Search Documents

By Franz Wever

ACCORDING to Tammann,1 the explanation of the effect of mechanical deformation in producing changes in the properties of metals is one of the most important problems of physical metallurgy, taking rank with the study of the constitution of alloy systems; and this problem has long attracted-the attention of practitioner and scientist alike. Its solution was not advanced materially until Tammann2 set up his translation hypothesis with its crystallographic basis, while other hypotheses, such as the amorphous metal hypothesis of Beilby3 and Rosenhain,4 have been shown by more intensive studies to be less and less satisfactory. The principles of the Tammann translation hypothesis have proved to be useful even up to today and in spite of all of the recent accumulation of experimental data, while the differences of opinion which have arisen relate to the extent to which the hypothesis accounts for the observed changes in properties and to what extent further assumptions are necessary. Stimulated by the proposals of Tammann, there soon developed a lively experimental activity which aimed at the elucidation of the structural or crystallographic changes produced by the mechanical deformation of metals. Parallel movements of crystal "blocks" along definite crystal slip planes had already been observed by lowing and Rosenhain5 in 1900, in metals which had been moderately deformed but without shedding light on the crystallographic nature of the processes accompanying more severe deformation. The solution of this important problem was not advanced until a much later date, or until the methods of X-ray crystal analysis had become available. Shortly after the discovery of the diffraction of X-ray by crystals, symmetrical diffraction effects were

Jan 1, 1931

By AIME AIME

FOLLOWING careful study of the relations of the Institute to students and the younger members of the profession, the Membership Committee recommended to the Board a change of plans abolishing the Junior Associate class of membership, substituting a -Junior membership and providing for Student Associates. The Board adopted this report at its meeting on Nov. 23, and asked Counsel to draft the necessary amendments to the By-laws, and gave formal notice of intentions to amend as provided in Section I, Article XI1 of the existing By-laws. The By-laws as it is proposed to amend Article I, 11, 111, IV, X, and XI follow. The new plan requires no changes in the other Articles. The matter will come before the Board for vote on Jan. 25.

Jan 1, 1929

By John Wulff

IN a previous paper Burwell and Wulff1 have shown by electron diffraction studies that allotropic transformations can be induced in 18-8 stainless steel by polishing to a depth of about 5 X 10-5 cm. The development of a successful etching technique, which removes accountable amounts of metal from the surface without pitting and without changing the root-mean-square profile as measured with an Abbot profilometer, led to the application of the whole technique and material to an investigation of various mechanical methods of surface preparation, such as grinding, lapping, superfinishing and cold-rolling. Ideally suited to such a study is 18-8 of low carbon and nitrogen content. The material can be heat-treated to produce a coarse-grained single-phase structure. On cold deformation there occurs not only a reduction in grain size but, at regions of maximum stress, a change of face-centered material to body-centered material, provided the metal is worked below about 200°C. When worked between 200° and 415°C., diffraction studies evidence a reduction in grain size without the appearance of any new body-centered ferrite. Ferrite, which can be referred also to strains induced by carbide precipitation, is evident when the material is worked at temperatures between 415° and 800°C. Stainless steel is advantageous because the usual surface-finishing operations do not readily oxidize it to any appreciable depth. In order to produce detectable oxide films on the surface of austenitic 18-8 in a time equivalent to that required to produce, for example, a fine ground finish on ½ sq. in., the sample must be held in a furnace or oxygen stream above 600°C. By using longer heating times, it is possible to achieve measurable oxide films on samples whose surface temperatures exceed only about 250°C. EXPERIMENTAL PROCEDURE The apparatus, material, and technique described in the previous paper1 were employed in this investigation. Samples of 18-8, 1 by 1 cm. by 4 mm., were carefully annealed in the austenitic range to produce a coarse-grained structure. They were then quenched and pickled to remove scale. On a lapping machine of the Graton2 type, both sides of each sample were polished to a flatness of 1/6 a wave length of sodium D light. Thereafter they were electrolytically etched to remove at least 1 X 10-3 cm. of the surface, a depth that is well below that of any deformations induced by surface preparation. Samples of this material, carefully mounted in steel holders, were then sent to various industrial organizations known for special finishing techniques. In the instrument shops at the Massachusetts Institute of Technology check samples were finished by the same methods, as far as they were available. Abbot profilometer3 readings were made on all the samples, which were then carefully degreased in double distilled benzine and alcohol, dried in a hot-filtered air blast, and kept in a desiccator. Suc-

