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By H. Cecil Spicer

The results described in this article are based On field work conducted during the periods April-May, I939, and May-July, 1940. The United States Potash Co. is mining potash on Government land under a permit from the Department Of the Interior and the geophysical investigation was completed under a cooperative arrangemerit made between that company and the Conservation Branch Of the Geological Survey. The writer, a member Of the SeCtion of Chemistry and Physics of the Geologic Branch, was assigned to this investigation. Four definite objectives were in mind for the geophysical work in the studies over the salt deposits. The first was to determine the measure Of success that could be attained in this type of work with the resistivity methods that were to be employed. These methods had been introduced into the work of the Conservation Branch by Benjamin E. Jones for the investigation of dam sites, and have been used under his direction by the author for such work. If the method proved to be be an effort was to be made to contour the top of the salt beds and also the other formation boundaries known to be present in this area. Salt-water aquifers were to be studied in an effort to determine their boundaries, and an attempt was to be made to delineate the potash-bearing beds. Earlier Studies Others have made, and reported, restivity studies over saliferous deposits in different areas. Friedell and Messrs. Schlumberger2 reported geophysical work performed in the discovery of the salt domes of Alsace; Carrette and Kelly? described the geology of the same area. Leonardon and Kelly' published a resistivity curve obtained over the Hettenschlag dome, and a further discussion of this same area was given by the Messrs. Schlumberger6 in a communication. Messrs. Alty6 described studies on salt deposits in which the single-probe method was used. sinerez7 mentions that electrical methods were tried over salt deposits in Spain. Geoffrey and Charrin8 show a resistivity curve obtained over marl, gypsiferous marl and salt which is similar to that obtained over the New Mexico salt deposits. Kelly9 reported resistivity work performed with the ground Comparaor of Zuschlag over the salt deposits near Syracuse, N. Y., where the Salina formation is at a depth of 700 to 800 ft. Some structural studies on the potash basin of Alsace are described by Poldini.10 Another single-probe resistivity study, made over salt deposits in New Mexico, is briefly described by Heiland,11 through the courtesy of Harry Aurand, of the Midwest Refining co, Geological Features OF Area Covered The area discussed in this paper is in Eddy County, southeastern New Mexico, a

Jan 1, 1946

By William E. Bonini, Eugene A. Hickok

IN the course of an investigation directed toward expanding ground-water facilities in Essex and Morris counties, New Jersey, the Board of Water Commissioners of the city of East Orange authorized a seismic-refraction survey1 for the purpose of delineating bedrock topography below unconsolidated overburden. Results of the survey were highly satisfactory and led to the preparation of a comparatively detailed bedrock contour map. Knowledge of the bedrock depth and configuration was an important aid in selection of sites for test drilling. The portion of the East Orange Water Reserve under consideration is in the flood plain of the Passaic River about 10 miles west of Newark, N. J. The flood plain is about 175 ft above mean sea level and is bordered by low hills rising to elevations of approximately 250 ft. The bedrock underlying the Water Reserve consists of sandstone and shale of the Triassic Brunswick formation and is covered everywhere by deposits of unconsolidated glacial outwash sand and gravel, lacustrine clay, and recent river silt as much as 150 ft thick. Yield of wells in the sandstone and shale averages 100 to 200 gpm. Since production wells constructed in the sand and gravel aquifer in the buried river valley shown on the contour map (Fig. 1) yield 300 to 1400 gpm, it was proposed to locate additional production wells in this buried valley, where the yields per well would be maximum.

Jan 4, 1958

By I. S. Levy, J. L. Brimhall, B. Mastel

Specimens of' Hastelloy X-280, a low-cobalt version of the solid-solution- hardened nickel-base alloy Hastelloy X, were given a series of thermomechanical treatttzents. They were then Lensile-tested at room temperature and 1350°F. The Microstructures of the specimens tested at 1350°F were studied by electron Microscopy. Microscopy showed that dislocation tangling, caused by the cold working, mas still in evidence after aging-for 24 hr to temperatures as high as 1550oF. (Cr, Mo)23 C6, (Fe, Mo)6 C'. as well us an unidentifiable phase precipitale due to the combination of the thermomechanical treatments and subsequent tensile strain. The room -temperature and 1350°F tensile properties show a general increase ill strength and decreccse in ductility with increusing cold-work level. This is due to the dislocation taangling-. PerLurbatiot~s to this general trend occur- due to solid-solution weakening at the higher cold-work levels as a direct result of the preciplitation reactions. THE requirements for corrosion resistance and high-temperature strength place nickel-base alloys among the more promising materials for advanced nuclear reactor applications. However, when these alloys are irradiated at service temperatures, they generally suffer severe embrittlement'" and reduction in rupture life.3 Certain experimental treatments resulted in improvements in the tensile and stress-rupture properties of Hastelloy X-280, a solution-hardened nickel-base alloy.' To provide a basis for understanding these improvements, unirradiated tensile specimens were examined by electron microscopy. The results are reported in this paper. EXPERIMENTAL DETAILS Material. Hastelloy X-280, a low-cobalt version of Hastelloy X, is a member of the solution-hardened class of nickel-base alloys. The Hastelloy X-280 was obtained from 4- and 1-in: thick plates in the mill -annealed condition. Table I gives the chemical composition of the material as reported by the National Spectrographic Laboratories. ~x~erimental Treatments. Plates of suitable size, 12 by 3 by 1 in., or by + in., were cut under a water jet from the stock material and examined ultrasonic -ally for homogeneity of grain size and absence of voids. The acceptable plates were solution-treated at 2150°Ffor 1 hr and air-cooled. These plates were then reduced in thickness by cold rolling 0, 10, 15: or 20 pct along the original rolling direction. The plates were machined into buttonhead tensile specimens with a gage diameter of 0.125 in., with a gage length of 1.125 in., and with their tensile axes parallel to the rolling direction. The specimens were examined for quality of finish with a penetrant dye, ultra son ically checked for voids, and finally given a dimensional tolerance check with an optical comparator. The acceptable specimens were aged for 24 hr at either 1000" or 1500 F and air-cooled. These specimens were then held at 540°F in a water loop for approximately 18 days to qualify as controls for similar specimens irradiated under the same conditions of time, temperature, water chemistry, and flow rate. Table U summarizes the treatments. These treatments were investigated to establish whether prior precipitation and stabilization of carbide phases at strain sites within the matrix could reduce the amount of carbides available for precipitation at grain boundaries during service. Tensile-Test Conditions. Specimens were tested to fracture at room temperature or 1350 F in air on an Instron tensile-testing machine at a crosshead speed of 0.05 in. per min. The time for the furnace to reach equilibrium at 1350°F was approximately 30 min; soak time prior to testing was 15 min; and test duration was approximately 5 min.

