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By T. Toda, R. Maddin

A study has been made of the microstructure and mechanical properties of splat-cooled aluminum-base gold alloys with gold concentration from 0.25 to 5.0 wt pct. These alloys have been quenched from the liquid state by a torsion-catapult technique, which has made it possible to pepare specimens suitable for mechanical property measwements. From the electron micrographs it has been shown that the solid solubility of gold in aluminum can be extended to 2.5 wt pct (0.35 at. pct) by splat-cooling, while the maximum equilibrium solubility is known to be less than 0.3 wt pct (0.04 at. pct). The very fine grain size (several tenths of a micron), the extended solid solubility, and the fine dispersion of a second phase (AuAl2) contribute concurrently to a substantial strengthening effect. In Al-5 wt pct Au splat-cooled specimens of less than 50 thickness, the yield strength is 17 kg per sq mm or 6 times as large as the strength of bulk specimens. For the Al-1.0 to 2.5 wt pct Au solid solution obtained by splat-cooling, the yield strength reaches 7.5 kg per sq mm after an aging treatment (for 10 hr at 200°C), while it is 3.7 kg per sq mm for the corresponding bulk specimens. A great deal of research has been done in recent years on the structure and the properties of metals and alloys rapidly quenched from the liquid state.' The term "splat-cool" has been used with the meaning of a rapid quenching from the liquid state., The splat-cooling techniques have produced large numbers of new structures, which are expressed in terms of metastable phases,3 concentrated solid solutions,4 amorphous phases,5'6 new phases,7 and so forth. Nearly all previous studies have concentrated on the physical properties; i.e., crystallography, structure, electrical resistivity, magnetism, and so forth, of the splat-cooled metals and alloys. The mechanical strength of splat-cooled metals and alloys has hardly been investigated except for some recent work by MOSS' on A1-V alloys. The principle common to all experimental techniques developed to obtain very rapid quenching rates is based on the heat transfer by conduction. Liquid must be in good thermal contact with a substrate of high heat conductivity. Both of the published devices known as the "gun" and the "piston and anvil" techniques suffer from certain shortcomings. For example, the specimen obtained by the gun technique is very small and flaky, and hence inadequate for mechanical properties measurements. On the other hand if the material is forced to yield a continuous speci- men by the piston and anvil technique, it is probable that some plastic deformation occurs during the quench. A novel method for rapid quenching of a liquid metal or alloy, the "torsion-catapult", has been devised by Roberge and Herman9 at the University of Pennsylvania. In the apparatus the melt is thrown out of a curved furnace by a catapult and impinges on a copper substrate. The apparatus has the advantage of producing a continuous foil which is relatively large in size and of a quality suitable for the measurements of mechanical properties. The quenching rate is estimated to be of the order of l05 to l06 ºC per sec, (comparable to rates achieved by the piston and anvil technique). In selecting an alloy to be studied we were made aware of the fact that gold was believed to be "insoluble" in in and consequently age hardening in the A1-Au system appeared to be interesting. Quite recently Heirnendahl13-15 revealed that the solid solubility, as determined by transmission electron microscopy, was 0.3 wt pct Au at 640°C and 0.25 wt pct Au at 600°C, decreasing with decreasing temperature. In an A1-0.2 pct Au alloy after quenching from a solution treating temperature of 600°C the yield stress was 2 kg per sq mm, and it increased up to 6 kg per sq mm after aging for 1 to 10 hr at 200°C. The precipitation occurred in the form of platelike particles mainly on (100) matrix planes. The intermediate phase n', the equilibrium phase n (AuAl2), and lattice relationships between both precipitates and the matrix were also investigated by electron microscopy. One of the purposes of the present research is to determine whether or not the solid solubility in this system, in which gold has a very small solubility in

Jan 1, 1970

By Tell Ertl

An annual invitational address by an outstanding man in mining, geology, or geophysics who has contributed significantly to the progress of technology in these fields. IN 1954, the first year the award was conferred, Fred Searles, Jr., remarked, "The earlier years are the easiest." In this, the second year, it was easy to choose the outstanding mining engineer. Our conferee this year has been destined to mine. He comes from pioneer stock, and though a son of the American Revolution he is most proud that all four of his grandparents came to the Jordan River Valley of Utah the "first summer," which all Utahns will recognize as 1847. At the time of discovery of high-grade ore in Bingham, his grandfather, Archibald Gardner, had a crew of men getting out saw timber in the area. The first claim staked in Bingham Canyon was named the Jordan, and Bishop Gardner was the colocator of the claim as well as the man to record it. E. D. Gardner was born in West Jordan, Utah, in view of Little Cottonwood Canyon, the site of the Emma Mine. Park City in the Wasatch Mountains a few dozen miles to the east, and Tintic, not much further to the south, were developing their vast ore-bodies throughout his youth. As a boy he was near the present Midvale metallurgical area and could see the Lark and Bingham Canyon mine dumps and imagine the mining activities at Tooele, Ophir, and Mercur just over the nearby Oquirrh Range. He was 11 years old when the first car of copper ore was shipped from Bingham Canyon. It was not surprising that he attended the University of Utah and graduated with an engineer of mines degree. Five years with the Utah Apex in Bingham Canyon as chief engineer and assistant superintendent completed his training for the 44 years of unselfish and lightly rewarded service he was to give the mining industry as a Government engineer. All of us in mining are familiar with the great work he carried on and directed during the genera- tion he supervised the Southwest Experimental Station at Tucson. He has written scores of papers and books. His observations and experiments on drilling and blasting have led to the important improvements in this field during the past quarter century. Whereas those of us who consider ourselves widely informed about underground metal mining methods make hasty trips through a half dozen or dozen mines a year, our conferee has visited them all—not only the metal mines, but also coal and hundreds of nonmetallic mines, in the United States, Canada, Latin America, and overseas. His keen observations and analytical mind have resulted in an encyclopedic knowledge of mining and mines. His improvements in mining technology have been steady and predictable. His elucidation of mining problems to the many young engineers that have come under his guidance have made them grow strong and useful to his industry. When he chooses to stop, his influence will continue to expand and prosper because of the inspiration and dedication he instilled in so many of us. The profits from his ideas have been distributed throughout the mining industry. He has remained a technical man who felt that he could serve the mining industry best as a Government engineer. But he is the staunchest advocate of the belief that the public should gain from his work through private industry. This is not the first recognition E. D. Gardner has received. The Department of the Interior awarded him the coveted Medal for Distinguished Service in October 1949, and he received the Engineering & Mining Journal's Salute in March 1951. His friends who are presenting him the Daniel C. Jackling Award today know this great mining engineer simply as "Ed" Gardner.

