conditions is single-phase NisAl. Taylor and F&apos;loyd3 have shown that in Ni-Al-Cr alloys containing at least 8 at. pct Cr, liquid compositions which solidify by the eutectic reaction in the nickel-rich portion, precipitate nickel-base solid solution and NiAl rather than nickel-base solid solution and NkA1 in the binary Ni-A1 system. Since the nickel-base alloys contain chromium in excess of 8 at. pct and are further alloyed with one or more of the elements titanium, cobalt, molybdenum, or tungsten, it is possible that the eutectic could contain NiAl rather than NisAl. In addition, Benson4 has reported that in low-nickel austenitic high-temperature alloys, which possess Ni/(Al + Ti) atomic-weight ratios <18.0, the Ni (Al, Ti) phase may precipitate from the melt during solidification. Since SM 200 and similar high-temperature materials were developed from alloys which were designed for solution treatment, the appearance of a eutectic would indicate that the limit of solid solubility has been exceeded. The purpose of this note is to confirm that the massive white constituent in the complex nickel-base alloys investigated is based on the binary eutectic Ni + NbAl and that the limit of solid solubility need not be exceeded to produce it, in common with other observations of cast alloys. Successive polishing of a sample of SM 200 showed that, in agreement with Schobel and Stadelmaier, particles of the constituent were spherulitic and in particular were a) situated between cored dendrite arms, Fig. 1, and b) nucleated at the surface of dendrites, Fig. 2. The Ni/(Al + Ti) atomic-weight ratios for the nickel-base alloys which were observed to contain the massive eutectic constituent in the interdendritic regions are 12.1 (Nicrotung), 9.2 (IN loo), 19.5 (INCO 713), and 14.5 (SM 200). However, the results of X-ray analysis of these alloys in the as-cast condition failed to reveal the presence of the Ni (Al, Ti) phase. An electron microanalyzer was therefore employed to analyze the composition of this constituent in SM 200. The results of analyses of representative particles are as follows5: 8.4 at. pct Ti, 8.8 at. pct Co, 5.5 at. pct Cr, 0.9 at. pct W, 12.8 at. pct Al, and 63.6 at. pct Ni. Assuming that