Jan 1, 1941

By J. B. Clark

An exploratory study of the 60 wt pct Mg and 80 wt pct Mg sections of the solid constitution in the magnesium-rich region of the Mg-Al-Ca-Zn system was undertaken. The objective of the investigation was to determine the general configuration of the phase fields with respect to the magnesium solid solution in this complex system. The 335°C (635°F) tetrahedron was selected for study because the solid constitutions of the bounding ternary systems—Mg-Al-Zn,1 Mg-A1-Ca,2 Mg-Ca-zn3—were well known and, at least in these ternary systems, diffusion was rapid enough at 335°C for equilibrium to be reached fairly rapidly. Metallography and powder X-ray diffraction were selected as the best corroboratory methods for determining the solid phase equilibria. A total of forty-six quaternary alloys on the 60 wt Mg and 80 wt Mg sections were prepared, annealed to equilibrium at 335°C, and the phases present identified. Singly sublimed (99.99 pct) magnesium, electrolytic (99.99 pct) zinc, high-purity (99.99 pct) aluminum, and USP calcium were alloyed in graphite crucibles under a chloride flux and chill cast into a split graphite mold. Alloy samples were sealed under argon in Pyrex vials and annealed at 335°C ± 1/2° for a minimum of 500 hr. At the conclusion of the anneal, the alloy samples were quenched rapidly in ice water. Standard metallographic procedures for magnesium alloys were used. Powder X-ray diffraction patterns were taken on a G. E. Camera with a diameter of 14.32 cm using nickel filtered copper radiation. The phase equilibria in the 60 wt pct Mg section of the 335°C (635°F) tetrahedron is shown in Fig. 1. The complex equilibria in the zinc-rich region were not accurately determined and are shown only tentatively with dotted lines. The equilibria of the three bounding ternary 335°C sections from pure magnesium to 60 wt pct Mg are also shown as though folded away from the tetrahedron. The 80 wt pct Mg section has the same configuration of phase fields as that shown in Fig. 1. Thus it is reasonable to conclude that in higher magnesium sections, the same relative configuration of phase fields is maintained though the relative proportions of the individual phase fields may change slightly as the magnesium solid solution is approached. Note that all the ternary phases present in these ternary diagrams enter into the quaternary equilibria with the exception of the phase of the Mg-Al-Zn system which becomes unstable with the addition of as little as 1/2 pct Ca. No quaternary intermetallic phases were found. No liquid phase was detected in any of the quaternary alloys annealed at 335°C suggesting that if a quaternary eu-tectic exists, it must lie between 335°C and 339°C, the temperature of the ternary eutectic in the Mg-Al-Zn system.

Jan 1, 1962

By S. H. McFarlane, K. H. Zaininger, G. W. Cullen, C. C. Wang, G. E. Gottlieb

Heteroepitaxy of silicon on stoichiometric spinel has been studied. Both boron-doped (p-type) and arsenic-doped (n-type) single-crystal silicon films have been grown by the pyrolysis of silane on sioichiometric spinel (MgAl2O4) substrates prepared by a flux technique. The spinel crystals are free from strain and subgrains, and exhibit no thermal instability at temperatures employed for silicon deposition. The growth parameters of epitaxial silicon have been studied. Effects of substrate orientation, surface preparation, and growth conditions on the silicon Properties have been determined. The silicon-spinel composite was characterized by X-ray diffraction, electron diffraction, electron microscopy, and optical techniques. Information on epitaxial orientation relationship, defect structures and film-substrate interface has been obtained. A parallel orientation relationship was found between silicon and spinel. The silicon films exhibit no subgrain structures. However, growth pyramids, microtwins, stacking faults, and dislocations are the prevalent defects. The deformation of epitaxial silicon was measured by an X-ray technique. It was found that the epitaxial silicon is strained under compres-sive stress due to the thermal expansion difference between the film and substrate. The stress was estimated using the classical plate theory and beam equation. Electrical properties of the epitaxial silicon have been measured, including resistivity, carrier concentration, and Hall mobility. MIS and vertical through diffused junction structures have been fabricated wing silicon-spinel composite. Information on MIS characteristics, minority carrier life time, and junction properties has been obtained. THE achievement of single-crystal growth of large area silicon semiconductor films on oxide insulating substrates is of technical importance to many solid state electronic devices. The semiconductor-insulator composite structure is also of scientific interest because the heteroepitaxy is determined by the spatial relationship between the atomic arrangement in the substrate and that of the atoms in the appropriate crystallographic plane of silicon. The degree of crystalline perfection of the silicon deposits depends also on the physical condition of substrate surface. Epitaxial growth of silicon on commercial flame fusion Al-rich spinel (MgO:3.3A12O3) has been reported by several investigators.'-4 The lattice of spinel of this composition is distorted. The material cracks and exsolves the excess alumina in the lattice at temperatures (-1200°C) used in fabricating silicon devices. Stoichiometric MgA12O4 spinel exhibits neither lattice distortion nor thermal instability. Results are given on the epitaxial growth and characterization of silicon on stoichiometric spinel. EXPERIMENTAL Fabrication of Silicon-Spinel Composite Structures. The MgA12O4 spinel substrate wafers were prepared from bulk single crystals grown at about 1200°C by a flux technique5 using a PbF2 flux. The crystals are free from strain and subgrains, and exhibit a typical dislocation density of less than 50 lines per sq cm. The crystals are thermally stable without cracking and exsolution of alumina to at least 1500°C. The spinel crystals were oriented for cutting by the Laue X-ray back-reflection method.6 Substrate wafers (about 25 mil thick) of (Ill), (loo), and (110) orientations have been obtained bu cutting the X-ray oriented crystals using a standard type diamond wheel. An accuracy of better than 1/2 deg is maintained throughout the operation. The spinel substrate wafers were mechanically lapped and polished to produce the flat and smooth surface which is required for silicon epitaxy. Lapping was carried out with about 30-µ boron carbide abrasives to obtain a flat coplanar surface. The lapped surface was further polished using successively finer grades of alumina, ending with the 0.3-µ grade. After polishing the wafers generally have a flatness of ±0.4 µ per cm, as revealed by interferometry. Fig. 1 shows (111) oriented MgA12O4 spinel wafers of various shapes.