Jan 1, 1956

By F. W. C. Boswell, R. L. Cunningham, H. M. Weld

Chemical analysis shows the partition of the magnesium addition between the metal and the graphite is independent of whether the graphite is in the form of nodules or flakes. The bright central spot observed in nodular graphite polished sections is shown to be due to the structure of the nodules. DURING the past few years numerous papers have been published on the production1-7 and heat treatment" of nodular cast irons. However, very little information is available on the structure of the nodules and the reason for their formation. It would appear that an explanation of the phenomenon of nodulation must await a detailed knowledge of the nature of the nodule. Disagreement exists among various workers on such a fundamental point as to whether or not a nodule actually contains a microscopically visible, nongraphitic nucleus.9-11 Work was initiated with a view to obtaining definite information on this and other aspects of the problem. Chemical Separation and Analysis Microscopic appearance had indicated9-11 that a nongraphitic core might exist in nodules (Fig. 1). It appeared that a chemical comparison of separated nodules and flake graphite would be profitable, for if the core is nongraphitic a relatively large amount of certain elements would be found in the nodules as compared to the flake. This comparison could best be made by obtaining nodules and flake from the same melt of cast iron, part of which had been in-noculated with a suitable addition reagent for the formation of nodules. A 300 lb melt was produced. About half of this was innoculated in the ladle with an Fe-Si-Mg alloy to produce nodules and cast into keel blocks; the remaining half of the melt had silicon added in an effort to compensate for the silicon in the innoculant used in the other half of the melt and this was cast into similar keel blocks. The analyses of the resultant irons are given in Table I. Nodules and flake were chemically extracted from 2 kg samples of metal as described in the appendix. While this method dissolved the iron and chromium carbides, it did not dissolve the titanium, vanadium, and molybdenum carbides. These latter carbides could have been removed by nitric acid, but in other experiments it was found that it attacked pools of metallic iron entrapped in the nodules which had, until the nitric acid treatment, been protected from the attack of the sulphuric, hydrochloric, and hydrofluoric acids. It will be shown in the next section that entrapped iron exists in nodules but not in flake. On microscopic examination many tiny irregular particles were observed to accompany both the nodules and the flake. These were identified by tabling a sample of nodules from which a sufficient fraction was obtained for X-ray analysis. A good pattern of titanium carbide was obtained indicating that this was the predominant compound present. Since it was not possible to determine how completely the carbides could be removed mechanically and since their removal from flake is much more difficult, it was decided not to resort to any separation as this would render further comparisons more difficult. The samples were ashed in a combustion

Jan 1, 1953

By M. E. Fine, A. A. Hendrickson

The critical resolved shear stress and the strain rate dependence of the .flow stress are reported for Ag base A1 single crystals up to 6 at. pct A1 over a temperature ralzge of 4.1° to 470°K. At room temperature the solid solution strengthening is attributed brinciballv to an increase in the dislocation density on alloying. At 42°K the alloys are relatively stronger because the dislocations widen on alloying and are more difficult to cut. In a previous paper, the authors reported the characteristics of strain aging in Ag base A1 alloys.' The variation of the magnitude of the strain-aging yield drops on aging time, aluminum content, and testing temperature strongly indicated that the phenomenon is due to the Suzuki mechanism. In the present paper, the critical resolved shear stress (CRSS) and the strain rate dependence of the flow stress are reported for Ag base A1 single crystals as functions of testing temperature (4.2" to 470") and A1 content (0 to 6 at. pct). Observations on the substructure and measurements of the effect of crystal growth rate are also given. The experimental re- sults appear explainable considering that aluminum additions increase the dislocation density and dislocation width. EXPERIMENTAL METHOD The methods of specimen preparation and tensile testing were described previously.' Briefly, single crystals were grown from the melt in a vacuum (1 x lom5 mm Hg), shaped into tensile samples by a combination of abrading and acid etching, annealed at 850°C in a vacuum (1 x 10" mm &Z) for several days, and furnace cooled to 200'. The testing was done on a model TM Instron using friction grips and a strain rate of about 5 x 106 per sec unless otherwise noted. The various testing temperatures were obtained by immersing the specimens in the following media: 1) 4.2': liquid helium using the apparatus of G. Byrne;' 2) 77°K: liquid nitrogen; 3) 200"K: dry ice and acetone; 4) 415' K: ethylene glycol; 5) 460' \ to 480' : molten Stanalax. In the determination of the CRSS above 296' K, a ratio method was used; the crystals were strained initially at the higher temperature, 0.1 pct shear strain, and then tested at 296' . The ratio of the flow stress between the two temperatures was then multiplied by the average CRSS at 296' K to obtain the value of the CRSS at the high temperature. (The test at 296' showed a yield point resulting from strain aging; the flow stress at 296' K was taken as the lower yield stress.) The ratio method, we believe, is more accurate than using different crystals since