Jan 1, 1964

By David L. Holt, Walter A. Backofen, Anwar-uI Karim

Specimens of a hydrided Mg-0.5 Zr alloy were strained in tension at 500°C and constant rates of 2 x10-3 5 x 10-3, and 2 X 10" min-1. Hydride-denuded zones formed at grain boundaries normal to the tensile-stress direction as a result of magnesium transport during difusional flow. The width of the zones could be measured and the measurement used for calculating the diffusional component of the imposed tensile strain. The strain from diffusional flow was found to increase with imposed strain at a diminishing rate, tending to saturate at approximately 12 pct. Strain rate sensitivity of flow stress was low. The apparent non Newtonian character of the diffusional flow is attributed to a non Newtonian process acting in parallel with it which could be boundary shear. Fracture grows out of voids that form in the denuded zones. DEFORMATION of a grain by diffusion of atoms from boundaries stressed in compression to boundaries stressed in tension is Newtonian viscous,1-3 and evidence has accumulated in recent years that such a process may be responsible for the high strain-rate sensitivity of the flow stress of super-plastic alloys.4"7 One piece of evidence is that experimental stress: strain-rate relationships can be quantitatively explained.5-7 There is also metallo-graphic evidence of diffusional flow in superplas-ticity, but in a limited amount. The formation of striated bands on the surface of superplastically deformed specimens has been attributed to diffusional flow.5"7 The basis of that attribution came from experiments on a coarse-grained, nonsuperplastic and hydrided Mg-½ wt pct Zr alloy which formed hydride-denuded, light etching zones at tension-stressed boundaries when strained in tension at 270?C.6 The origin of these zones had already been traced to the diffusional flow of magnesium atoms to the boundaries.&apos; The particular observations in the more recent work were of striated-band formation on the surface and denuded-zone formation internally, with both the bands and zones having the same width and appearing at tension-stressed boundaries. It was argued that the bands were a surface manifestation of the zones and hence of diffusional flow. Of course in superplastic alloys which do not contain internal metallographic "markers", the surface bands can be the only metallographic indication. In the present work, denuded-zone formation was utilized, as it has been by others,9-11 to extend the observations of diffusional flow and to measure the strain, ed, resulting from it. Grain size had to be large to measure ed with accuracy. The grain size chosen for this study was -30 , and with that a strain of 10 pct from diffusional flow produces a denuded zone only 3 µ in width. The large grain size naturally precludes superplasticity. The observations of diffusional flow were complemented by determining the strain from the other operative deformation modes: slip, e,, and grain boundary shear, egb. An incremental specimen extension is the sum of increments from slip, and grain boundary shear as well as diffusional flow. Division by a common length is required to convert to strain. If this length is taken as the initial specimen length, then imposed engineering strain, e, is given in terms of the component engineering strains by e = ed + es + egb [1] Stress:strain-rate relationships are determined by the way in which this "strain balance" is made up. EXPERIMENTAL Material. Zirconium hydride markers were introduced into the Mg-0.5Zr alloy by annealing in hydrogen at 450°C for 30 min. The hydride concentration was particularly high at zirconium rich stringers, which was fortunate in that the transverse boundaries at which denuded zones form lie perpendicular to the stringers. Grain size after annealing was 30 µ. Photomicrographs of unstrained and strained material are shown in Fig. 1. Procedure. Specimens were strained in tension with an Instron machine at crosshead velocities of either 2 x 10"3, 5 x X or 1 x 10-2 in. min-&apos;. Specimen length and diameter were 1.0 and 0.2 in., respectively, so that initial strain rates in tests at constant crosshead speed were 2 x 10"3, 5 x X and 1 X l0-2 min-1. Tests were made at 500°C which is a compromise temperature at which diffusional flow is still measurable but grain growth is not active enough to interfere with metallographic measurements. The tests were made in a hydrogen atmosphere. Strain Balance. An equation additional to [I] is eg = ed + es [2] where eg is strain measured from grain elongation. Measurement was made of ed, eg, and, of course, e, which enabled all the strains in Eq. [I] to be determined. For this purpose, strained specimens were sectioned longitudinally, polished, and etched. The strain from diffusional flow, ed, was computed by measuring on photomicrographs the width in the tensile direction of denuded zones at either end of a grain XI, X2, adding them, and dividing by twice the initial longitudinal grain dimension L0, Fig. 2. Reported values are the results of measurements on seventy randomly selected grains; 95 pct confidence limits on ed were +1.5 pct strain. To measure eg, the maximum length, L, and the maximum width, W,