Jan 1, 1970

By J. Jay Jacobsen

A dynamic regional coal development model is constructed for the Eastern Powder River Basin of Wyoming. Using this model, alternative development schedules from a recent environmental impact statement submitted to the Department of the Interior are simulated (Ref. 1). These alternatives include different mixes of export capacity, different coal conversion techniques within the region, as well as various levels of coal production. Exportation of 70 to 80 percent of an ultimate coal production of 180 million tons (163.3 x l09 kg) per year and the careful phasing of additional public services with population growth effectively reduce the social and environmental impacts of coal development. The alternative involving the addition of 43,000 megawatts of electrical generation capacity has very significant adverse social and environmental impacts on the region.

Jan 1, 1977

By J. S. Marsh

TUESDAY, Feb. 16, was no day for strolling along the cold sidewalks of New York, and a large number of metallurgists sat down with pleasure to the warming task of wiping a few soldered joints. Presented by a joint-wiper of the modern school, G. M. Bouton, of the well-known team of Schumacher, Bouton, and Phipps, the initial paper brought into focus the theme of conservation of strategic metals and described the technique of making the fillet-type joint now employed by the Bell System. Using an over-all average of only 40 per cent of the solder formerly used by the conventional method. this important development bids fair to stick when the war is over. D. L. Martin and E. R. Parker then described the embrittling effect of hydrogen on silver previously heated in oxygen and the less serious but troublesome result obtained under the converse conditions. An interesting example of grain growth restriction created additional material for the lively discussion that ensued among those who have encountered one or another of these phenomena in silver and copper.

Jan 1, 1943

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

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

Jan 1, 1958

By L. M. Clarebrough, A. K. Head, G. W. West, M. E. Hargreaves

RECENTLY Welber and Webelerl reported that during the annealing of fatigued copper no energy was released, but that energy was absorbed in the range of temperature 250" to 400°C. In view of the fact that strain hardening occurs during the fatigue of copper, this result was surprising and it seemed desirable to check the measurements. This note describes measurements made by a different technique which indicates that energy is stored during the fatigue of copper. Two test bars with gage length ¾ in. in diameter and 6 in. long were machined from OFHC copper and annealed in vacuum for 1 hr at 600°C. These were fatigued to fracture in an Avery pulsator at a frequency of 2000 cycles per min. The first specimen fractured after 0.25x10 cycles under a push-pull