Jan 1, 1968

By H. W. Knott, M. H. Mueller

The crystal structures of Ti2Cu, Ti2Ni, Ti4Ni2O, and Ti4Cu20 have been determined using powder specimens examined by X-ray and neutron diffraction. Lattice constants have been determined for all four phases using X-ray powder diffraction films. Atom positional parameters of all four phases have been determined from observed neutron intensities. X-ray diffraction calculated intensity data have been presented also for the phase Ti2Cu to point out the particular suitability of neutron diffraction in this case. Interatomic distances have been determined using the positional parameters obtained from neutron diffraction. ALTHOUGH some investigations of the crystal structures have been made of these four compounds previously,'-13 it was the purpose of the present investigation to expand the previous work in order to locate the various atoms, determine their coordinates, and to confirm or to correct some of the previous work. It was convenient to group these four compounds together since they are related chemicallv and/or structurally. The compound Ti2Cu is tetragonil; and Ti2Ni, Ti4Ni2O, and Ti4CU2O are all large fees of the same space group. Ti2Cu has been previously reported as a fee phase by Laves and Wallbaum;1 and Rostoker2 which was possibly the oxide phase, Ti4Cu20. Joukainen, Grant, and Floe;3 and Trzebiatowski, Berak, and Ramotow-ski4 have also reported a phase of this composition. karlsson5 has reported a small fct phase of the composition Ti3Cu which may be the presently discussed Ti2Cu phase. More recently Ence and Margolin6 have reported a small fct phase for Ti2Cu and the present authors7 together with Nevitt8 have briefly reported it to be a bet related to the fct with a co three times the length of the co of the fct and have also reported that this phase has a very limited composition. Further refinements will be reported which have varied some of the parameters of this bct structure slightly. Ti2Ni has been reported as a fee phase by Laves and wallbaum;1 Duwez and taylor;9 Rostoker;2 Poole and Hume-Rothery;10 and Yurko, Barton, and parr.11 In a later paper Yurko, Barton, and parr12 have given the complete structure of this phase based on an X-ray diffraction study which was independently confirmed with neutron diffraction by Mueller and knott.7 Additional crystal structure information will be given. Ti4Ti2O, Ti4Cu2O, and a number of other compounds including Ti4Fe2O have been reported as fcc phases by Rostoker,2 and more recently Nevitt13 has confirmed the Ti4Ti2O phase. Rostoker,2 however has reported diffraction lines for Ti4Fe2O which do not have all odd or all even indices. These lines, therefore, cannot be observed if this compound has a fee structure. This same error has crept into the diffraction results reported for TiNi2O and Ti4Cu20 in the ASTM powder data which has been credited from Rostoker's data. Complete crystal structures of these two phases will be presented. Although all four of these structures have large unit cells and hence do not lend themselves for completely resolved neutron powder patterns, a sufficient number of individual reflections was observed for solving the structure. They also serve as good examples of some of the advantages to be gained by using both neutron and X-ray diffraction techniques. EXPERIMENTAL PROCEDURE All of the alloys were prepared by arc melting. The starting metals had the following purity: Cu 99.999 pct, Ni 99.83 pct, and Ti 99.92 pct. Oxygen was introduced into the two oxide phases as chemically pure TiO2, with the remainder of the titanium coming from the above mentioned metal. All of the sample buttons were annealed in evacuated Vycor tubes, the two binary phases for 5 days at 700°C and the two oxide phases for 3 days at 900°C. Oxygen analyses were performed on all four phases by two independent laboratories with the following amounts of oxygen present in atomic percent; Ti2Cu-0.06, Ti2Ni-1.03, Ti4Ni2O-13.95, and Ti4Cu20-13.87. The stoichiometric amount for the oxide phases is 14.29 at. pct. Since all of the samples were very brittle they were easily reduced to a powder for diffraction measurements. The lattice constants given in Table I were determined for the four compounds from X-ray diffraction patterns of powder samples exposed to filtered copper radiation using a 114.59 mm diam Debye-Scherrer type camera using the Straumanis loading. None of the patterns showed a detectable amount of a second phase. The lattice constants were obtained from an IBM 704 computer program employing a least squares treatment with systematic correction terms as previously reported.14

Jan 1, 1963

By W. A. Backofen, G. Y. Chin, W. F. Hosford

The effect of machine stiffness on discontinuous flow and fracture of the 2024 aluminum alloy was studied in tension at 4.2OK. An increase of machine stiffness was found to decrease the amount of elongation and drop in load during discontinuous flow, thereby postponing fracture to larger strains and higher stresses. The possibility of utilizing stiffened tools in deformation processing to suppress shear fracture originating from unstable flow was indicated. The problem of nucleating discontinuous flow and the role of the effective mass of the system in discontinuous flow were also considered. AT low temperatures the plastic flow of metals is often discontinuous, with sudden load drops and elongations.1,3 Basinski1,4 has presented strong evidence that discontinuous flow, at least in aluminum alloys, occurs under nearly adiabatic conditions. During testing the load may drop suddenly and flow become localized when the thermal softening, due to heat generated in plastic straining, is greater than the strain and strain-rate hardening. This instability criterion is more easily satisfied at low temperatures because 1) the volume specific heat is reduced so that relatively large temperature increases are possible in straining, and 2) the flow stress is relatively temperature-dependent. The important role of adiabatic shear in ductile fracture processes has been emphasized,5-1 and consideration has already been given to the influences of thermal and mechanical properties on the tendency of a material to undergo adiabatic shear.17677 By focusing attention on how the mechanical loading system influences low-temperature discontinuous flow, additional insight into adiabatic shear and its effect on fracture may be gained. EXPERIMENTAL PROCEDURE Because of its low thermal conductivity, the 2024 aluminum alloy exhibits a highly consistent discon- tinuous-flow behavior at 4.2°K and was therefore chosen as the material for study. Machined specimens of 0.113 in. diam and 1.125 in. gage length were solution heat-treated at 490°C for 3 hr, quenched into cold water, and immediately immersed in liquid nitrogen until just before testing. Testing was done at 4.2°K by immersion in liquid helium at a crosshead drive rate of 0.03 in. per min. As normally used (hard-machine basis), the spring constant of the testing machine was k = 25,000 lb per in. By inserting beam springs in series with the specimen, this value could be lowered by a factor of about 100. Details can be found elsewhere.? As a result of variable machine stiffness, the actual strain rate ranged from about 3 x 10 5 to 3 x 10-4 per sec from one test to another, as well as within any one test. However, preliminary tests had established that the tensile curves were not altered significantly by this strain-rate variation. Fig. 1 shows a typical load vs plastic-elongation curve for a solution heat-treated 2024 aluminum alloy specimen pulled in the standard hard machine (k = 25,000 lb per in.) at 4.2"K. The elastic extension has been subtracted. Plastic flow proceeded smoothly from yielding at approximately 22,000 psi (load = 220 lb) to a strain of about 4 pct at which point the flow became discontinuous. The magnitude of the load drops as well as the plastic elongation per drop increased with increasing strain until the specimen finally broke abruptly. The load-elongation behavior of a sample tested with a relatively soft machine under otherwise identical conditions is given in Fig. 2. In general, there

Jan 1, 1964

By Alan F. Stewart, Douglas R. Piteau, Dennis C. Martin

Three examples of open pits where toppling failure controls the stability and design of the slopes are described. Two examples involve the design of overall slopes in base metal mines. The third example concerns the analysis and design of remedial measures to prevent toppling failure from occurring in a critical slope in a coal mine. The analytical techniques for assessing toppling failure on a rational basis are discussed for the three examples. This includes an assessment of the important parameters which govern the stability for the toppling failure mode. The geological setting and input data for each example are described, as are the important external or limiting factors pertinent to the sites in question. A statistical cumulative technique was used to assess one of the most important input parameters in the two examples involving overall slope design. Both deep-seated toppling failures, involving the entire slope, and shallow bench failures are considered. Results of the stability analyses and their related engineering significance with regard to slope stability and design are discussed. A sensitivity analysis of various parameters is effectively utilized. Design charts are developed and evaluated accordingly. In the example where toppling failure was unavoidable, the rationale for design of stabilization techniques to prevent toppling is discussed.

