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By Edward Capillon

THE problem of scrap is probably of greater importance inn the production of gold, silver and other precious metal alloys than is the case for base metals and alloys. Remelting of gold and silver scrap in the shop is always a costly process because it involves losses by oxidation of the base metals in the alloy with a consequent increase in the percentage of precious metal. This is most marked in the case of alloys containing the low-boiling and easily oxidized metals zinc and cadmium. Since it is. not generally feasible to assay every shop remelt it follows that the possibilities of lost values are large. So-called rolled gold and silver plate is made by soldering or welding the precious metal alloys onto base, metal. Such plate when defective must be sent to the refinery to recover the gold and silver values, thereby involving additional expense in the form of refining charges. It is obvious therefore that gold and silver alloy scrap is an important item in manufacturing cost and must be reduced to a minimum. The amount of scrap resulting from poor metal will depend on a number of factors in the manufacturing operations, not least among which is the melting and casting practice. The notes which follow are a summary of experiments performed at various times to determine what variables in melting and casting are influential in the production of sound alloys.

Jan 1, 1930

By L. J. Health

Synthetic rock with predictable porosity and permeability has been Prepared from mixtures of sand, cement and water. Three series of mixes were investigated primarily for the relation between porosity and permeability for certain grain sizes and proportions. Synthetic rock prepared of 65 per cent large grains, 27 per cent small grains and 8 per cent Portland cement, gave measurable results ranging in porosity from 22.5 to 40 per cent and in permeability from 0.1 darcies to 6 darcies. This variation in porosity and permeability was caused by varying the amount of blending water. Drainage-cycle relative permeability characteristics of the synthetic rock were similar to those of natural reservoir rock. INTRODUCTION The fundamental behavior characteristics of fluids flowing through porous media have been described in the literature. Practical application of these flow characteristics to field conditions is too complicated except where assumptions are overly simplified. The use of dimensionally scaled models to simulate oil reservoirs has been described in the literature. 1-3 These and other papers have presented the theoretical and experimental justification for model design. Others have presented elements of model construction and their operation. In most investigations the porous media have consisted of either u ncon soli da ted sand, glass beads, broken glass or plastic-impregnated granular substances—materials in which the flow behavior is not identical to that in natural reservoir rock. The relative permeability curves for unconsoli-dated sands differ from those for consolidated sandstone. The effect of saturation history on relative permeability measurements is discussed by Geffen, et a1.4 Wyga15 has shown quite conclusively that a process of artificial cementation can be used to render un consolidated packs into synthetic sandstones having properties similar to those of natural rock. Many theoretical and experimental studies have been made in attempts to determine the structure and properties of unconsolidated sand, the most notable being by Naar and Wygal.6 Others have theorized and experimented with the fundamental characteristics of reservoir rocks. This study was conducted to determine if some general relationship could be established between the size of sand grains and the porosity and permeability in consolidated binary packs. This paper presents the results obtained by changing some of the factors which affect the porosity and permeability of synthetically prepared sandstone. In addition, drainage relative permeability curves are presented. EXPERIMENTAL PROCEDURE Mixtures of Portland cement with water and aggregate generally are designed to have certain characteristics, but essentially all are planned to be impervious to water or other liquids. Synthetic sandstone simulating oil reservoir rock, however, must be designed to have a given permeability (sometimes several darcies), a porosity which is primarily the effective porosity but quantitatively similar to natural rock, and other characteristics comparable to reservoir rock, such as wettability, pore geometry, tortuosity, etc. Unconsolidated ternary mixtures of spheres gave both a theoretically computed and an experimentally observed minimum porosity of about 25 per cent.7 By using a particle-distribution system, one-size particle packs had reproducible porosities in the reproducible range of 35 to 37 per cent.6 For model reservoir studies of the prototype system, a synthetic rock having a porosity of 25 per cent or less and a permeability of 2 darcies was required. The rock had to be uniform and competent enough to handle. Synthetic sandstone cores were prepared utilizing the technique developed by Wygal.5 Some slight variations in the procedure were incorporated. The sand was sieved through U. S. Standard sieves. A 18-20 sand denotes that the sand passed the Number