Jan 1, 1956

By J. B. Hess, C. S. Barrett

TO reach equilibrium between different phases in cobalt-rich alloys requires prohibitively long annealing cobalt-richalloystimes when temperatures are below about 700°C. The fact that a transformation from face-centered cubic to close-packed hexagonal readily tered takes place at temperatures below this in the cobalt-rich solid solutions is not an indication that thermally activated processes occur at an appreciable rate, for the transformation is well established as martensitic in nature. Wide divergence between heating and cooling experiments and high sensitivity to prior heat treatment make it difficult to judge temperatures of equilibrium between the phases.&apos; One object of the present work was to see if the information object of on the relative stability of phases could be gained by substituting plastic deformation for thermal agitation. Procedures were worked out that led to the determination of a diffusionless type of phase diagram, which represents the temperature of of phase equal stability for phases of the same composition, and the technique was applied to the Co-Ni system. Another object of the work was to see whether or not deformation would generate frequent stacking faults when these were thin lamellae of quentstackingfaultsa phase having higher free energy than the parent phase. The alloys were prepared in 80 to 100 g melts from cobalt (with metallic impurities estimated spectrochemically as follows: Ni, 0.05 pct; Fe, 0.001 pct.; Mg, Si, Cu, Cr, Al, < 0.001 pct) and Mond Car-bony1 nickel (with Fe, 0.05 pct; Si, 0.003 pct; C, 0.61 pct.; Cu, 0.001 pct; Co, Cr not detected, < 0.01 pct). The metals were melted in pure Al2O3 crucibles. An atmosphere of argon, that had been purified by passing over hot magnesium chips, was used for the alloys that, by analysis of the portions of the ingots actually used, were found to contain 15.3, 25.7, and 35.0 pct Ni, and vacuum melting (after degassing) was used for those containing 29.4 and 31.5 pct Ni. After induction melting the alloys were allowed to solidify in the crucible, and slices % in. thick x ½ in. in diam were annealed 12 hr at 1350°C for homogenization. These same specimens were used throughout the series of experiments, with annealing treatments of 4 hr at 900°C in purified hydrogen followed by furnace cooling, alternating with the deformation and X-ray tests discussed below. Results Spontaneous transformation was observed on cooling to room temperature in all alloys containing 29.4 pct Ni or less and by cooling the 31.5 pct alloy to — 195°C but was not observed in the 35 pct alloys after cooling to —195°C. These results are in satisfactory agreement with the cooling experiments of Masimoto.4 From these data it is clear that the temperature of beginning transformation M,,, drops to 20°C with the addition of about 30 pct Ni. The test for spontaneous transformation was metallographic. Specimens were thermally polished by annealing 10 hr in hydrogen at 1350°C, then furnace cooled; if trans- formation had occurred there were relief effects visible on the thermally polished surfaces. These markings were narrow straight lines, usually resolvable at high magnification as clusters of fine lines that resembled slip lines. It was concluded that they resulted from displacements on (111) planes, for the number of directions in individual grains often reached but never exceeded four, and lines could always be found parallel to the thermally etched (111) boundaries of annealing twins. The markings were thus consistent with the idea that the transformation occurs by (111) plane displacements (Shockley partial dislocations moving on (111) planes). This was further confirmed by X-ray tests for stacking disorders. Using an oscillating crystal technique previously employed to detect strain-induced faulting in Cu-Si alloys," streaks indicative of the stacking faults were looked for and found on X-ray films of the spontaneously transformed 25.7 pct Ni alloys, as expected by analogy with Edwards and Lipson&apos;s results on pure cobalt." The streaks were much intensified after rolling at room temperature. Transformation induced by plastic strain was investigated as a function of alloy composition and temperature of deformation. A series of tests was made to determine suitable straining and X-raying techniques. Filing was found inferior to abrasion in converting cubic samples to hexagonal, and abrasion was less effective than peening in producing smooth unspotty Debye rings in the X-ray patterns. Because the diffraction lines were broad, Geiger-counter spectrometer records of filings were less sensitive in revealing small amounts of transformed material than X-ray patterns recorded on films in a small diameter camera. After these exploratory tests the following methods were adopted. Specimens that had been annealed at least 4 hr at 900°C and furnace cooled were mounted in a block of aluminum, brought to temperature, and peened thoroughly with a mullite pestle preheated to the same temperature. The specimens were then quenched to room temperature. In peening, a circular area of % in. diam was given 500 blows. A few control tests showed that an additional 1000 blows did not detectably change the proportions of the phases present. The amount of transformation was judged by X-ray reflection patterns from the peened surface, using the innermost four lines of the cubic and the hexagonal patterns with filtered CoKa radiation,

Jan 1, 1953

By Frank S. Gardner, Morris Cohen, Dara P. Anita

There is a conspicuous lack of information in the literature on the precise role played by residual quantities of austenite in heat-treated steels. While retained austenite may be expected to have significant effects on such important properties as the impact resistance of tools and carburized parts and the dimensional stability of dies and gauges, attempts to study these problems systematically have suffered from the absence of a reliable technique for ascertaining absolute amounts of austenite. With such a technique, not only could the relation between residual austenite and service behavior be investigated, but the chemical and heat-treatment factors that control the quantity of the austenite could also be established. Thus, the retained austenite content could then be regulated in accordance with the results desired. The presence of retained austenite may be inferred by observing the changes in properties (hardness, specific volume, electrical resistance, etc.) due to its decomposition on subatmospheric cooling1 or on tempering,2 but these indirect measurements are not readily translated into percentages of austenite. Quantitative determinations have been achieved in special cases by means of dilatometric3 and magnetic4,5 measurements; but the former procedure requires that observations be conducted during the hardening and involves difficult calibrations that limit its applicability, while the magnetic procedure is very sensitive to extraneous influences and depends upon assumptions that can only be considered as approximate in an absolute sense. Furthermore, both the dilatometric and magnetic effects are volume properties, and cannot be conveniently utilized to explore variations in retained austenite from point to point in a suecimen. Some microstructures lend themselves to accurate evaluation of retained austenite contents by metallo-graphic methods,3 but such instances are not too common, and at best, the procedure is tedious. The characteristic X-ray diffraction lines of austenite permit positive identification of its presence; and in the present paper the intensities of these lines, or the corresponding densities* on photographic film, are employed to measure the amount of the retained austenite. In order to cancel the effect of uncontrollable variations in the X - ray exposure and film - development conditions, a standard reference line is Superimposed on each film by maintaining a foil of aluminum in the path of the incident X-ray beam during the entire exposure. With different samples of steel and the same foil, the ratio of the density of some one austenite line to the density of