Jan 1, 1970

By G. R. Leverant, M. Gell

The high- and low-cycle fatigue poperties of MAR-M200 directionally -solidified into columnar-grained and single crystal forms were determined at 1400" and 1700°F. These results were compared with the corresponding properties of conventionally -cast MAR-M200. The low-cycle fatigue lives of the columnar-grained and single crystal materials were similar at both temperatures and were one to two orders of magnitude greater than those of conventionally-cast material. The variations in the fatigue lives among the three forms of MAR-M200 were related to the more rapid rate of intergranular muck propagation compared to that of transgranular propagation. In conventionally-cast MAR-M200, cracks were initiated in grain boundaries and crack popagation occurred rapidly along an almost continuous grain boundary path. In the columnar-grained material, crack initiation occurred on short transverse segments of grain boundaries, but crack propagation was transgranular. The fatigue lives of columnar-grained and single crystal materials were approximately the same because most of the life in both materials was spent in trans-granular propagation. For the directionally -solidified materials, the number of cycles to failure, Nf, can be related to the total strain range, , by: heT = K where n and K are 0.16 and 0.044 at 1400&apos;F and 0.29and 0.098 at 1700, respectively. In addition to intergranular crack initiation in the columnar-grained material, initiation also occurred at we-cracked MC carbides and micropores in both directionally-solidified materials. At 1400°F, fatigue life was reduced with increasing MC carbide size, but at 1700 there was no effect of carbide size. THE creep and stress-rupture properties of conventionally-cast nickel-base superalloys can be greatly improved by directional solidification into either single crystal or columnar-grained forms. The improvement in properties results from a reduction in intergranular cavitation and crack growth in the columnar-grained materials and the complete absence of this fracture mode in the single crystals. This paper describes the effect of grain boundaries on the elevated temperature fatigue properties of the nickel-base superalloy MAR-M200. The effect of cycling frequency on cracking arid fatigue life and the role of MC carbides and micropores on crack initiation are also emphasized. The fatigue properties of columnar-grained and single crystal MAR-M200 at room tem- perature,4,5 and the change in the mode of fatigue crack propagation with temperature6 have recently been described. I) EXPERIMENTAL PROCEDURE The material used in this study was the nickel-base superalloy MAR-M200, directionally-solidified into columnar-grained and single crystal forms. The columnar grains were approximately 0.5 mm in diam. The nominal composition of these materials in wt pct was 0.15C, 9Cr, 12.5W, loco, 5A1. 2Ti, lCb, 0.05Zr. 0.015B, bal Ni. They were solutionized for 1 to 4 hr at 2250°F followed by aging at 1600°F for 32 hr. which resulted in 0.2 pct offset yield stresses of 150,000? 144,000, and 95,000 psi at room temperature? 1400°, and 1700°F, respectively. The corresponding elastic moduli parallel to the testing direction were 19.2. 15.0, and 12.5 x 106 psi, respectively. Specimen design, testing procedures and alloy mi-crostructure have been described previously and will only be summarized here. Following the 1600°F aging treatment. MAR-M200 contains an ordered, cuboidal, y&apos; precipitate 0.3 1 on edge, which is coherent with the 1 matrix. The y&apos; precipitate is quite stable; even after testing at 1700°F. the precipitate is only slightly enlarged and its corners somewhat rounded. The alloy also contains a small volume fraction of micropores, and MC carbides. some of which contain preexisting cracks5 formed during casting. These cracks are always parallel to the long dimension of the carbide. Measurement of MC carbide size has been described previously.5 Axial fatigue tests were conducted in air over a wide range of strain amplitudes in both the high - and low-cycle fatigue regions, with specimen lives varying from about 10&apos; to 10&apos; cycles. Low-cycle fatigue (LCF) tests were strain-controlled with strain varied between zero and a maximum tensile value at a frequency of about 2 cpm. High-cycle fatigue (HCF) tests were stress-controlled with the stress varied between 5000 psi and a maximum tensile value less than the yield stress at a frequency of either 10 cps or 0.033 cps (2 cpm). The temperature in the gage section was controlled to 52°F. Specimen axes were within 5 deg of the [001] growth axis of the single crystals and the common [001 ] growth axis of the columnar-grained material. Specimen gage sections were electro polished prior to testing. After the standard heat treatment, three specimens were coated with a typical aluminide coating applied as a slurry. An additional specimen was given the coating heat treatment without actually being coated. In all cases: specimens were reaged at 1600°F for 32 hr after receiving the coating heat treatment at 1975&apos;F for 4 hr.