Jan 1, 1966

Elected Died 1903 * ADAMS, CHARLES C. 1905 1884 *ADDY, MATTHEW 1896 1894 *ALLFN R B 1896 1874 *AMIOT, H 1892 1886 *AMSLER, CARL 1894 1895 *ÅNGSTROM, CARL 1901 1895 *ARMSTRONG, JOHN F 1898 1882 *ARNOLDS, HUGO 1886 1875 *ASHBURNER, CHARLES A 1889 1872 *ASIIBURNER, WILLIAM 1887 1883 *ATKINS, C M , JR 1885 1897 *AYERS, WILLIAM 1898 1885 *BABCOCK, GEO H 1893 1884 *BAILEY, EDWARD 1889 1880 *BAILEY, JACKSON 1887 1900 *BALLOU, FRANKLIN 1903 1886 *BARNES, F W 1892

Jan 1, 1910

By R. B. Booth, W. F. Linke

The continuous interest of the American Cyanamid Company in producing superior polymeric flocculants and dispersants for the mining industry has resulted in a broad, general study of the physical chemistry of mineral-polymer systems. The aim of this program has been to establish a sound theoretical basis on which practical problems could be analyzed, and which would lead to the development of new and improved flocculating and dispersing agents. This study has required the cooperative effort of physical, analytical, and polymer chemists, as well as engineers familiar with mining problems. This report summarizes the results of some of our investigations over the past two years. Further studies along these and other lines are in progress and will be reported in the near future. MEASURING FLOCCULATION IN THE LABORATORY The foremost problem in studying flocculation in the laboratory has been to establish reproducible methods of comparing and evaluating the effectiveness of various reagents. Previous workers have measured settling -rates 1,8 filtration rates2 , and sediment volumes3 . Direct observations of the floc size, or the clarity of the supernatant liquid, can also be used. AIthough these parameters are all interrelated, they do not always measure the same physical properties of the suspensions, and hence are not equally useful or reliable. Whatever the method of comparison selected. the testing procedure must be carefully defined and standardized. The results must be satisfactorily reproducible, and for practical purposes must accurately reflect the results obtained in mill use. In order to compare the data obtained in these various types of test, the physical nature of the flocculated system must be examined in some detail. In an unflocculated system, only the larger or denser particles (the "sands") settle at a useful rate. The sediment can be observed to build up from the bottom of the cylinder, while the fines remain in suspension for a long period of time. If the system is not disturbed, even the microscopic fines can be seen to classify themselves as they fall over a period of days. When a high molecular weight polymer is added to the system, the colloidal particles are tied together randomly in flocs, and the sands and fines settle together. The line of demarkation between solid and liquid phases moves downward from the top of the cylinder. The settling rate of the flocs depends on their size and on their effective density. For a given mineral sample, the larger the flocs, the faster the settling. Since the large flocs cannot pack as closely as small ones, they produce a sediment with more pore spaces, and hence of larger volume, which is easier to pump and to agitate. Although it is nearly impossible to measure individual floc sizes, it is relatively easy to determine settling rates and sediment volumes. Of these two, the settling rate is simpIer to measure, and hence generally more practical. Reproducible sediment volumes can only be obtained by allowing the solids to pack for a rather long period of time (e.g., hours to days), and although the volumes thus observed are directly related to the degree of flocculation (average floc size), it is often impractical to wait so long for the results.

Jan 1, 1961

By AIME AIME

AS a new departure the annual business meeting was held at 4 p. m. on Tuesday, Feb. 16, instead of in the morning, as previously. The retiring President, Robert E. Tally, called the meeting to order and briefly spoke of the large measure of success that had been attained in balancing the budget of the Institute in 1931, so that, although receipts had declined over $26,000 compared to the previous year, expenditures had come within $3,000 of income. He referred in complimentary ,terms to the work of the committees on Membership, Admissions, Papers and Publications, and MINING AND METALLURGY, from which more would be heard late:. He also announced that a large and important committee on economics has been under consideration, and will be announced later. As an evidence of growth it was noted that a new Division, Mineral Industry Education, had been organized just an hour previously.