Jan 1, 1943

By Morris Cohen, Dara P. Anita, Frank S. Gardner

There is a conspicuous lack of information in the literature on the precise role played by residual quantities of austenite in heat-treated steels. While retained austenite may be expected to have significant effects on such important properties as the impact resistance of tools and carburized parts and the dimensional stability of dies and gauges, attempts to study these problems systematically have suffered from the absence of a reliable technique for ascertaining absolute amounts of austenite. With such a technique, not only could the relation between residual austenite and service behavior be investigated, but the chemical and heat-treatment factors that control the quantity of the austenite could also be established. Thus, the retained austenite content could then be regulated in accordance with the results desired. The presence of retained austenite may be inferred by observing the changes in properties (hardness, specific volume, electrical resistance, etc.) due to its decomposition on subatmospheric cooling1 or on tempering,2 but these indirect measurements are not readily translated into percentages of austenite. Quantitative determinations have been achieved in special cases by means of dilatometric3 and magnetic4,5 measurements; but the former procedure requires that observations be conducted during the hardening and involves difficult calibrations that limit its applicability, while the magnetic procedure is very sensitive to extraneous influences and depends upon assumptions that can only be considered as approximate in an absolute sense. Furthermore, both the dilatometric and magnetic effects are volume properties, and cannot be conveniently utilized to explore variations in retained austenite from point to point in a suecimen. Some microstructures lend themselves to accurate evaluation of retained austenite contents by metallo-graphic methods,3 but such instances are not too common, and at best, the procedure is tedious. The characteristic X-ray diffraction lines of austenite permit positive identification of its presence; and in the present paper the intensities of these lines, or the corresponding densities* on photographic film, are employed to measure the amount of the retained austenite. In order to cancel the effect of uncontrollable variations in the X - ray exposure and film - development conditions, a standard reference line is Superimposed on each film by maintaining a foil of aluminum in the path of the incident X-ray beam during the entire exposure. With different samples of steel and the same foil, the ratio of the density of some one austenite line to the density of

Jan 1, 1943

By Dara P. Antia, Morris Cohen, Frank S. Gardner

THERE is a conspicuous lack of information in the literature on the precise role played by residual quantities of austenite in heat-treated steels. While retained austenite may be expected to have significant effects on such important properties as the impact resistance of tools and carburized parts and the dimensional stability of dies and gauges, attempts to study these problems systematically have suffered from the absence of a reliable technique for ascertaining absolute amounts of austenite. With such a technique, not only could the relation between residual austenite and service behavior be investigated, but the chemical and heat-treatment factors that control the quantity of the austenite could also be established. Thus, the retained austenite content could then be regulated in accordance with the results desired. The presence of retained austenite may be inferred by observing the changes in properties (hardness, specific volume, electrical resistance, etc.) due to its decomposition on subatmospheric cooling1 or on tempering,2 but these indirect measurements are not readily translated into percentages of austenite. Quantitative determinations have been achieved in special cases by means of dilatometric3 and magnetic4,5 measurements; but the former procedure requires that observations be conducted during the hardening and involves difficult calibrations that limit its applicability, while the magnetic procedure is very sensitive to extraneous influences and depends upon assumptions that can only be considered as approximate in an absolute sense. Furthermore, both the dilatometric and magnetic effects are volume properties, and cannot be conveniently utilized to explore variations in retained austenite from point to point in a specimen. Some microstructures lend themselves to accurate evaluation of retained austenite contents by metallographic methods,3 but such instances are not too common, and at best, the procedure is tedious. The characteristic X-ray diffraction lines of austenite permit positive identification of its presence; and in the present paper the intensities of these lines, or the corresponding densities* on photographic film, are employed to measure the amount of the retained austenite. In order to cancel the effect of uncontrollable variations in the X-ray exposure and film-development conditions, a standard reference line is superimposed on each film by maintaining a foil of aluminum in the path of the incident X-ray beam during the entire exposure. With different samples of steel and the same foil, the ratio of the density of some one austenite line to the density of

Jan 1, 1943

By B. D. Cullity

GOLD and beryllium form an intermediate phase composed of the two metals in equal atomic proportions and having the formula AuBe. According to Winkler,1 this phase probably exists in two modifications: beta, stable below about 600°C, and alpha, stable between 600°C and the melting point, about 740°C. Only the low- temperature beta form will be considered in this paper. EXPERIMENTAL PROCEDURE The gold used had a fineness of 999.75 to 999.85, balance mainly silver, and the beryllium purity was better than 99.8 pct. AuBe was prepared by melting the constituents in a beryllia crucible in an evacuated induction furnace. After melting and thorough mixing, the alloy was allowed to solidify in the crucible. No difficulty was encountered in obtaining a homogeneous ingot. Both chemical analysis and microscopic examination of the ingot showed that the alloy was essentially one phase, containing 50 at. pct gold. The alloy was quite brittle and powder samples could easily be pre- pared by grinding in an agate mortar. The X-ray diffraction patterns were made with CuK-alpha radiation in a Debye-Scherrer powder camera 57.3 mm in diameter. The film was placed unsymmetrically in the camera in order to afford a basis for am-shrinkage corrections. A sample homogenized at 5o0°C gave the same diffraction pattern as a sample taken from the as-melted ingot. GENERAL RESULTS The diffraction pattern of AuBe was readily indexed on the basis of a simple cubic lattice with ao = 4.659 ± 0.001kX. If the unit cell is assumed to contain four AuBe "molecules," the calculated X-ray density is 13.46 grams per cc as compared with the measured density of 13.55 gm per cc. The only missing reflections in the dsraction pattern are (100) and (220) (see Table I). Since these missing reflections are not those characteristic of body or face centering, the lattice of AuBe must be simple cubic. To locate the positions of the atoms within the unit cell, two possibilities had to be considered: I. The structure was disordered and there were eight positions to be filled by an "average" gold-beryllium atom. That the structure was disordered seemed unlikely since the lattice parameter did not vary with composition in alloys containing some- what more and somewhat less than 50 at. pct gold, indicating a fixed composition for AuBe.