Jan 1, 1983

By E. C. Dominguez

INTRODUCTION The first commercial plant in the world to successfully produce pellets from manganese ore fines is the ICOMI pelletizing facility in northern Brazil. The main purpose of this paper is to describe the manganese pelletizing process that was developed through a cooperative R & D program by the Bethlehem Steel Corporation and ICOMI, i.e., Industria e Commercio de Minerios, S. A. The process combines heavy- media and gravity separation, reduction roasting, magnetic separation, and pelletizing on a straight-grate indurating machine. It produces high-grade manganese pellets from reviously unsalable low-grade ore fines at a rate of 20,000 tonnes (1) per month. The physical properties of the manganese pellets are comparable to those of iron ore pellets. The pelletizing plant, built at a cost of about 18 million dollars, is part of an ICOMI complex that includes manganese ore mining, an ore-washing plant, and railroad and port facilities, as well as two town sites. These two towns, one at the mine and the other at the port, each with complete community services, were built by ICOMI to serve the needs of over 1500 employees that operate the industrial complex. To give an idea of the magnitude of the investment represented by this complex, the cost up to 1957 to develop the mine and supporting services and social infrastructure was over 100 million dollars. It should be borne in mind that the above capital cost figures are in dollars of the years during which the respective projects were initiated and completed.

Jan 1, 1977

By H. H. Podgurski, H. E. Knechtel

Annealed Fe-Al alloys do not react readily to form AlN when held at 500ºC in NH3-H2 gas mixtures, but do so upon the introduction of dislocatims. Nuclea-tion of the nitride phase occurs on dislocation sites. In turn, the growth of the aluminum nitride particles causes the ferrite phase to yield plastically, generating more dislocations for the nucleation process. The nitride phase extracted from an Fe-2 pct A1 alloy nitrogenated at 500°C was identified as stoichio-metric aluminum nitride with a hexagonal crystal lattice. THIS investigation reveals the role that dislocations play in initiating and sustaining the nitriding reaction in Fe-A1 alloys. As early as 1931 the work of Meyer and Hobrock1 suggested that the initiation of the nitriding reaction could involve a nucleation controlled process. Recently Bohnenka2 depicted the gas-phase nitriding process below 600°C as one of mixed control limited by nitrogen penetration through the surface, by nitrogen diffusion, by aluminum diffusion, and by nucleation of the nitride phase, Fig. l(a). In our research in a comparable alloy (0.57 pct Al) at 575ºC, we have observed a nitrogenation which we feel is better described by Fig. l(b). In the case of a 2 pct-A1 alloy partially nitrided at 500°C we propose the profiles shown in Fig. l(c). For a complete and accurate description of the process, a concentration profile of the dislocation density in the test specimen would be needed. EXPERIMENTAL Nitrogenization was conducted between 500" and 575°C in a variety of NH3-H2 gas mixtures on three Fe-A1 alloys: 1) zone-refined iron + 0.16 i 0.2 pct Al—levita-tion melt, 2) zone-refined iron + 0.57 0.02 pct Al— levitation melt, 3) plastiron + 2 pct Al—melted by induction heating. To demonstrate the effect of dislocations on reactivity, both cold-worked and annealed samples were investigated. All nitrogenation rate studies were conducted gravimetrically with a gold-plated invar balance4 contained in a gas-flow system. To avoid contamination of the specimens in the reaction zone of the system, the reaction chamber was constructed of high-purity dense alumina. The activity of nitrogen was fixed by specific NH3-H2 gas mixtures whose compositions were continually monitored by calibrated thermal conductivity gages and checked by chemical analysis. Variations of ± 0.1 pct NH3 could easily be detected by both methods. Throughout this paper the activity of nitrogen is defined as PN3 /PH23/2 , where PNH3, and Ph2 are partial pressures in atmospheres. Electron transmission, density measurements, and chemical analyses were made on specimens before and after nitrogenating in order to reveal structural and chemical changes. Similar studies as well as X-ray diffraction studies were conducted on nitride extractions from the nitrogenated 2 pct-A1 alloy. These extractions were obtained by the use of an anhydrous bromine-methyl acetate solution which dissolves the iron and leaves the insoluble nitrides as a residue. Hardness profiles were obtained on cross-sections of partially nitrided specimens to demonstrate the extent of nitriding through the thickness of the specimens. RESULTS AND DISCUSSION The nitrogen activity in the NH3-H2, atmospheres was never allowed to reach a level capable of producing iron nitride (Fe4N). Hence, the term nitriding as used in this paper refers only to the formation of aluminum nitride whereas nitrogenation refers to the total uptake of nitrogen regardless of how it is distributed throughout the alloy. The weight increases observed during the initial stage of a nitrogenating treatment are due primarily to the solution of nitrogen in the ferrite phase, particularly when starting with annealed specimens. Because this initial nitrogenation rate in the case of the 0.57 pct A1 alloy, see Figs. 2 and 3(a), was most rapid the weight change that occurred thereafter might be attributed to the nitriding reaction with the exception of a small weight increment due to the irreversible pickup of oxygen by aluminum. The oxygen (<70 ppm) came from traces of H2O and 0, in the hydrogen and ammonia gases. On the basis of discrepancies between total weight increase and the increase in the nitrogen content of the sample as determined by chemical analysis, it was estimated and later established by activation analysis, that as much as 200 ppm of oxygen were taken up by a fully nitrided Fe-0.57 pct A1 specimen at 575°C. Most of the oxygen could have been picked up from the nitriding atmosphere on the surface of the samples during cooling to room temperature. Even 50 ppm of water in the gas phase will become oxidizing to iron before the sample has cooled to room temperature. The lack of reactivity* of these alloys in the annealed