Jan 1, 1962

By R. P. Fischer

The Colorado Plateau region has been the principal domestic source of uranium, vanadium, and radium. The value of these commodities produced from the region through 1964 slightly exceeds $2 billion. Most of the deposits occur in streamlaid lenses of sandstone in the Chinle and Morrison Formations. The ore minerals below the zone of oxidation are low-valent oxides and silicates of uranium and vanadium; all of these, except the quite stable vanadium silicates, oxidize readily to a variety of high-valent uranium and vanadium minerals. The ore minerals partly replace fossil wood but mainly impregnate sandstone, typically forming tabular ore bodies that are nearly concordant to the bedding of the host rock. The deposits range in size from those containing only a few tons of ore to those containing more than 1 million tons. Stratigraphic, lithologic, and sedimentary structural factors obviously influenced the localization of these deposits, but igneous activity, hydrothermal mineralization, and tectonic structures show no similarly consistent influence on localization. The deposits are epigenetic, but the source of the ore metals, the nature of the ore-bearing solutions, and the time of ore emplacement are uncertain. A few uranium deposits in the region are dominantly discordant to bedding and occur in collapsed breccia pipes or along linear fractures. Their origins are also uncertain.

Jan 1, 1968

By A. P. Woods, J. A. Elias, A. J. Heckler

A method is described by whichX-ray pole figures and axis density figures may be plotted automatically. The X-ray data are obtained using a Siemens texture gonionleter and the Schulz reflection method. Composite sampling methods are used to obtain a full quadrant of the pole figure. The contour lines of the pole figure and axis density figures are drawn using a computer-controlled x-y plotter. The computer program used to draw the contours was obtained from ZBM. POLE figures used to describe crystallographic orientations of poly crystalline sheet materials are usually plotted manually from X-ray diffraction output in the form of a strip chart recording of the intensity distribution of a given crystallographic pole in physical space. Today's computers and associated plotting equipment now make it possible to plot pole figures and axis density figures automatically. Inverse pole figures have been determined by mathematically "inverting" X-ray pole figure data.'-' In general, these methods require complicated, time-consuming numerical calculations. A more economical but less accurate method is to determine the axis densities of low-index crystallographic poles using an X-ray diffractometer. When these axis densities are plotted in a unit stereographic triangle contour lines can be drawn to represent the axis density distribution. This can now be done automatically. Computers were used to plot pole figures by a method developed by Holland, Engler, and powers.' In their method intensity ratios based on a random standard sample were obtained from a strip chart recording, and the stereographic (x, y) coordinates of these ratios were determined by a computer. Symbols characteristic of different intensity ratio levels were then plotted using an automatic x, y plotter and intensity contours were drawn manually. The present paper describes a method by which pole figures and axis density figures have been automatically plotted from digital data obtained from a Siemens X-ray unit. Plotting was accomplished using an IBM 1620 computer and a Calcomp 563 digital plotter. COMPUTER PROGRAM The computer program was obtained from IBM Systems Reference Library, No. 1620-CS-05X, and was designed to plot contour maps from randomly distributed data. It consists of a set of twelve separate subprograms, four of which were used in this work. The program takes a given distribution of data points and by a numerical method determines the values at mesh points of a square grid system superimposed over the input data. The output data from this program is in a form suitable for input to the contour plotting program. A smoothing program is also available which calculates new mesh point values from a continuous function fitted to neighboring mesh points. The degree of smoothing depends on the number of points around a given grid point which are used to adjust or smooth the grid value. The contour plotting program is designed to allow the user to specify the interval, scale, and annotation of the contours to be plotted. EXPERIMENTAL PROCEDURE Pole Figure Data Points. Diffracted X-ray intensities were determined using a Siemens texture goniometer and the schulzs reflection method. Due to geometric

Jan 1, 1968

By Albert Sauveur

SOME writers believe that when austenite transforms completely into pearlite on slow cooling through the thermal critical range, such transformation does not imply the formation of any of the so-called transition constituents: martensite, troostite and sorbite. Might it not be claimed with as much justification that when water freezes it does so suddenly, solid ice being obtained without passing through the intermediate stages of ice and water? Obviously, regardless of the speed of solidification, this would be erroneous. Before reaching the completed solid condition, this must of necessity pass through an unbroken series of stages when the system consists of mixtures of water and of ice, the former decreasing and the latter increasing in amount. Are not these "transition" stages in the freezing of water similar to the transition stages occurring in the transformation of austenite into pearlite? To clarify, let us consider in Fig. 1 the mechanism of the transformation of eutectoid steel from its austenitic to its pearlitic condition as it cools slowly through its thermal critical range. It is generally admitted that this transformation is the result of two distinct phenomena: (1) the allotropic change of gamma iron into alpha iron and (2) the crystallizing out of solution of the carbide Fe3C. Whether this crystallizing of Fe3C implies also its formation is immaterial for our purpose. In other words, whether it is the carbon in atomic dispersion which is present in gamma iron or molecules of Fe3C has no bearing upon the matter to be discussed. The transformation of gamma iron into alpha iron cannot take place suddenly. It must of necessity be progressive, regardless of the speed with which it may take place. At A, for instance, there would be present AB gamma iron and BC alpha iron. The distance MN does not refer to falling temperature, but to the passage of time. It may be assumed that the transformation takes place at a constant temperature (the Ar321 point). In a similar way, the crystallization of Fe3C out of the austenite solid solution must be progressive as depicted between M and N. At A there would be present AB gamma iron, BC alpha iron, CD carbon dissolved in gamma and in alpha iron and DE Fe3C. This condition may be described according to individual preference as martensite or troostite. To sum up, can the metal pass from condition