Jan 1, 1932

By Amitava Gangulee, Michael B. Bever

The order-disorder transition in Ag-Mg alloys in the range 17 to 26 at. pct Mg was investigated and some thermodynamic, electrical and mechanical properties of ordered Ag-Mg alloys were measured. A modification of the phase diagram is proposed on the basis of measured transition temperatures. The stability of the ordered structure is analyzed in terms of the quasichemical theory. Kinetic aspects of the order-disorder transition were also investigated. The energies of ordering at 273°K of Ag-Mg alloys were measured by liquid metal solution calorimetry. The electrical resistivities and the tensile Properties of the ordered alloys were measured. The exothermic energy of ordering increased with magnesium concentration up to the composition Ag3Mg; it is discussed in terms of the quasichemical theory. Pronounced order hardening was observed and can be explained by several strengthening mechanisms, which are particularly effective because of a change in crystal structure associated with the ordering transition. IN silver-rich solid solutions containing approximately 17 to 26 at. pct Mg, long- range ordering may occur during appropriate therma1 treatments. Clare-brough and Nicholas1 first detected such long-range order in the solid solution of composition Ag3Mg and suggested that the unit cell of the superlattice contained 256 atoms. x-ray2 and electron diffraction3 investigations confirmed the occurrence of long-range order, but indicated a shifted Ll2-type structure. On the basis of recent X-ray measurements the crystal structure of ordered Ag3Mg has been confirmed as type D023.4 The present paper is concerned with the order-disorder transition in silver-rich Ag-Mg solid solutions and some thermodynamic, electrical, and mechanical properties of the ordered alloys. The effects of short-range order on the properties of silver-rich solid solutions containing up to 26 at. pct Mg are discussed in a concurrent paper.5 1) EXPERIMENTAL PROCEDURES 1.1) Preparation of Specimens. Specimens of Ag-Mg alloys containing from 18 to 26 at. pct Mg were prepared in the form of 1.0-mm-diam wires as described in Section 1.1 of Ref. 5. Disordered specimens were prepared by annealing at 773°K for 1 hr and quenching into iced brine. Ordered specimens were prepared by annealing at 773°K for 1 hr and slowly cooling to room temperature over a period of 15 days. The specimens were stored at 78°K. 1.2) Resistivity Measurements. Electrical resistivi- ties were measured by a potentiometric method.' Equilibrium values were obtained at several temperatures. The kinetics of ordering were investigated by following the time-dependent changes of the resistivity of initially disordered specimens during annealing. The specimens were enclosed in copper capsules and immersed in salt pots; the heating up was accelerated by injecting preheated helium into the capsules. 1.3) Calorimetry. The energies of ordering of the alloys were measured in a tin solution calorimeter as the difference between the heat effects of additions of completely ordered and disordered specimens of the same composition. The procedure and the method of calculation have been described.6 Magnesium was used for thermal compensation in most calorimetric runs in order to improve the accuracy.677 1.4) Mechanical Tests. Tensile tests were carried out with wire specimens at room temperature as described in Section 1.5 of Ref. 5. Microhardness measurements were also made.? 2) RESULTS AND DISCUSSION The characteristics of the order-disorder transition of silver-rich Ag-Mg solid solutions will be discussed first. Some thermodynamic, electrical, and mechanical properties of the ordered alloys will then be considered and compared with the corresponding properties of dis-disordered alloys. 2.1) The Order-Disorder Transition. 2.1.1) Thermodynamic and Structural Aspects. The transition temperatures Tt were determined from discontinuities in the slope of the equilibrium resistivity vs temperature curves. Normalized curves for three compositions are shown in Fig. 1. The transition temperature increases with the magnesium concentration and reaches a maximum at the stoichiometric composition Ag3Mg. The transition temperature of the alloy Ag3Mg was measured as 665° ± 2°K and compares with published values of 660°,1 663°,8 and 66°k.3 In the slopes of the resistivity vs temperature curves of alloys containing 22.2 and 22.5 at. pct Mg, discontinuities were observed at two temperatures. Such upper and lower discontinuities indicate a two-phase field. A modified form of the published phase diagram9 is shown in Fig. 2. A two-phase field was found only on the low-magnesium side of the composition Ag3Mg. On the high-magnesium side, the existence of a two-phase field could not be established because of insufficient resolution, but such a field must be present. This part of the phase diagram can be made complete by a eutec-toid-type reaction a = (a' + ß). The existence of a boundary between the two-phase fields (a + ß) and (a' + ß) is also in accord with published lattice parameters.3 The crystal structure of ordered Ag3Mg (type Do23)