Jan 1, 1970

J. D. Fast and J. L. Meijering (Philips Research Laboratories, N. V. Philips&apos; Gloeilampenfabrieken, Eindhoven, Netherlands)— After the departure of our friend Dijkstra to the United States, investigations on the effect of alloying elements on the behavior of nitrogen in a iron were continued in Eindhoven. We too found internal friction curves with two separate peaks for iron containing nitrogen in addition to 0.5 atomic pct V or 0.5 atomic pct Mo. Our first publication on these investigations" appeared almost simultaneously with the paper now under discussion. At first sight our experimental results seem to be in harmony with their conclusions, but a closer examination reveals that in the case of the Fe-V-N alloy the abnormal peak is not controlled by one time of relaxation only. Whereas iron containing 0.5 atomic pct Mn or Mo absorbs an amount of nitrogen of about the same magnitude as that absorbed by pure iron under identical conditions, iron containing vanadium absorbs in addition one nitrogen atom for every vanadium atom. This last amount, far exceeding the first amount in the case under consideration, combines chemically with the vanadium and causes no internal friction. The "free" nitrogen in the vanadium alloy gives rise not only to a damping peak corresponding to that in pure iron but— due to the presence of VN particles in the metal—also to the abnormal peak at higher temperatures. The VN particles create interstitial sites around themselves where the free nitrogen atoms are bound much tighter than in the normal interstices. These abnormal interstices, therefore, will capture free nitrogen atoms rapidly, whereupon these give rise to the abnormal damping. The binding energy in the abnormal interstices is not the same for all, and with coarsening of the VN precipitate the distribution of these energies is displaced toward the side of stronger binding. This is deduced from a shift of the summit of the second peak toward higher temperatures (from 80" to 88°C in our experiments) caused by prolonged heating at 950°C. From the intermediate state where they cause the abnormal damping, the nitrogen atoms pass over rather rapidly into the fully precipitated state (iron

Jan 1, 1954

By R. H. Hiltz

Three titanium alloys, known to provide a mechanically unstable p structure after quenching, were selected as material for a study of the Origin and nature of stress-induced transformation. Data from hardness and tensile tests were used to study the initiation of marten site and the effect of the transfornation and transformation products on the mechanical properties of B titanium, particularly the stress-strain relationships. With the exception that the materials investigated showed a natural aging reaction in the P condition, their behavior is analogous to that of&apos; stress-transforming stainless steels. The transformation starts after initial yielding and is essentially complete just prior to .maximum loading. Once initiated, the martensite itself is capable of propagating the transformation. The deforn-ing materials show low strength, high ductility, and a high strain-hardening exponent. In metallic systems which undergo a diffusionless transformation on cooling, it is possible to produce a similar transformatiorl by plastic deformation under special conditions. Dewez&apos; in delineating Ms temperatures for the titanium-rich end of most titanium binary systems:, established the point of intersection of Ms with room temperature for those particular alloys. Alloy compositions which would quench to mechanically unstable p were established from these data. The first investigation into the possibility of stress-induced transformation occurring in titanium met with little success. It was concluded that such a transformation in titanium was possible only under very special conditions. Continued effort in this direction, however, showed certain Ti-Mo binaries to be highly susceptible to this phenomenon. This fact was utilized by Liu to study the habit planes of martensite and by Machlin and wenig5 to study the effects of stress and plastic deformation on the P to a prime transformation in titanium alloys. The first investigation of the mechanical properties of these alloys was conducted by Holden and his coworkers at Battelle Memorial Institute.&apos; The potentiality of the alloys i3s sheet-forming material was recognized, and the data reappeared in a survey of this type of titanium material.? The initial optimism was tempered by the difficulties in obtaining homogeneous 2i-Mo alloys in commercial-size ingots. The increasing need for good sheet-forming material kept investigation in this direction active, resulting in the development of a commercial alloy of this type.&apos; This study was undertaken to obtain a clearer picture of the mechanism of stress-induced transformation in titanium. MATERIALS AND TEST PROCEDURE Three alloys were selected for this investigation: one a Ti-Mo alloy; another a Ti-Cr-Mo alloy, known to deform martensitically; and the third, a Ti-V alloy with an Ms below room temperature and an Md above room temperature, but known to contain w phase in the quenched condition. The compositions of these alloys are given in Table I. These alloys were cast as 5-lb experimental ingots, employing skull melting. The ingots were hot-forged into 1-in.-round bars. Two 72-in.-thick slices were cut from each bar for hardness testing; the remainder was cut into 0.252-in. tensile blanks. The tensile blanks and one hardness disc from each bar were heated in salt to a temperature 100°F above the 0 transus, held 2/2 hr, and brine quenched. X-ray analysis showed the pieces to be 100 pct 8.* *Omega cannot be distinguished from p by the technique employed. Tensile blanks were machined to size after this treatment. TO prevent transformation due to machining stresses, the shoulders and gage length were ground. True stress-true strain curves were

Jan 1, 1960

By G. S. Tint, M. Herman, V. V. Damiano

Dislocation arrays and substructures were studied in cadmium doped zinc crystals using a newly devised etching technique. Cadmium precipitates delineating the dislocations were revealed by etching a surface closely parallel to the (0001) slip plane. Cinephotomicrography of the continuous etching process revealed the three-dimensional aspects of dislocations in the bulk crystal. Dislocation etch patterns were studied in both deformed and annealed crystals after suitable aging at room temperature. The effect of annealing was evidenced by a rearrangement of the dislocations into low-angle boundaries and hexagonal networks. ETCH pit techniques have been used extensively to study dislocations in both deformed and annealed bulk metal crystals. Ideally one hopes to obtain a one-to-one correspondence between the etch pits and the points of emergence of the dislocations at the surface. One then attempts to deduce the way in which dislocations are arranged in the bulk crystal from the arrangement of etch pits on the surface. It is clear that one can obtain only limited information of the dislocation configurations inside the crystal from etch pit studies of single surfaces. Considerably more information is obtained if one is able to follow the course of the dislocations through the crystal using progressive etching technique. Techniques of this sort were used by Gilmanl to study dislocations on the slip planes of NaCl crystals and by Damiano and Tint2 to study dislocation arrangement in zinc crystals grown from the melt. The present paper makes use of a technique first described by Tint and Damiano3 to observe and continuously record the dislocation structures which appear while a crystal surface was being progressively etched. Studies were made on cleaved (0001) surfaces to reveal the dislocations along their length on the surface closely parallel to the slip plane. The technique for revealing segments of dislocations along their length by etching is well known. Wilsdorf and Kuhlmann-wilsdorf4 revealed disloca- tions along their length in aluminum containing a few percent copper, when precipitates segregated along the dislocations. The technique was used by Low and Guard5 to study dislocation configurations on the slip plane in Fe-Si alloys containing carbon. In the present work the technique was applied to zinc containing cadmium since it was shown by Gil-man6 that a cadmium-rich phase could be made to precipitate from supersaturated solutions along dislocations in zinc. Segments of dislocations delineated by the precipitates were revealed by etching a surface prepared by cleaving the crystal. The three-dimensional nature of dislocations and substructures was thus studied from the cinephotomicro-graphic record of the continuous etching process. EXPERIMENTAL Single crystals of zinc containing the order of 0.1 pct Cd were prepared by slowly lowering a graphite crucible containing the melt through a temperature gradient of 15°C per cm at a rate of 1.5 X 10-3 cm per sec. "As grown" crystals were aged for periods of 1 month at room temperature, then cleaved in liquid nitrogen, and etched according to the procedure used by Gilman.&apos; The etchant containing 32 g of CrO3, 6 g of hydrated Na2SO3 in 100 ml of water behaved as a chemical polish for zinc and etch pits were produced at the site of precipitates or inclusions. After the precipitates or inclusions were removed from the surface, the etch pits left behind were eventually polished smooth. This behavior enabled one to continuously observe the surface while the specimen was immersed in the etchant. Best results were obtained when the specimen surface was vertical and the reaction products of polishing were continuously removed by gravitational convection. Some crystals were heavily deformed in excess of 25 pct strain, others were lightly deformed the order of a few pct by compression such that the deformation occurred essentially by basal glide. Some crystals were etched immediately after deformation, others were allowed to age at room temperature for several weeks prior to etching. Heavily deformed crystals were annealed at various temperatures and etched on the cleavage plane immediately after annealing, others were allowed to age at room temperature for several weeks prior to etching. The etched structures of deformed and annealed structures were studied. Similar experiments were conducted on 99.9999 pct pure zone refined Tadanac zinc crystals which