Jan 1, 1931

By J. B. Cohen, M. B. Beaver, R. J. Black

RECENT investigations have shown that face-centered cubic metals may deform by twinning. Blewitt, et al' found that at 4.2"K the mode of def~rmation of single crystals of copper changed at large strains and markings formed on (111) planes. Later they- emonstrated by X-ray diffraction and metallography that the markings were twins and showed that favorably oriented single crystals of copper deformed by twinning at 78°K. They also observed twinning in silver and gold deformed at 4.2 and 78°K. Wagner3 obtained evidence for twinning from the peak shape of diffraction lines of silver cold-worked at 78°K, but twins small enough to cause such effects are not likely to be detected metal-lographically. In the work reported here lamellar structures were observed in deformed silver-gold alloys. They appeared to be mechanical twins, but metallography could not establish this conclusively. Their tendency to form depended on strain rate, temperature and composition. Specimens of silver-gold alloys (0 to 83 wt pct Au) were deformed plastically. One set was worked by hammering under liquid nitrogen, at room temperature and at intermediate temperatures. Another set was compressed slowly in liquid nitrogen to the same reductions as those produced by hammering. Tensile specimens (0.015 x 0.120 x 1.5 in.) of various compositions and approximately equal grain size (0.011 to 0.016 cm) were tested at -195°C and at room temperature. In microsections of all specimens deformed by hammering at —195°C thin lamellae appeared, Fig. 1. They were aligned in definite directions in each grain. In some grains they had two orientations. Where lamellae intersected, a displacement was apparent. Near the center of the left margin of Fig. 1 shear has taken place beyond the fully developed intersecting lamella. Many lamellae resembled Neumann bands in alpha iron. They were parallel to one side of triangular etch pits in the matrix (as in Figs. 1 and 2). The individual lamellae were narrow and had little substructure. This suggested that they did not result from concentrated local slip. The shape of etch pits within the lamellae differed from that of pits in the matrix, as can be seen in Fig. 2; this indicated a difference in orientation. Specimens slowly deformed at —195°C contained regions in which the lamellae were clustered. In these specimens some lamellae were bent and presumably had formed before the termination of the deformation. Structures of greater width than the lamellae were also seen.4 More lamellar structures formed on impact than during slow compression to a given reduction. This was true of all compositions. The structures became less abundant with increasing temperature of deformation. None was observed after extension to fracture at room temperature, but they could be pro-

Jan 1, 1959

By A. R. Krause, C. Laird

In order to establish whether or not there is a real temperature effect in fatigue (independent of environment) , poly crystalline copper and Cu- 7.9 A1 alloy have been cycled at 298° and 7° K in vacuo and the fatigue lives compared with those in air and in liquid nitrogen. The lives of both copper and the alloy were found to be highly temperature-dependent in the absence of environment. This result casts serious doubt on the validity of the cell structure hypothesis for stage I crack propagation as presently formulated, because it predicts that there should be no such tempevnture dependence. On the other hand, the plastic blunling process is consistent with the result. Effects of environment aside, the homogenization of slip which accompanies testing at low temperature, and at low strains, seems to be the main cause for increased fatigue life. At high strain amplitudes, the fatigue lives of wavy slip materials, typically copper, are independent of temperature.' It is well-known, however, that low-strain lives greatly as as the temperature of testing is decreased. By contrast, the lives of planar slip materials, such as Cu-7.9 pct A1 alloy, increase to an even greater extent with decreasing temperature throughout both the high and low strain ranges.1'2'5 The mechanism of this temperature effect is associated with the earliest stages of fatigue failure,'" crack nucleation, and stage I growth,"' which is slow propagation along slip bands to the depth of a few grain diameters. Such life behavior has been interpreted on at least two different bases. On the one hand, those interested in the temperature effect at high strain amplitudes1 believe that stage I growth occurs by the plastic blunting process of crack propagation.7'9 They explain the effect in planar slip materials by the homogenization of slip* which accompanies fatigue testing at low temper- atures and serves both to delay crack nucleation and to decrease the rate of stage I propagation. On the other hand, Holt and Backofen,2 who have studied the effect in low strain fatigue, believe that stage I growth can be interpreted by a cell structure hypothesis.10-12 They have challenged2 the conclusion that there is a real temperature effect in this regime of fatigue testing and have interpreted the increased fatigue lives almost entirely in terms of the "environmental-protective'' effect of the liquid nitrogen and helium baths used to obtain low temperatures. This interpretation by Holt and Backofen2 may offer a means of discriminating between these two mechanisms as currently formulated and used to explain stage I growth. On the basis of the plastic blunting process applied to stage I crack propagation,7* the low strain fatigue lives of both wavy and planar slip materials should be increased with decreasing temperature. This follows because both materials show increased slip homogenization in this strain regime."13 Consequently, crack nucleation in intensified bands will be delayed and the linking of such small cracks into larger stage I cracks will be difficult. In addition, the blunting process required to lengthen a stage I crack from the order of 2 to 10 (where the strain concentration of the crack begins to overcome the slip homogenization property of the material) will also be retarded. These delays will give rise to longer lives in both kinds of material. In contrast to the blunting hypothesis, no temperature dependence has been predicted on the basis of the cell structure hypothesis, because it is well-known that materials cycled at low temperature show no differences in type of dislocation structure for a given strain amplitude.18"20 If the lives of wavy and planar slip materials do show a temperature dependence when the environment is eliminated as a variable, then it is questionable whether cell structures per se have a fundamental role in fatigue fracture. Accordingly, specimens of copper and Cu-7.9 wt pct A1 have been cycled at 298° and 77°K in vacuo and the fatigue lives compared with those in air and in liquid nitrogen, in order to establish whether or not there is a real temperature effect in low strain fatigue. Since it is difficult to measure the strains in specimens when cycled in vacuo, S-N curves have been used as the basis of comparison. In studying the influence of temperature on fatigue life in ordinary environment, Holt and Backofen2 used the superior basis of E-N curves. However, they also published S-N curves and thus established the relationship between E-N and S-N curves. This relationship is used to support the S-N comparison reported in the present investigation. EXPERIMENTAL Materials. The copper employed in this investigation was of 99.99 pct purity and the cu-7.9 pct A1 was prepared from metals of the same purity. The stock, of 3 in. initial diam, was reduced in size by rolling