Jan 1, 1970

By F. Weinberg

Lead single crystals have been deformed in tension over the temperature range of 4.2°K to the melting point. Changes in flow stress resulting from temperature cycling and strain rate cycling have been measured as a function of temperature for crystals of different orientations and purity. It was found that the flow stress ratio, after correcting for the temperature dependence of the shear modulus, decreased progressively with temperature above approximately 0.5Tm. The activation energy calculated from the high-temperature portion of the curve was found to be markedly higher than that of self-diffusion. For single glide crystals, the corrected flow stress showed an increase above 0.5 Tm before decreasitzg with temperature. This increase is attributed to static recovery occurrittg during temperature cycling. THE temperature dependence of the flow stress, based on temperature cycling and strain rate cycling, has been extensively investigated,&apos; and on the basis of these results dislocation models of the work-hardening process have been proposed. In general, the flow stress is divided into two parts, ts, the short-range interaction term, which is only effective at low temperatures and which decreases with increasing temperature, and TG, the long-range stress term, which is independent of temperature after allowing for the temperature dependence of the shear modulus. The observations demonstrating that tG/µ is independent of temperature were generally carried out at low temperatures to minimize recovery effects. Several investigations have been reported on flow stress measurements at high temperatures2"5 which demonstrate that TG/µ does not remain constant at temperatures above 0.5Tm (where Tm is the melting temperature of the material in OK). Specifically, Hirsch and warrington3 carried out temperature cycling tests at two strain rates on single and polycrystalline aluminum up to 0.8 Tm and on polycrystalline copper. For aluminum they found that the flow stress ratio (the flow stress at temperature T2, divided by the flow stress at the reference temperature T1 in one temperature cycle) dropped progressively with increasing temperature above 0.5Tm. From the slopes of the high-temperature portions of the curves, they determined an activation energy for the deformation process of 1.6 ev (at best) which they considered was in agreement with the activation energy of self-diffusion, 1.35 ev. Calculations of the activation volume demonstrated that the deformation was not controlled by dislocation climb. They proposed a mechanism in which the rate-controlling process at high temperatures was due to the rate of move- ment of vacancies away from jogs, i.e., that of self-diffusion. Results of Lucke and Buhler4 on single crystals of aluminum confirmed this conclusion. They measured the critical resolved shear stress of aluminum over a wide range of temperature and strain rates. They found that the temperature dependence of the critical resolved shear stress was similar to that of the flow stress ratio, as determined by Hirsch and Warrington, and from their data calculated an activation energy for high-temperature deformation of 1.35 ev identical to that of self-diffusion. More recently Gallagher5 has carried out a detailed investigation of the temperature dependence of the flow stress ratio of copper, silver, and gold. In all cases, he found that the flow stress ratio, after adjusting for the shear modulus temperature change, drops at high temperatures. The activation energies he determined were found to be appreciably higher than the activation energy of self-diffusion of the material being considered. The flow stress ratio was found to be dependent on the orientation of the material, and, in addition, an anomalous increase in the flow stress ratio for copper, oriented for single glide, was observed above 0.5Tm. The purpose of the present investigation was to measure the critical resolved shear stress, the flow stress ratio, and the strain rate sensitivity of lead, primarily as a function of temperature. The results should indicate whether, following Lucke and Buhler, the critical resolved shear stress of lead has the same temperature dependence as the flow stress, and, following Hirsch and Warrington, whether the activation energy for high-temperature deformation in lead is the same as that of self-diffusion. Lead deforms as a normal fee material,6&apos;7 is available in high-purity form, can readily be grown as single crystals, and, for this investigation, has the very considerable advantage of having a low melting point, 327°C. The observations of the critical resolved shear stress of lead have been published elsewhere.&apos; EXPERIMENTAL PROCEDURE The experimental procedure was essentially the same as that used in the critical resolved shear stress measurements.&apos; Single crystals of 99.999 pct (59) and 99.9999 pct (69) lead were deformed in tension with a table-model Instron in a silicone oil bath above room temperatures and in a cooled methyl alcohol or liquid-nitrogen bath below room temperatures. The test specimens were rectangular in section, 0.65 by 0.33 cm, and had a 5-cm gage length. The specimens were grown as single crystals with tapered ends, which fitted into matched tapered grips for testing. To obtain the flow stress between two temperatures, specimens were first deformed approximately 1.0 pct at the higher temperature. The test was then stopped, the load relaxed, the oil bath removed without disturbing the specimen, the grips and specimen cooled with a fan and then immersed in liquid nitro-