Jan 1, 1963

By P. T. Chiang

Chemical etching methods for the simultaneous revealing of the tellurium or selenium Phase and the chalcogenide grain boundaries of the alloy systems are given. A tellurium eutectic was found Present in zone-melted ingots. Similarly, a selenium monotectic was present in ingots. In general, the second phase (tellurium or seleniumn) occubies three different sites; viz., along the chalcogenide grain boundaries, as inclusions within the chalcogenide grain, and on the undersurface of the ingot. The detection limit for the tellurium phase is about 1 u in width. THERMOELECTRIC materials based on Group V (bismuth, antimony) and Group VI (selenium, tellurium) elements have aroused considerable interest in recent years in the practical application of thermoelectric cooling. In many cases, a small amount of excess tellurium (or selenium) was added to the material to optimize its thermoelectric properties. Then the question immediately arises as to the number of phases present in the resultant alloy. In the binary systems of Bi-Te, Sb-Te, and Bi-Se, the congruent melting compositions have been reported to be non-stoichiometric and are represented by Bi~Te respectively. It is to beexpected and known that Bi2Te3 and SbzTe3 crystallize from the melt with an excess of bismuth and antimony in the lattice and that tellurium forms a eutectic.~&apos; The same could be assumed to take place in the pseudo binary systems of (Bi,Sb)zTe3 and Bi2(Se,Te)3 as well as in the system studiedby puotinen5 and other workers. Likewise, BiaSe3 crystallizes from the melt with an excess of bismuth in the lattice and selenium forms a monotectic.~ Therefore, in practice, alloys solidified from the melt often contain a second phase (tellurium or selenium) in one region or another of the solid mass even without the addition of excess tellurium (or selenium). ~u~~recht&apos; studied the thermoelectric properties of (Bi,Sb)2Te3 alloys with excess tellurium and simultaneous additions of selenium. He mentioned that the materials show two phases because of the considerable excess of tellurium or selenium. However, he did not report as to how the tellurium or selenium phase was identified. It is generally believed that the presence of an excessive amount of tellurium or selenium phase in the alloy would adversely affect its thermoelectric properties and its uniformity. Consequently, there is a need for a simple method for the identification of the tellurium and selenium phase. The quantity of the second phase present is usually too small to be detected either by chemical analysis or by normal X-ray techniques. This investigation was therefore carried out, first, to devise a simple metallographic method for the identification of the tellurium or selenium phase coexisting with the chalcogenides and, second, to determine the distribution and specific location of the tellurium or selenium phase in the ingots. EXPERIMENTAL PROCEDURE The starting materials used for the alloy preparations were 99.999 pct pure bismuth, antimony, and tellurium and 99.997 pct pure selenium. The bismuth and antimony were obtained from Consolidated Mining and Smelting Co. of Canada Ltd., while the selenium and tellurium were obtained from Canadian Copper Refiners Ltd. The tellurium was purified further in the laboratory by zone refining. The elements were pulverized in a stainless-steel pestle and mortar. The amounts for the desired composition were weighed out each time on an analytical balance to make up a 100-g sample. Then the sample was introduced into a Vycor ampule (19 by 150 mm), pumped down to a vacuum of 10"5 Torr for 15 min, and sealed off. The ampule was then heated in a horizontal resistance furnace at 800" to 900°C for about 20 hr. During this period the assembly was rocked back and forth several times to ensure good mixing. At the end of the heating period, the ampule was quenched in cold water and then transferred to the zone-melting apparatus described in a previous publications to grow large-size aligned polycrystals. The background and ring-heater temperatures were adjusted to make the freezing solid-liquid interface slightly convex to the liquid. The recorded temperature gradient in the vicinity of the freezing solid-liquid interface was around 15°C per cm. The ampule was moved horizontally at a speed varying from 0.4 to 2 cm per hr so that the ring heater would cover the whole ingot length from end to end. A single zone-melting pass was used for the Bi-Te, Sb-Te, and Bi-Sb-Te ingots. Two passes in the forward and reverse directions were carried out for the Bi-Se and Bi-Se-Te ingots. Six passes in the forward and reverse directions were performed for the Bi-Sb-Se-Te ingot. The zone-melted ingots were found to contain several large crystals, with their basal planes (0001) approximately parallel to the growth axis. Samples of bismuth and antimony tellurides coated with a layer of tellurium, and bismuth selenide coated with a layer of selenium, were prepared for comparison in phase identification. These coatings were made by dropping a piece of the zone-melted ingot into some molten tellurium or selenium under argon atmosphere and allowing them to cool slowly to room temperature. The metallographic specimens were prepared by