Jan 1, 1969

Jan 1, 1962

By P. Chiotti, J. T. Mason

Metallographic, thermal, X-ray, and vapor-pressure data were employed in establishing the Ce-Zn phase diagram. Nine compounds and three eutectics were observed. The eutectic compositions in weight percent zinc and temperatures are 10 pct and 495"C, 37 pct and 795°C, and 56 pct and 810°C. Three of the compounds, CeZn, CeZnn, and CeZne.5, melt congru-ently at 825°, 87.505°, and 980°C, respectively; the other six compounds, CeZns, CeZns.67, CeZn4.5, CeZn5.25, CeZn,, and CeZnll, decompose peritectically at 820°, 840°, 870°, 885", 960°, and 795"C, respectively. The compound CeZn5.25 is an AB5 type with a small range of composition which lies on the zinc-rich side of the 1 to 5 stoichiometry. Zinc vapor-pressure data obtained by the dewpoint method were employed in calczilating the thermodynamic properties of both the liquid alloys and solid compounds. The data for the A critical review of the information available on the Ce-Zn system up to 1960 has been given by K. Gschneidner, Jr.' Of particular interest is the work by J. schramm2 who investigated the region between 55 and 100 wt pct Zn and reported a CeZn,, compound which decomposes peritectically at 785"C, a CeZn, compound which melts congruently at 972"C, and five temperature horizontals at 79@, 817", 840", liquid alloys were fitted to the relation from which the relation was obtained by integration. In these relations F XS is the excess partial molal free energy, N is atom fraction, and the constants c and d have the values c = (-22,000 + 7.0T) and d = 6171,000 + 74.0T). Relations for the standard free energy of formation for the solid compounds were derived from the data. At 973°K the enthalpy in kilocalories per gram-atom z)aries from —11.3 for CeZnz to —8.21 for CeZn~l and the free energy in the same units varies from —7.1 joy CeZn, to -3.82 for CeZn11. and 942°C in the region between 55 and 75 wt pct Zn. No attempt was made to identify other features of the system. I. Johnson and R. yonko3 used a fused-salt cell to measure the electromotive force between pure cerium and an alloy consisting of zinc-rich liquid in equilibrium with CeZnll. Solubility data for cerium in zinc has been reported by J. Knighton et u1 .4 Johnson and Yonko give the following equa-. tions for the mole fraction of cerium in zinc and the standard free energy of formation of CeZnll:

Jan 1, 1965

By R. W. Stormont, F. Wald

The phase diagram of the Pseudobinary section PbTe-Fe was determined. It was found to contain a monotectic and a eutectic reaction, the latter one taking place at 14 at. pct Fe and 875° * 5°C. The solid solubility of iron in PbTe was found to be 0.3 at. pct by electronmicroProbe analysis. No solubility of PbTe was detected in iron. Slight deviations from true pseudobinary behavior were found to occur in the range of - 5 to 10 at. pct Fe. In the course of a general investigation of reactions of various metals with lead and tin telluride,' the lead telluride-iron system was reinvestigated. It had been established much earlier than iron does not chemically react with lead telluride but forms a eutectic with a melting point of 879" The eutectic composition or other related information has never been reported, but for a number of years iron has been in general use for contacting of lead telluride and lead telluride alloys for thermoelectric applications. It seems therefore desirable to clarify the exact constitution of the system to furnish a base for the long-term evaluation of bonds made between lead telluride and iron either by pressure contacting or by brazing methods. I) EXPERIMENTAL METHODS Lead telluride-iron alloys were prepared in 10-g charges, using premelted lead telluride. This material was prepared from high-purity, semiconductor-grade lead and tellurium obtained from the American Smelting and Refining Co. and described as 99.999 pct pure. The iron used was "Armco" iron; the major impurities found here were 0.02 pct C, 0.018 pct Si, and 0.015 pct Cr. All remaining impurities were less than 0.01, the total of all impurities not exceeding 0.15 pct. Charges were prepared in closed quartz arnpoules which were evacuated and in some cases backfilled with high-purity argon to retard excessive lead telluride evaporation and deposition in slightly cooler parts of the ampoule. For high iron concentrations, this can lead to total separation of the constituents, since the vapor pressure and the sublimation rate of PbTe are quite high.4 Nevertheless, since the ampoules are closed, no change in overall composition was expected and the nominal composition of all alloys was assumed to be retained. X-ray diffraction analysis, thermal analysis, and microsections were used in the evaluation of the alloys. The nature of the system was such that X-ray diffraction was not particularly helpful. It merely served to establish that at all concentrations PbTe and a! iron were in equilibrium at room temperature. Thermal analysis was carried out by taking direct temperature vs time curves on a Sargent recorder where a width of 10 in. was kept as 1 or 0.5 mv by use of an automatic bucking voltage network. Quartz ampoules with minimized dead space, coated with boron nitride and fitted with a thermocouple reentrant, were used as containers for the charge. At high temperatures and over long periods of time, boron nitride reacts with iron. For the thermal analysis runs, however, this was not significant. More significant was the fact that the vapor pressure of PbTe at some of the meas -uring temperatures apparently exceeded I atrn quite considerably. This, in some cases, caused the slightly softened quartz tubes to blow out if great care was not taken to contain them and minimize time and temperatures used. As containers pure nickel tubes were used which also served to avoid temperature gradients in the quartz ampoule. Nevertheless, the experimental difficulties at high temperatures were severe and the monotectic temperature could therefore not be determined accurately. In general, the accuracy reached by the thermal analysis setup in this case is *4"C as determined with gold, silver, and tin, under the conditions of analysis here. Inherently, the apparatus is capable of reaching accuracies better than i 1°C. Also, difficulties were encountered in microsection-ing. They were related to polishing, since it is rather difficult to avoid pulling the iron out of the weak and brittle lead telluride matrix. It proved best to follow a procedure where, after grinding to 600 grit on carborundum paper, a polish with 6 p diamond was used on nylon cloth. Finally, #3 "Buehler" alumina and an automatic polisher were used for -5 min only, to avoid relief. The best etching results were achieved with

Jan 1, 1969

By C. David Mann

Metal prices continued to improve in 1964, resulting in the opening of new mines and re- activation of old ones. Larger and deeper shafts are being bored. At the AEC's Nevada Test Site, a 72-in. diam shaft is being bored to 3200 ft. In New Mexico a 1650-ft shaft was bored with a 48-in. bit, then reamed to 124 in. to 935 ft, and 102 in. to 1650 ft. Deviation was only 26 in. In California a shaft sinking machine has been developed which combines drilling and mucking equipment into one mobile, integral unit.

Jan 2, 1965

By Ralph C. Flow

In Cleveland County, North Carolina, 1 ½ miles south of Kings Mountain, Foote Mineral Co. operates an open pit for the production of spodumene, feldspar, mica and commercial stone. Spodumene concentrate is sent to Foote Mineral's Sunbright, Va., plant and to other customers. Exton, Pa. and New Johnsonville, Tenn., plants produce lithium com- pounds sold to the oil industry for multipurpose lithium-base greases, to the metal industry as welding flux, to the air conditioning market and to the glass industry. Ceramic-grade spodumene, feldspar, and mica concentrates go to other processing companies from the Kings Mountain plant. Waste amphibolite is delivered to a neighboring quarry operation. Geology and exploration of the deposit have been described by T. L. Kesler, Chief Geologist of Foote Mineral Co., in the September 1961 MINING ENGINEERING. Measured ore reserves as published at that time were 20.7 million tons. The ore deposit consists of a series of lithium-bearing pegmatites enclosed in amphibolite and mica schist wall rocks. The general strike of the pegmatites is northerly, and in the southern part of the pit, they dip slightly towards the west. The largest body being mined has a fairly uniform thickness of about 200 ft. Other pegmatites in the pit area range from 20 to 100 ft in thickness. Minerals in the pegmatites are 20% spodumene, 32% quartz, 6% muscovite, 41 % feldspar and 1 % trace minerals.