Jan 1, 1969

By C. A. Stetefeldt

Jan 1, 1895

By G. Donald Emigh

WESTERN phosphate resources which lie in Ida- ho, Montana, Utah, and Wyoming, have seen great expansion of activity in recent years. Growth has been two-pronged: expansion in fertilizer use, and since 1949, into the elemental phosphorous industry. Elemental phosphorous, produced in the electric furnace, goes largely into chemical making. Phosphate ore was first recognized in the West about 1889. Production started in 1906, and for many years consisted of underground operations by small companies operating sporadically. In 1920 Anaconda Copper Mining Co. opened the underground Conda mine near Soda Springs in southeastern Idaho, and has maintained and increased its operations since then. About 1930 Montana Phosphate Products Co. began underground mining in Montana and has remained a steady producer. In 1945 San Francisco Chemical Co., one of the oldest companies in the western field, initiated strip mining at the Waterloo mine near Montpelier, Idaho, and later at Leefe mine near Sage Junction, Wyo. In1946 J. R. Simplot Co. began open pit mining at Gay mine near Fort Hall, Idaho. In 1950 Victor Chemical Works began underground development work in the area of Maiden Rock, south of Butte, Mont.: and has since mined there. Monsanto Chemical Co. began open pit mining near Soda Springs, Idaho, in 1951.

Jan 11, 1954

By J. H. Brophy, M. H. Kamdar, J. Wulff

A constitutional diagram for the Ta-W-Re alloy system is presented. Rhenium dissolves in the complete range of solid solutions between tungsten and tantalum up to 48 wt pct in tantalum 'to about 30 wt pct in tungsten. Intermediate x and u phases only are found. X-ray diffraction and fluorescence, metallography and melting-point measurements were employed. THE constitution diagram of ternary alloys of tungsten, tantalum, and rhenium for temperatures above 1000°C is reported in this paper. Alloys in this system rich in tantalum and tungsten are of interest for high-temperature applications, and those rich in rhenium for electronic applications. No ternary phase diagram appears to be available in the literature. The three-component binary diagrams have been previously established1-3 and the present ternary data are consistent with these. EXPERIMENTAL TECHNIQUES Commercially pure tantalum (99.7 pct), rhenium (99.99 pet), and tungsten (99.9 or 99.95 pct) powders were purchased from Fansteel Metallurgical Corp., Chase Brass and Copper Co., and Fansteel or Westinghouse Electric Corp., respectively. These powders were pressed without binder and arc-melted under helium. The preparatory and analytical techniques employed were identical to those used for the Ta-Re system investigation carried out in this laboratory.324 These included X-ray diffraction and metallographic phase identification, X-ray fluorescent and wet chemical analyses, solidus determinations and heat treatments in a resistance-heated tantalum-filament vacuum furnace. For microstructural examinations standard mechanical polishing techniques were used through diamond laps. Polished speciments of all compositions were etched by swabbing with 4 parts HI?, 4 parts HNO3, and 1 part H20. Since the microstruc-tures of alloys containing one or two phases closely resembled their counterparts in the respective binary systems, typical examples are omitted in this presentation. In all the alloys examined, it was possible to observe the number of phases present. Particularly when there were small amounts of one phase involved, it was possible to identify it only by a combined conclusion based on X-ray diffraction, position of an alloy in a composition series, and the phase rule. A total of 100 different alloy compositions was arc-melted and studied in the as-cast condition metallographically and by X-ray diffraction. Specimens of each of these compositions were heat-treated at 2680, 2530, and 2020°C for 1, 2, and 4 hr, respectively. Those which were treated at 2020 were given a preliminary homogenization treatment at 2500°C for 1 hr. Specimens of 25 alloys were heat-treated at 1200o C for 168 hr. Solidus temperature measurements were made by the detection of incipient melting in eighteen alloy compositions. The metallographic and X-ray diffraction results are summarized in Table I. Graphically, this information appears in the isothermal plots of Figs. 2 and 3. Within the accuracy of the experimental methods, two such plots are sufficient to locate these data, since the results for 1200°C were similar to 2020 and those at 2530 resembled 2680