Jan 1, 1947

By A. Hellawell

Specitlrens of the Al-Ge eutectic alloy have been frozen unidivectionally at rates between 2.5 x 10-6 and 2.5 x 10-4 cm per sec and the structure examined by optical and X-ray methods. There is no epitaxial relationship between phases, the aluminum having random orientation and the germanium a preferred (011) fiber textuve. Lamellar colonies which are BINARY eutectic alloys occur between either silicon or germanium with the metals aluminum or silver. common in this alloy are constructed from axial and nonaxial (111) plates of germanium which are related by a variety of twin configurations. Irregular or globular regions of the microstructure are composed of continuous single crystals of each phase, the germanium being heavily twinned. There is limited solid solubility in these systems, and the eutectic phases all involve diamond cubic with fcc crystal structures. In the microstructures of these eutectic mixtures the silicon and germanium crystals exhibit an almost infinite variety of shapes which are notably sensitive to

Jan 1, 1968

By W. V. Kotlensky, H. E. Martens

In an earlier communication, Ref. 1, the authors presented the tensile properties and the changes in crystal structure and microstructure for pyrolytic graphite tested at 2750°C. It was suggested that changes in the structure may have an effect on the tensile properties of this material. Accordingly, tensile tests were run on a series of specimens, from one block of pyrolytic graphite, some of which were hot-worked by being strained at 2750°C, others of which were tested in the as-deposited condition. According to the manufacturer, General Electric Co., the polycrystalline material was deposited at 2100°C on a substrate of synthetic graphite by decomposition of a dilute natural gas mixture. The as-deposited material had a density of approximately 2.19 g per cc, and as shown in Fig. 1 had a structure of medium size growth cones which were regenera-tively nucleated. All specimens had a gage section 0.75 in. long by 0.06 in. wide by 0.1 in. thick with the thickness direction perpendicular to the basal planes. The testing method and equipment used have been previously described, Ref. 2 and 3. For both the hot-working and the testing the load was applied parallel to the basal planes; a cross-head speed of 1.5 x l04 in, per sec was used. All heating was done in an atmosphere of bottled helium.

Jan 1, 1962

By C. E. Birchenall, W. Batz, H. W. Mean

AT temperatures between 1095&apos; and 1347ºC, 13 runs have been made on the diffusion of silicon in iron. In two of the runs the couple compositions were entirely within the loop of the Fe-Si system; the base alloys contained 0.0 and 1.0 wt pct Si. The other runs in which the couples consisted of a 2.3 wt pct Si alloy welded to a 3.7 pct Si alloy were a phase throughout. The alloys were made by melting electrolytic iron and commercially pure silicon. Trace impurities were not determined. The butt welded couples were diffused in an inert atmosphere of argon or hydrogen. After cooling, cuts of two mils or greater thickness were machined parallel to the weld interface. The chips were analyzed for silicon. When the concentration and distance data were examined on the conventional probability plot,&apos; no marked variation of the diffusion coefficient with concentration was indicated over the narrow composition ranges employed. Therefore, a single diffusion coefficient is recorded for each run in Table I. The temperatures and atmospheres of the diffusion anneal are listed along with the compositions of the base alloys. For a iron the silicon diffusion coefficient is given by the equation: D = 0.44 e-48,000/RT where R is the gas Constant and T, the absolute temperature. However, since the scatter in the data is fairly large, the activation energy may be in error by as much as 6000 cal per g-atom. The two ? iron points do not permit estimation of the activation energy with any reasonable certainty. They do indicate that the coefficients reported by Smithells2 and Jost,3 based on the work of Fry,4 are much too high. Although very dilute solutions in iron of manganese,5 nickel,8 cobalt,7 and molybdenum8 give dif- fusion coefficients quite close to those obtained for self-diffusion in iron, the silicon values are considerably higher, though of the same order of magnitude. This seems to be consistent with the fact that the silicon atom is the only one of those listed here which is appreciably smaller than iron. The authors are grateful to the Office of Naval Research for their support of this work under Contract N6ori-47, Task order IV, Project NR 031-184, to J. K. Stanley and the Westinghouse Research Laboratories for the silicon alloys used, to several steel companies for the silicon analyses, and to C. Wells, of the Metals Research Laboratory, Carnegie Institute of Technology, for numerous suggestions during the course of the work. References &apos;C. Wells: Atom Movements (1951) Chapter 2. A.S.M. 2C. J. Smithells: Metals Reference Book (1949) p. 405. Interscience. Pub. Co. 3W. Jost: Diffusion (1952) p. 223. Academic Press. 4 A. Fry: Stahl und Eisen (1923) 43, p. 1039. T. Wells and R. F. Mehl: Trans. AIME (1941) 145, p. 315. "C. Wells and R. F. Mehl: Trans. AIME (1941) 145, p. 329. 7M. F. Hawkes and R. F. Mehl: Trans. AIME (1947) 172, p. 467; Metals Technology (August 1947). .J. L. Ham: Trans. A.S.M. (1945) 35, p. 331.