Jan 1, 1969

By M. J. Marcinkowski, A. S. Sastri

A detailed compressive stress-strain analysis and transmission electron microscopy investigation has been made of the deformation behavior occurring in a 50 at. pct Ni-Ti (hypoeutectoid) alloy and a 54.5 at. pct Ni-Ti (hypereutectoid) alloy. In the case of the hypoeutectoid alloy, three stages of work hardening are observed. Stage I occurs at a very low stress and is associated with plastic deformation via martensite formation. Stage 11 is characterized by very rapid work hardening and is due to difficulties in causing further deformation in the fine martensite aggregate produced in Stage I. Stage III which occurs at very high stress levels is characterized by smaller work hardening rates and is due to the plastic deformation arising from alternate reconversions of the original martensites to martensites of varying orientation. Rapid quenching of the hypereutectoid alloy leads to very high yield strengths and is related to a fine precipitate dispersion that such treatment brings about. The present investigation represents the final phase of a three-part study directed toward an understanding of the solid-state transformations in near equi-atomic Ni-Ti alloys as well as the deformation mechanisms associated with these alloys. In the first part,"2 to be henceforth referred to as I, it was found that alternate simple shears on {112} planes and in (111) directions convert the parent B2 structure in the equiatomic NiTi alloy into two distinct close-packed monoclinic martensites. All of the marten-sites were of this type, whether they were formed by cooling or by plastic deformation, whether induced to form in bulk samples or in thin foils, or whether examined in the electron microscope at room temperature or below. On the other hand, in the second part of this investigation,3 to be reffered to as 11, it was shown that upon slow cooling to about 640°C. alloys in the neighborhood of NiTi which possess the B2 structure transform eutectoidally into their equilibrium phases Ti2Ni and TiNi3. However, preceding the formation of these equilibrium phases a series of metastable intermediate phases are formed. This paper will set as its goal the elucidation of the remarkable deformation behavior exhibited by NiTi. In particular, Buehler and Wiley4 have found equiatomic NiTi to be surprisingly soft, while Buehler et al.5 have shown this alloy to possess a memory effect: i.e., upon bending at room temperature it will revert to its original shape when heated to above about 50°C. In I it was shown that NiTi was soft in the sense that the yield stress was low; nevertheless, the alloy work-hardened at an extremely rapid rate to very high stress levels. On the other hand, the hypereutectoid alloys with somewhat higher nickel, say 54.5 at. pct (60 wt pct) have enormously increased yield strengths compared to those of the equiatomic alloys. In order to determine the atomistic processes giving rise to the above behavior, it was decided to examine samples that were wafered from bulk specimens deformed in compression to various strains using the techniques of transmission electron microscopy. EXPERIMENTAL TECHNIQUE All of the alloys used in the present investigation contained either 50 at. pct Ni (55.06 wt pct) or 54.5 at. pct Ni (60 wt pct) and were arc-melted in the form of a finger using the same techniques described in I and II. The finger was capsulated in a stainless-steel jacket and swaged at 850°C into rods. Compression specimens 0.300 in, long and 0.200 in. in diam were machined from these rods. In order to completely re-crystallize the samples and remove residual stresses, all of them were capsulated in evacuated quartz, annealed for 1/2 at 1050°C. and then furnace-cooled. Compression tests were carried out in an Instron tensile testing machine covering a range of temperatures from —196° to 200°C using procedures described previously.6&apos;7 In all cases crosshead speed was 0.02 in. per min. Wafers 0.015 in. thick were spark-cut from the cylindrical samples at 45 deg to the compression axes after they had been deformed to the desired strain. These specimens were then spark-planed to about 0.005 in. and then electrochemically thinned for examination by transmission electron microscopy as described in I.

Jan 1, 1969

By R. G. Woolery

INTRODUCTION Since 1975, Union Carbide Corporation has been conducting uranium exploration in southwestern South Dakota. This program has resulted in the discovery of an ore body about eight miles north of Edgemont in Fall River County. The site which was previously mined for uranium in the 1950&apos;s and 1960&apos;s consists of 950 lode claims (approximately 20,000 acres) and is within the Black Hills National Forest. Preliminary development plans indicate that fewer than 200 surface acres will be involved in the mining and heap leaching of the ore. The ore occurs in both the Fall River and Lakota formations. The exploration to date has developed something in excess of two million tons of ore averaging -0.1% U308. About 75% of the ore is expected to be mined from underground with 25% coming from five to seven small pits. The surface mining will be extensions of previously mined areas with a disturbance of 35-40 new acres near 35-40 previously disturbed acres requiring a total reclamation of 70-80 acres. Several options for processing the ore including conventional milling by UCC, conventional milling in joint venture with another producer, and heap leaching are under consideration. This paper is concerned with the preliminary assessment of the heap leaching option based on the limited test work conducted on surface samples and on available cores from the deeper ones. The final design for a commercial operation will not be available until an underground bulk sample has been obtained and evaluated. Union Carbide has been operating heap leach facilities commercially since 1973 at Gas Hills, Wyoming and Maybell, Colorado. During this period, we have made considerable progress in heap construction

Jan 1, 1983

By L. Adler

A relatively simple and effective technique is proposed to deal with the failure of geologic masses containing weakness planes. This technique, termed irextended" rupture envelope, provides a means to clearly distinguish rock and soil from fractured rock and, on a theoretical level, considers a matrix-inclusion system. It may also constitute the link between Mohr&apos;s and Griffith&apos;s failure theories. Included in the article are five sample problems concerning site location, structural design, strengthening the plane of weakness, changing the magnitudes of major and minor principal stresses and changing the orientations of major and minor principal stresses. Engineers trying to solve design problems in rock and soil mechanics have often assumed an iso-tropic and homogeneous medium. For naturally occurring geologic masses this assumption has always been viewed with regret. The following analysis which deals with the effects of plane anisotropy on failure presents a solution to this. The planes of weakness are joints, faults, bedding planes, fracture and cleavage (natural and induced), foliation and schistosity. The physical properties of these weakness planes include an undulating surface, frictional resistance, discontinuous extent, filling material, tightness and presence of water to cause a hydrostatic pore pressure. All of these properties relating to failure can be summarized in Mohr&apos;s rupture envelope for the plane of weakness. This, along with the geometrical orientation, strike and dip, of the plane of weakness produces what is termed an irextended" rupture envelope. MOHR&apos;S STRESS CIRCLE AND RUPTURE ENVELOPE The significant features of these concepts are listed below.&apos; 1) A point on the u - r coordinate plane represents the normal and tangential stress components on a reference area in the material. This area can have any orientation. (Fig. la)