Jan 10, 1962

By R. I. Jaffee, E. S. Bartlett, D. N. Williams

The oxidation resistance and fabricability of molybdenum powder-metallurgy alloys containing up to 20 wt pct nickel in the form of a fine dispersion were studied. The effects of dispersion distribution and of amount and type (pure nickel or nickel compounds) of additive were considered. A definite improvement in oxidation resistance was observed, but the amount of improvement fell far short of requirements for an oxidation-resistant alloy. Fabricability by hot-rolling was limited. INVESTIGATIONS at Ohio State university1 and Battelle Memorial institute2 have indicated that the attainment of a truly oxidation-resistant molybdenum-base alloy for high-temperature service, with the coincident retention of high-temperature strength and toughness, will be a difficult, if not impossible, feat. Among the most promising alloy systems studied was the molybdenum-nickel system shown in Fig. 1. Alloys in this system show good oxidation resistance at temperatures well above the normal melting point of molybdenum trioxide because of the regenerative formation of protective nickel-molyb-date (NiMoO4) on the surface of the alloy during exposure at high temperatures. Unfortunately, the required alloy content to obtain oxidation resistant molybdenum-nickel alloys far exceeds the limits of the narrow terminal solid-solution boundary, and closely approaches the peri-tectic composition involving the brittle intermetal-lic compound, MoNi. Because of the peritectic reaction, fusion alloys are characteristically brittle, since the MoNi phase, being the last to form, tends to occur as a continuous grain-boundary network around each molybdenum grain. An added problem with this system is that the protective nickel-molybdate layer formed at high temperatures is unstable, undergoing one or more allotropic modifications upon cooling. The volume changes associated with this modification during cooling are such as to cause violent expulsion of the protective molybdate coating from the surface of the piece. This is, of course, quite detrimental in material exposed to cyclic temperature during service. The research reported here resulted from an attempt to overcome the aforementioned problems associated with the molybdenum-nickel alloys primarily by controlling the amount, size, and location of the MoNi phase. By using powder-metallurgy techniques of alloy preparation and sintering the blended molybdenum-nickel powder mixtures at a temperature below the peritectic reaction temperature, molybdenum-nickel alloys with a randomly dispersed MoNi phase were produced. MATERIALS The molybdenum powder used in the preparation of alloys for this study was commercial hydrogen reduced, minus 325-mesh (Tyler) material. Master alloys, by which nickel was added, consisted of elemental carbonyl nickel powder (12 average particle size), an alloy of 50 wt pct Ni-50 wt pct Cr, and compounds of MoNi, Ni,Si, and Ni2B. The nickel-chromium powder was prepared by filing a vacuum-arc-melted ingot, separating impurities magnetically, and screening to minus 200-mesh. The MoNi powder was prepared by pulverizing a hydrogen-sintered powder-metallurgy compact to minus 325-mesh material. Further sizing of this powder for study of effects of dispersion distribution was accomplished by air classification of the minus 325-mesh powder. The Ni2Si and Ni2B powders were prepared by crushing vacuum-sintered powder-metallurgy compacts to minus 200-mesh material. EXPERIMENTAL PROCEDURE Specimen Preparation—The general procedure followed in the preparation of alloys for testing is described as follows: 1) Blending. Either hand-blending of the powders in a ceramic mortar and pestle for X 1/2 or mechanical blending was used. Hand-blending seemed preferable for optimum homogeneity. 2) Compacting. Most of the blended powders were pressed to green compacts at pressures of 15 tons per sq in. in a single-action die, although some were pressed at 80 tons per sq in. A 1 X 11/4 X 1/4-in. green compact was the standard size for oxidation test material, and 7 X 1/2 X 1/4-in. compacts were used for fabricability test specimens. 3) Sintering. All green compacts were sinteredat

Jan 1, 1959

By H. O. Hofman

THE leading antimony mineral is stibnite. In smelting stibnite ore two processes are available, precipitation and roasting-reduction. The former is suited only for high-grade ores. As low-grade ores are more common than high-grade, roasting-reduction is of greater importance than precipitation. In the roasting process the aim may be to leave the oxidized antimony in the ore, or it may be to volatilize as much of the antimony as possible, collect the volatilized oxide as a rich intermediary product and smelt it for antimony, leaving the gangue poor enough to be considered a waste product. Whichever way the roast is conducted certain difficulties inherent in stibnite are encountered. These are: 1. The low melting point of stibnite which; according to Pelabon,1 is 550°C., according to Wagemann2 540°C., and according to Borgström3 546°C. 2. The ignition temperature: According to Friedrich,4 stibnite, if heated in air, begins to oxidize at 290°C. if the size of a grain is 0.1 mm. in diameter; at 343°, if 0.1 to 0.2 mm.; and 430° if 0.2 mm. 3. The fusibility of a mixture of Sb2S3 and Sb203 which in the form of kermesite (Sb2S3)2.Sb203 melts at 517°C.5 4. The volatility of Sb2S3 and Sb203, for which no numerical data appear to exist, although practical experience has shown that they are volatile at low temperatures.

Jan 1, 1916

By T. L. McCall

THE late Walter Herd1 in 1929 gave a full description of past and present conditions in No. 2 mine, Springhill, Nova Scotia, developed theories regarding the cause of these bumps and made certain suggestions regarding possible methods of future development. Recapitulating briefly from Mr. Herd's paper, the seam is bituminous coal, averages 9 ft. in thickness and has a well defined parting containing fusain about 14 in. from the roof. This roof coal is somewhat stronger than the rest of the seam and has a tendency to cling to the roof. The pitch of the seam where it is now being worked is about 20°. The first manifestations of bumps began when the room and pillar workings had reached a depth of cover of 1900 ft. and under continuously increasing depth of cover these bumps increased to such an extent, both in number and severity, that in the year 1924 it became apparent that some change in the system of extraction was necessary. After closely studying all the factors involved and benefiting largely by valuable out-side advice obtained by the Provincial Department of Mines of Nova Scotia,2 the system of working was changed from room and pillar to longwall retreating. Mr. Herd's paper described in detail three remarkable bumps in the year 1928 in April, July and October that affected the 5700-ft. and 5900-ft. East levels, the last bump being so severe both in intensity and in extent of damage done that this district was abandoned. The longwall workings to the west of the slope had been stopped in the year 1926 owing to an inbreak of water, coming from the flooded waste of No. 3 seam lying some 400 ft. vertically overhead. This inflow was not excessive, but a large quantity of water being impounded in the old workings it was considered advisable to take the prudent course and not incur the risk of possibly increasing the flow by further working. This district has remained idle ever since.