Jan 1, 1953

By C. E. Morris, S. R. Pollack

Current -vo1tage -temperature characteristics were studied for Al-A12O3-Al, Au structures. The oxide film was grown by gaseous oxidation in an 0, glow discharge. The electron-transfer mechanism was identified as tunneling and the barrier heights and thickness were determined. It was found that the barrier height at the parent aluminum-oxide interface is 1.5 ev and the built-in vloltage with an aluminum counter electrode is 0.35 v. The growth mechanism of the oxide is also discussed and it is suggested that Mott&apos;s theory is not applicable in describing the growth. Discrepancies were observed in the detailed comparison of tunneling theory, based on a trapezoidal model, with the data, and several possible explanations are discussed. THEORETICAL analyses of electron tunneling from one nonsuperconducting metal to another through an extremely thin insulating film have been presented.1-6 These calculations relate the current density, J, to the voltage, V, between the two metals, and to the temperature, T. The results of these calculations indicate that the magnitude of J and the detailed shape of the J-V characteristic will in general depend most strongly upon such properties of the insulating film as the thickness, the dielectric constant, and the structure of the electron energy barrier profile. The experimental results of many7-11 workers have corroborated the main features of these calcu- lations and have in fact been used to determine properties of the thin insulating film. It has been demonstrated, for example, that the tunneling current formulation of simmons4 is adequate to describe the observed J-V characteristic over approximately 10 orders of magnitude of current. Furthermore, from these observations and analyses, insight into the nature of the A1-A12O3 (thermally grown) interface region has been obtained.&apos;&apos; The temperature dependence of the tunnel current has also been studied and, although a self-consistent set of tunneling parameters can be chosen to describe these data at low voltages (i.e., <0.5 v), the tunneling parameters are different from those obtained from higher voltage (i.e., of the order of 1 to 5 v) measurements." We have measured the effect of temperature and voltage upon the tunnel current at higher applied voltages and find that the theory is inadequate to describe all of the effects reported here. A discussion of the origin of this inadequacy is presented following a description of the samples used for these experiments, and the experimental results. SAMPLE PREPARATION Metal-insulator-metal structures were fabricated in the following way. A 99.999 pct A1 charge was used to deposit, in vacuo, thirty films, 2000Å thick, onto a 1 by 2 in. glass substrate (7059 Corning glass). Prior to deposition the substrate was glow-discharged for final cleanup and then baked at 200°C for 2 hr at a pressure of 5 x 10-7 torr. The pressure during deposition of the metal films was 2 X 10-6 torr and the deposition rate was 50 to 100Å per