Jan 1, 1969

By P. W. Gilles, B. D. Pollock

THE pioneering work of Steinitz1 and Steinitz, Binder, and Moskowitz2 has shown conclusively the existence at high temperature of two additional phases in the molybdenum-boron system and thus brings to a total of six the number of structures appearing in this system. To the structures Mo2B, MOB, and Mo2B5 they have added MO3B2, a new -MOB form, and have shown that MOB,, which has the same range of composition as Mo2B5, is only a high temperature structure of the latter. This solid solution, interestingly enough, includes neither of the compositions corresponding to the stoichiomet-ric compounds, MOB, or Mo2B5, but rather at all temperatures has intermediate values of composition. These workers have also, in the course of their work, measured melting points, transition temperatures, eutectic and peritectic points in the system and have shown that Mo3B2, because of its dispro-portionation at low temperature to Mo2B and MOB, is stable only in a limited high temperature range. During the course of the present work on the vaporization properties of the molybdenum-boron compounds, a few transition temperatures were observed. When the report of the other workers appeared, it was decided to repeat, in part, their study of the system. As a result, considerable evidence has been obtained that substantiates the specific kinds of melting processes they report as well as the general features of their diagram. However, a marked difference was found between the temperatures they report and the ones observed in this study, with the latter being higher. The purposes of this paper are to present the evidence obtained in this laboratory that verifies their diagram of the system, to give some important temperatures in the system, to compare them with those previously published, and to seek an explanation of the difference. Samples The metal starting material was 400 mesh molybdenum powder with a purity stated by the manufacturer to be 99.9 pct. The initial treatment, designed to remove volatile contamination, consisted of heating in a vacuum for 10 min to a temperature of from 800" to 1000°C during which a loss of 0.3 to 0.4 pct occurred. An assay following this treatment showed it to be 99.4 pct pure, with the principal impurity probably being oxygen. The boron starting material was obtained from the Cooper Metallurgical Laboratories and the Fair-mount Chemical Co. as 325 mesh powder with manufacturers&apos; analyses of 99 pct or better. Initial treatment consisted of heating in molybdenum in a vacuum at about 1700°C for 10 min. During this time a loss of 3.5 pct occurred. An assay following this treatment showed the different samples to have purities ranging from 95.5 to 99.0 pct with iron and carbon as the principal impurities. Following the initial treatment, the elements were combined to form stocks of Mo2B and MOB by heating pressed mixtures in a vacuum to 1100" to 1200°C to accomplish reaction and to 1500" to 1900°C for a few minutes to evaporate the more volatile impurities. Analysis of the two compounds for boron by a modification of the method of Blumenthal3 and for molybdenum by the lead-molybdate method indicated them to have purities greater than 99 pct. The individual samples to be studied had compositions in the Mo2B-MOB range and consisted of mixtures of the stock compounds. Procedure As is usually the case in high temperature work the selection of containers for the samples posed some problems. For vapor pressure studies tantalum crucibles, allowing little contact with the pressed samples, were used and some of the observations made during these experiments are pertinent to the study of the phase diagram. Most of the experiments, however, were performed in graphite containers, as were those of the previous authors. Two kinds of spectroscopic grade graphite crucibles were used. One was a % in. cylinder, 3/4 in. high, containing seven 3/16 in. holes drilled 1/2 in. deep into which were packed samples of the different mixtures weighing 250 to 500 milligrams. The other, consisting of separate crucibles, was prepared by drilling 3/16 in. holes, 1/2 in. deep into 1/4 in. graphite rods % in. long. The 7/8 in. cylinder was heated directly by induction while the small crucibles were packed in a tantalum heating element for induction heating. All heating was done in a high vacuum system in which the pressure was generally less than 1x10-5mm and never rose above 2x10-5mm when the samples were hot. The general pattern of the heating in graphite was to heat rapidly to a temperature somewhat below the desired one, then to raise the temperature slowly. The samples were held for 2 to 5 min at the maximum temperature, which in all cases was far higher than that needed to produce reaction. The short time was employed to reduce possible contamination by the crucible material and to reduce composition changes that would occur because of vaporization. After examination following the heating, the samples were reheated to a higher temperature. Temperatures were measured with a Leeds and Northrup disappearing filament optical pyrometer, certified by the National Bureau of Standards, by sighting through a window at the top of the vacuum

Jan 1, 1954