Jan 1, 1934

By T. W. Beck

Roof bolter occupations in underground coal mines continue to experience overexposure to respirable dust. One potential source of dust in roof bolting operations is the exhaust from the roof bolter dust collection system. A wet exhaust conditioner (water box) has been developed to reduce dust emissions from the exhaust of the vacuum dust collection system on roof bolting machines. The exhaust conditioner consists of a muffler chamber and a water chamber with four internal partitions to direct airflow over the surface of the water. The National Institute for Occupational Safety and Health conducted a series of laboratory tests to assess the respirable dust capture ability of this device as compared to the standard exhaust muffler. To determine the dust collection efficiency, both devices were placed in the exhaust stream of a simulated roof bolter dust collection system. Gravimetric samplers were operated upstream and downstream of the exhaust conditioner and muffler to evaluate the ability to capture both respirable coal and limestone dust. Researchers observed a 41 % reduction in dust concentrations for the water exhaust conditioner in the laboratory configuration. Significant levels of dust deposition in the sampling chambers may have contributed to this effective capture rate.

Jan 1, 2012

By J. J. Hauser, H. C. Theuerer

A cathode sputtering technique is described which elin7inates the need for ultrahigh vacuum in preparing thin films of materials sensitive to gaseous impurities. This technique uses a fraction of the atoms sputtering within an anode container to getter actice gases, such as HzO, Oz, and Nz. The gases alzd gettering metal are deposited on the container walls, thus shielding the coating zone of the system from contamination. The use of the method for preparing superconducting-normal metal couples such as Ph-Cu and Ph-Pt is described, and the properties of the individual and composite films are given and discussed. GETTER sputtering is a method which greatly simplifies the preparation of thin films in cases where composition control is critical. A major difficulty with conventional sputtering and other vacuum-deposition techniques is the contamination of the forming film caused by residual gases, such as H20, CO, Oz, and Nz, in the coating equipment. The difficulty arises from the fact that even when the residual pressure in the system is as low as 1 x 10"6 Torr, with a deposition rate of 10A per sec, there are as many contaminating gas collisions with the substrate as there are with film-forming metallic atoms. It is not surprising, therefore, that with reactive metals, such as tantalum and niobium or with semiconductors, such as silicon and germanium, films with properties far different from the starting materials are obtained. In the case of niobium and tantalum, deposited either by sputtering or vacuum evaporation in systems with reactive gases at pressures of the order of 1 x l0-' Torr, the loss of superconductivity is traceable to interstial oxygen or nitrogen. On the other hand, working in vacuum of the order of 1 x l0-" Torr, Marchand and enema' have shown that superconducting films of tantalum with properties approaching those of bulk material are possible. At this level of gaseous impurities -lo6 metallic atoms arrive at the substrate before a contaminating collision occurs again assuming a deposition rate of 10A per sec. It is evident from the above that any successful vacuum technique requires the elimination of reactive gases from the region of the system where coating is occurring. Getter sputtering accomplishes this using conventional vacuum equipment with residual pressures in the 106 Torr range. In fact? vacuum systems with residual pressures of lo-" Torr are adequate for most purposes. With this method, sputtering is confined within an anode can and, by geometric design, sputtering itself is used to purify the argon at the lower and upper parts of the system by the gettering action of the reactive metal. In consequence, the central region of the system where coating occurs is shielded from gaseous contamination. Getter sputtering is particularly useful for the preparation of alloy and compound films. With this method, if a cathode of homogeneous composition is bombarded with high-energy argon ions, transfer of material to the substrate having the same composition as the cathode will occur. This is true after an initial equilibration time, even though the constituents of the cathode may have different sputtering rates. During equilibration, the surface of the cathode changes composition due to differences in sputtering rate, but mass conservation demands a steady-state condition such that the atoms sputtered from the surface have the same composition as the cathode material from which the surface is generated. GETTER-SPUTTERING APPARATUS The original form2 of the getter-sputtering apparatus is shown in Fig. 1. It consists of a closed nickel or stainless-steel can 4 in. tall and 2-3/8 in. in diameter. Mounted symmetrically from each end

Jan 1, 1965

By Herty, C. H.

The effect of temperature on the physical properties of structural materials has been the subject of many investigations during the past decade. The literature on the effect of elevated temperatures. is voluminous, and during the last four years a great deal of experimental work has been carried out on the effect of low temperatures on the impact properties of steel. For many engineering purposes it is important to know the shock resistance of steels at low atmospheric temperatures, and with the ever-developing field of refrigeration and separation of materials at low temperatures, the normal limits of atmospheric temperature have been exceeded in practice. Iron and its alloys in the unnotched condition have a high impact strength at low temperatures, but in practice variations in type of notches result either from design or accidentally through scratches and surface or internal defects. A study of notched bar impact tests is, therefore, highly important to the engineer. A survey of the literature on low temperature impact testing indicates that chemical composition, heat treatment and method of testing have been the variables which have been considered in most previous work. In only a few instances has any mention of the steel- making method been mentioned and in these the comparison was between steel-making processes and not between steel-making methods on the same process. In view of the wide variations in impact properties at room temperature, in quench and strain ageing and in grain growth of steels of identical chemical composition, (by this is meant the usual five element analysis reported), it was felt

Jan 1, 1957