Jan 1, 1963

By W. Weissberger, Frankiewicz, L. Pommier

Introduction In the U.S., about one-quarter of the fuel oil and natural gas consumption is associated with power production in utility and industrial boilers and process heat needs in industrial furnaces. Coal has been an attractive candidate for replacing these premium fuels because of its low cost, but there are penalties associated with the solid fuel form. In many cases pulverized coal in unacceptable as a premium fuel replacement because of the extensive cost of retrofitting an existing boiler designed to burn oil or gas. In the cases of synthetic fuels from coal, research and development still have a long way to go and costs are very high. Another option, which appears very attractive, is the use of solid coal in a liquid fuel form - coal slurry fuels. Occidental Research Corp. has been developing coal slurry fuels in conjunction with Island Creek Coal (ICC), a wholly-owned subsidiary. Both coal-oil mixtures and coalwater mixtures are under development. ICC is a large eastern coal producer, engaged in the production and marketing of bituminous coal, both utility steam and high quality metallurgical coals. There are a number of incentives for potential users of coal slurry fuels and in particular for coal-water mixtures (CWMs). First, CWM represents an assured supply of fuel at a price predictable into future years. Second, CWM is available in the near term; there are no substantial advances in technology needed to provide coal slurry fuels commercially. Third, there is minimal new equipment required to accommodate CWM in the end-user&apos;s facility. Fourth, CWM is nearly as convenient to handle, store, and combust as is fuel oil. Several variants of CWM technology could be developed for different end-users in the future. One concept is to formulate slurry at the mine mouth in association with an integrated beneficiation process. This slurry fuel may be delivered to the end-user by any number of known conveyances such as barge, tank truck, and rail. Slurry fuel would then be stored on-site and used on demand in utility boilers, industrial boilers, and potentially for process heat needs or residential and commercial heating. An alternative approach is to formulate a low viscosity pre-slurry at the mine mouth and to pipeline it for a considerable distance, finishing up slurry formulation near the end-user&apos;s plant. Finally, at the other extreme of manufacturing alternatives, washed coal would be shipped to a CWM manufacturing plant just outside the end-user&apos;s gate. Depending on fuel specifications and locations of the mine and end-user facility, any of these alternatives may make economic sense. They are all achievable in the near term using existing technology or variants thereof. The Coal-Water Mixture CWMs contain a nominal 70 wt. % coal ground somewhat finer than the standard pulverized ("utility grind") coal grind suspended in water; a complex chemical additive system gives the desired CWM properties, making the suspension pumpable and preventing sedimentation and hardening over time. Figure 1 shows the difference between a sample of pulverized coal containing 30 wt. % moisture and a CWM of identical coal/water ratio. The coal sample behaves like sticky coal, while the CWM flows readily. The combustion energy of a CWM is 96-97% of that associated with the coal present, due to the penalty for vaporizing water in the CWM. Potentially any coal can be incorporated in the CWM, depending on the combustion performance required and the allowable cost. CWMs are usually formulated using high quality steam coals containing around 6% ash, 34% volatile matter, 0.8% sulfur, 1500°C (2730°F) initial deformation temperatures, and energy content of 25 GJ/t (21.5 million Btu per st). Additional beneficiation to the 3% ash level can be accomplished in an integrated process. There are a number of minimum requirements which a satisfactory CWM must meet: pumpability, stability, combustibility, and affordability. In addition, a CWM should be: resistant to extended shear, generally applicable to a wide variety of coals, forgiving/flexible, and compatible with the least expensive processing. It was found that a complex chemical additive package and control of particle size distribution are necessary to achieve these attributes simultaneously, while maximizing coal content in the slurry fuel. Formulation of Coal-Water Mixtures A major consideration in the manufacture, transportation, and utilization of a slurry fuel is its pumpability, or effective viscosity. Most CWM formulations are nonNewtonian, i.e., viscosity depends on the rate and/or duration of shear applied. Viscosities reported in this paper were obtained using a Brookfield viscometer fitted with a T-spindel and rotated at 30 rev/min, thus they are apparent viscosities measured at a shear rate of approximately 10 sec-1. The instrument does reproducibly generate a shear field if spindle size and rotation rate are held fixed. By observing the apparent viscosities of several slurries at fixed conditions it is possible to obtain a relative measure of their viscosities for comparison purposes. A true shear stress-shear rate relationship at the shear rates at which the CWM will be subjected in industry may be obtained using the Haake type and a capillary viscometer. These viscometers are used for specific applications. However, for comparison purposes, apparent viscosities are reported.

Jan 1, 1985

By R. C. Thompson

The lead-zinc mill of Phelps Dodge Corporation, Copper Queen Branch, Mines Division, Bisbee, Arizona, is about 3 miles from the main hoisting shafts of the Junction and Campbell mines at Lowell. All the ore treated in the mill is obtained from these two mines. The mill was designed for an all-flotation treatment of 450 tons of lead-zinc ore per day, and has been operated at that capacity since the start of milling operations on Nov. 17, 1945. An expansion program is underway whereby the mill capacity will be doubled, but this article describes only the original program and presents results of the 450-ton operation. General Description The milling plant consists of an ore-receiving bin and three steel-constructed buildings housing, respectively, the primary crushing equipment, the secondary crushing equipment, and the ore-storage bins, grinding, flotation, and filtering equipment. The mill site is the one that was used for a previous copper-concentrating plant, which was operated over a period of years and then dismantled. There remained from this operation some milling equipment, a reservoir for mill-water supply, railroad tracks, tailings-disposal ponds, and a steel-constructed building, all of which were incorporated in the design of the present lead-zinc mill. The location plan of the plant layout is shown in Fig I. The flowsheet of the mill is based on the conventional scheme for lead-zinc treatment, however, several innovations were made necessary in order to utilize the existing building. Placing of equipment also was governed by the design of the building; thus making the mill unique in many respects. The following brief description of the mill building as adapted to the flowsheet points out the compactness of the installation and some of its unusual features. The first floor (Fig 2) houses the grinding equipment, with connecting conveyors for ore feeding, also an air compressor, two vacuum pumps, bins for lead and zinc concentrate storage with individual conveying systems for loading the two kinds of concentrates. Filtering of concentrates is done on the second floor, the concentrates discharging directly into the concentrate-storage bins. On this floor are the lead and zinc filters, two diaphragm pumps, sample-filtering equipment, sample-preparation room and a change room for the mill employees. The flotation machines are on the third floor, at elevations allowing a gravity flow of the lead and zinc concentrates to the thickeners. The annex to the building contains a freight elevator and provides space for all reagent mixing and feeding, also storage of reagents and grinding balls. All the water used for milling purposes is pumped from the Junction mine and

Jan 1, 1949

By P. Barnes

(Resident Engineer, 1873-75.) SEVERAL statements have been made to the Institute, somewhat detached from each other, as to the cost of some parts of these works, but they have not included any extended description of the. buildings or machinery. The general plan of the work connected with the water supply differs, in some important details, from that which has been common either in the Pittsburgh district or elsewhere, and a somewhat extended description may be of interest to the Institute, in connection with a note of the cost of the work. The plan as a whole, and nearly all the important details, were developed by Mr. William P. Shinn, C.E., the general manager of the Company. The immediate and responsible charge of the work was in the hands of Mr. John C. Lewis, C.E., to whom had been committed all the work of this general description, including the laying-out of the whole of the foundations, the erection of the buildings, and the grading and laying down of the entire railroad system. The continuous operation of the machinery and other fixtures of these waterworks, for more than three years, has fully demonstrated the correctness and economy of the plan adopted. No casualties of any moment have befallen the apparatus, and no improvements have been suggested as important except that the gate at the river end of the conduit should have been made more completely water-tight, so that the whole length of the conduit could be pumped out dry without resort to any temporary dam in the conduit itself. In general terms the works of the Edgar Thomson Company are situated on a plateau, about 52 feet above the low-water level of the Monongahela River, and about 2000 feet from its bank. The site of the works is bordered on one side by Turtle Creek, a small stream which drains a considerable area of coal mining territory. This creek is about 100 feet from the group of buildings which have been erected, but it flows into the Monongahela River at a point, about 1200 feet further up than that selected for the entrance to the water-works conduit. It was ascertained by analysis that the water in the creek contains an important percentage of sulphate of lime, while the water of the river is of unusual purity, in respect of any salts