Jan 1, 1965

By Subhas G. Malghan

Feldspathic deposits occur widely throughout the United States, but North Carolina, California, Connecticut, and South Carolina accounted for over 80% of the total domestic feldspar output for the year 1973.1 Pegmatites and granites constitute the major feldspar reserves of the United States, 2 and in addition, feldspar is produced as a byproduct by firms whose major products are spodumene and mica. 3 Feldspar flotation is practiced in the United States, Mexico, Finland, Norway, West Germany, Japan, and the USSR. According to the US Bureau of Mines estimates, the production of feldspar in the United States and rest of the world were 704,000 and 2,514,000 t, respectively. Feldspar is principally used as a flux in making glass, pottery, porcelain, enamel, tile, and other ceramic products. In recent years, the domestic feldspar industry is faced with a number of problems. As a result of increased cost of energy and the introduction in 1972 of new legislative programs relating to air, water, and noise pollution, land-use restrictions, and mined-land rehabilitation, the production costs have increased. Apart from the increased cost of operation, an operational problem exists with the feldspar producers in North Carolina, especially those in the Spruce Pine area. This problem is concerned with the use of hydrofluoric acid in the feldspar flotation. Feldspar producers in Spruce Pine, NC, have been discharging process waste water into the North Toe River. The mill waste water contains active fluoride ions. Fluoride in excessive concentrations is undesirable in waters used for drinking. It is stated that water containing 0.9-1.0 ppm fluoride will seldom cause mottled enamel on children&apos;s teeth; and for adults, concentrations less than 3-4 are not likely to cause endemic cumulative fluorosis and skeletal effect. Although the literature on this subject is rather confusing and inconclusive, the inference that concentrations over 4 ppm may affect bone structure is clear. According to the recent Federal Register,4 maximum fluoride level of 1.4 ppm at 79°-98°F is considered to be adequate and safe for the protection of health of the consumers. The EPA and state environmental agencies have accelerated their drive to reduce water pollution on a faster schedule. By 1977, the EPA specifications for maximum contaminant level of fluoride ions in the discharge waters of feldspar milling operatins is expected to be reduced to 2.0 ppm. The other problems of using hydrofluoric acid are the following: toxicity, hazards of handling and storage, and high cost as compared to other inorganic acids (almost 16 times the cost of sulfuric acid). In order to reduce fluoride levels in mill discharge waters, mining companies have taken the following steps: I) Recirculating a part of their mill water. Even though recirculation of mill water seems to be a novel method of reducing fluoride contamination of the discharge water, there are certain operational and handling problems. 2) Conducting research on the treatment of fluorides in mill waste water. The technology of treatment of fluoride ions has received considerable interest in the recent years. A recent research report5 estimates that the cost of fluoride ion removal to meet the present specifications in the feldspar industry is approximately $0.25/t of ore processed, and about $0.50/t of feldspar produced. At the request of the feldspar producing industries in North Carolina, the North Carolina State University (NCSU) Minerals Research Laboratory has taken up a research program directed towards overcoming the fluoride ion pollution problem. After a close study of the operational, technical, and economic aspects of feldspar flotation, it was decided to attempt to replace the conventional hydrofluoric acid process. Conventional Feldspar Flotatin Using Hydrofluoric Acid Since the inception of the feldspar flotation process using hydrofluoric acid by O&apos;Meara2,6 the process has achieved a great commercial success. In the conventional flotation separation of feldspar-quartz, hydrofluoric acid is used to suppress quartz and activate feldspar, and a long chain amine salt (acetate or chloride) is used as a collector. The bulk of amine collectors used in current feldspar operations are applied as the water-soluble acetates of the free-base amines. These products are pastes or waxy solids which are available in a range of acetic acid neutralization levels generally 50 to 100% neutralized. In spite of the problems mentioned in connection with the use of hydrofluoric acid, this process is extremely stable with respect to changes in the process variables. With the exception of a few operations, alaskite and pegmatite are the major sources of feldspar.7 In the flotation treatment of a pegmatite that contains iron-bearing minerals (heavy minerals), mica, feldspar, and silica, a logical order of removal presents itself considering the following:8 1) Mica is readily floated by an amine collector in a pulp pH 3.5. Some iron-bearing minerals will usually respond to amine collector in acid circuit with the mica concentrate. 2) Since iron minerals tend to occur invariably in the feldspar concentrate, it is desirable to remove most of these prior to feldspar flotation. A fatty acid or a petroleum sulfonate collector used in this flotation step in acid circuit will float iron-bearing minerals. 3) Using hydrofluoric acid to maintain pH of 2.5, an amine collector employed in a final step will float feldspar away from silica, usually leaving the latter in the tailing as a high-grade silica concentrate. The problems connected with the flotation separation of feldspar-quartz arise due to the similarities in their chemical structure. Therefore, any reagent system that is likely to succeed in feldspar-quartz separation should have adsorption affinity towards one of the minerals and depression effect towards the other mineral.

Jan 1, 1979

By P. Schwarzkopf, J. H. Brophy, J. Wulff

A constitutional diagram has been proposed for the tantalum-rhenium alloy system. Rhenium dissolved in tantalum up to 48 wt pct, and the maximum solubility of tantalum in rhenium is 5 wt pct. Intermediate x and s phases were found. X-ray diffraction, metallography and melting points were employed. SEVERAL investigators have described the phases present in the tantalum-rhenium alloy system, but no detailed account of the phase diagram prior to the present investigation appears to be available. Greenfield and Beck&apos; reported the solubility of 48 to 54 at. pct Re in tantalum, a s phase at 41 at. pct Ta, and x phase isomorphous with a Mn from 37 at. pct Ta to less than 25 at. pct. They employed as-arc melted specimens and heat treatments at 1200 °C lasting 72 hr.2 Duwez3 reported the existence of a a phase at the composition Re3Ta2. Niemiec and Trzebiatowski4 observed a lattice parameter a = 9.69A, for the x phase at a composition Ta7Re22, but no s phase. Savitiski and Tylkina5 have shown a hardness maximum at the composition 40 at, pct Ta and a somewhat lower plateau from 35 to 10 at. pct. Knapton6 indicated results similar to those of Greenfield and Beck.&apos; The present investigation describes the phase relationships in the tantalum-rhenium alloy system determined by melting point measurements, X-ray diffraction and fluorescence, and metallography. EXPERIMENTAL PROCEDURE Commercial 99.7 pct Ta powder from Fansteel Metallurgical Corp. and 99.9 pct Re powder from Chase Brass and Copper Co. were used for alloy preparation. The powders were weighed to desired nominal compositions and then pressed without binder into compacts weighing 5 or 10 g. The compacts were arc-melted six times on alternate sides on a water-cooled copper hearth using a nonconsumable tungsten electrode in an atmosphere of titanium gettered helium, at a pressure of 500 mm Hg. In most cases this procedure yielded alloy buttons of satisfactory homogeneity. A series of alloy specimens were analyzed wet chemically for use as standards for X-ray fluorescence. All specimens were analyzed by fluorescence and the results showed that the compositions differed by less than 3 pct Re from the original as-weighed nominal composition.* On the basis of self-

Jan 1, 1961