Jan 1, 1879

By Luiz C. Correa da Silva, Robert F. Mehl

A. D. Le Claire and R. S. Barnes (Atomic Energy Research Establishment, Harwell, Didcot, Berks., England)-—This much awaited paper admirably confirms that the Kirkendall effect is a true diffusion phenomenon and likely to be found in all diffusing systems. The most likely explanation put forward so far to account for the shift of interface is that the two components of the system, diffusing in opposite directions, do so with unequal rates so that there is a net loss of material from that half of the diffusion zone rich in the more rapidly diffusing component. This loss is accompanied, and at least partly compensated for, by a closing up or decrease in volume of this latter half of the diffusion zone and an expansion of the other half so as to tend to keep constant the overall volume per atom. This is manifest as a movement of the original interface. If this is a true picture of what is taking place then there are at least two important matters requiring further study."1—The quantitative relating of the observed shift with the independently measured separate diffusion coefficients of the two diffusing species."2—A detailed study of the mechanism and characteristics of the closing up process."We would like first to make a few remarks pertinent to these topics. In connection with the first of these, it is a pity that more and detailed measurements were not made on the Au-Ag system, the only one for which the separate diffusion coefficients of the two species have been measured.&apos;" One of us (A. D. Le C.) has calculated from Johnson&apos;s results the shift to have been expected in samples D.2 and D.3. Darken4 showed that the velocity v with which the markers move is related to the separate diffusion coefficients Dau, Dag, by the eauation:"dN"v = (Dag — Dau "dx"dN"where .is the concentration gradient at the mark-ax"ers. Under certain conditions,4, 20 it can also be shown that:"Xm"v = "2t"where x, is the total marker shift after time, t:"dN". . xm = 2t (Dag — Dau) [9]"dX"Johnson measured Dag and DAu in a chemically homogeneous alloy and so his reported figures represent the true or ideal diffusion coefficients"; the same quantities in eq 9 represent the actual diffusion coefficients as would be measured in the presence of a chemical concentration gradient, so we need to multiply Johnson&apos;s reported values of Dag and Dau by the"1 before insert-dlogN "ing them in eq 9. 7 is the activity coefficient of Ag at the concentration prevailing near the markers which we shall assume to be - 50 pct. The values of the thermodynamic factor for N = 0.5 and the temperatures at which D.2 and D.3 were annealed were obtained from thermodynamic data quoted by Darken.&apos; aN/ax was computed from the coefficient of inter-diffusion of Au and Ag given by Johnson on the assumption that in the samples D.2 and D.3, the concentration distance curve could be represented by the standard equation:""No is the original difference in concentration between the two halves of the couple, and + is the error or probability function."aN/ax at x = 0 is then given by:"adN/dx "2/nDt"and we assume that this represents the concentration gradient at the markers, although it is probable that the figure is slightly high."When all the appropriate quantities are inserted in eq 9, we find that the expected shifts are: for D.2, 0.0134 cm and for D.3, 0.0119 cm."The agreement between these results and those

Jan 1, 1952

By Luc Delaey, Horace Pops

The structure and morphology of thermoelastic and burst type martensitic phases that form upon cooling in Cu-Zn-Si p phase alloys have been studied by transmission electron microscopy. The martensitic phases are composed of a lamellar mixture of two close-packed structures with different stacking sequence, namely ABCBCACAB (orthorhombic) and ABC (fcc). Striations within thermoelastic martensite are most likely produced during interaction with impinging burst-type martensite and not as a consequence of secondary shears. In a study of the martensitic transformation in ternary Cu-Zn based 0 phase alloys1 the dependence of the martensitic transformation temperature, M,, with composition shows variations for elements within a constant valence subgroup and between different subgroups. Such variations are not reflected in a change in habit plane, which is approximately the same for each ternary alloy, namely in the vicinity of (2, 11, 12 Ip. The fact that the habit plane remained constant, despite large differences in M, temperature and electron concentration, suggested2 that the crystal structures of the martensitic phases could be nearly the same. Crystal structures of ternary Cu-Zn based martensites have been determined recently for alloys containing the three-valent elements gallium3, 4 and aluminm. The present studies have been made to examine the structures and morphology of the martensitic phase in ternary Cu-Zn based alloys containing a four-valent element, silicon. I) PROCEDURE Two alloys were prepared by melting and casting weighed quantities of the component high-purity metals in sealed quartz tubes under half an atmosphere of argon. They were subsequently remelted by levitation under a protective atmosphere of argon. After allowing for losses of zinc as determined by the difference in weight before and after casting, the compositions in atomic percent of both alloys were established to be Cu-33.5 Zn-1.8 Si and Cu-27 Zn-5.0 Si. These alloys were homogenized in the P-phase field for 2 days at 800" C. Bulk samples consisted of a martensite phase at room temperature, the M, temperature being approximately 30&apos; and 200" for the 1.8 and the 5 pct Si alloys, respectively. Thin disks were cut from the ingots using a spark machine, and they were heated for 5 min at 800&apos; and quenched into water in order to obtain martensite. These slices were thinned chemically at room temperature in a solution consisting of 40 parts HN03, 50 part H3PO4, and 10 parts HC1 and thinned further electrolytically by the Window technique, using a voltage of 15 to 25 v and a mixture of 1 part HN03 and 2 parts methanol, which was kept at a temperature near -30° c. Foils were examined by transmission electron microscopy using a Philips EM 200 electron microscope. 11) RESULTS AND DISCUSSION 1) Structure and Morphology. Fig. 1 shows the martensitic phase in the alloy containing 1.8 at. pct Si. This phase is composed of contiguous platelets, each containing striations. The direction of the striations changes at the boundary between individual platelets. These internal markings resemble the striations that are usually identified as stacking faults, as for example in Cu-A1 martensites6-a or the lamellar mixture of two close-packed phases in Cu-Zn-Ga marten-sites.3p &apos;9 lo In the present alloys, selected-area diffraction experiments have been obtained in order to determine the nature of the striations. Figs. 2(a), (61, and (c) are electron diffraction patterns of an area inside a single martensite plate. Fig. 2(a) contains diffraction spots which correspond to two close-packed structures with different stacking sequences, namely ABCBCACAB (orthorhombic) and ABC (fcc). Spots belonging only to the fcc structure are indicated by arrows. By tilting the foil either the orthorhombic structure, Fig. 2(b), or the cubic structure shown in Fig. 2(c) may be obtained. When the foil is oriented so that only the diffraction spots of the orthorhornbic structure are present, bright-field illumination shows small lamellae, as seen in Fig. 3. In this figure the lamellae that belong to the fcc structure are bright bands inside the dark extinction contours of the orthorhombic structure. The boundaries of the lamellae are parallel to the basal planes of the orthorhombic structure and to the {Ill} planes of the cubic structure, the close-packed directions of both structures being parallel. The 5 pct Si alloy shows similar features as those described for the 1.8 at. pct Si alloy.

Jan 1, 1969