Jan 1, 1962

By James Barr

Geology and Mineralogy1 TENNESSEE phosphates are commercially divided into three varieties: Brown, blue and white. The first two only are now of commercial importance. The white phosphates of Perry county are not being mined at present owing to their pockety occurrence. The white phosphate is Fig. I.-DEPOSITS OF 75 PER CENT. BROWN PLATE ROCK UNDERLAIN BY SAND. the highest grade of the three varieties, running often more than 90 per cent. tricalcium phosphate. The brown rock is found in three varieties, grading from the dense almost vitreous gray rock, 76 to 82 per cent. tricalcium phosphate, down

Jan 9, 1914

By David Cole

THE appearance of the Wilfley table in 1897 marked an epoch in the art of concentration of ores. The table has merited and received an almost unprecedented measure of public approval, lasting through its whole patent life. It has been very little improved in itself, or improved upon by competitors. The new machines bidding for popular favor have been of the Wilfley family, but without ability to do markedly better work than the parent m:-chine, or to (to more work except by the use of superimposed decks, the latter having obvious disadvantages. FIG. 1.-The- Butchart RIFFLE System. During the past three years there has been developed at Morenci a new type or arrangement of riffles applicable to the Wilfley type of concentrating table which corrects many of the objectionable features or limitations of the older system and obviates most of the difficulties encountered with it, particularly when handling ores having a low ratio of concentration. The new type is known as the Butchart1 riffle system, and its general arrangement is shown in Figs. 1 and 2.

Jan 2, 1915

By John V. Beall

Early this year at the University of Arizona in Tucson, a survey was made of student opinion about the minerals industry. Over 100 of the three page questionnaires were completed and these were analyzed by the following categories: 40 Mining Engineering students, 20 Geological Engineering with 2 Geophysical Engineering students, 15 Geology students, 7 Metallurgical Engineering, 26 Underclassmen, 29 Graduate students and a composite of 84 total students. Not all of the results of the survey were predictable. After graduation there is a strong preference toward going to work in the mineral industries. The next most popular options, but trailing the first choice greatly, was graduate work or employment in another industry. A smattering of other choices were for teaching, government or research. None checked the box for drop out.

Jan 1, 1971

By K. C. Mills, E. T. Turkdogan

A number of investigators1 6 have noted the presence of a liquid miscibility gap in the Fe-Sn binary system. However, the first attempt to measure the

Jan 1, 1964

By P. van Meurs, C. van der Poel

From observations of the linear displacement of oil by water from a porous medium as visualized in transparent models, new insight into the mechanism of vircous fingering, as occurring in the case of unfavorable oil-water viscosity ratios, has been obtained. A mathematical description of the observed phenomena leads to formulas. expressing both oil production and pressure drop across the formation as a func-tion of cumulative water injection with the oil-water viscosity ratio as a parameter. Theoretical results are compared with those obtained from scaled laboratory experiments in sand-filled rubes in which water was injected at the one end and production was obtained from the other end. In the second part of the paper the same principles are used to calculate a more realistic production scheme in which production of oil and water is obtained from wells regularly distributed over the field. Results show satisfactory agreement with production data of an actual oil field. Application of the theory is extremely simple as only a limited number of readily available parameters have to be known and results are presented in an analytical form. INTRODUCTION When oil is displaced from a porous medium by water having a viscosity lower than the oil. the oil-water interface is essentially unstable and has the tendency to break up into what are called "fingers" or "streamers". This Viscous fingering has been noted before by Engelberts and Klinkenberg' and has recently been demonstrated in transparent models by van Meurs-. It is highly questionable whether it is at all possible to perform relative permeability measurements In the laboratory reproducing the same distribution of water and oil in the cores as Present in practice. Therefore, we based our descriptive theory on an idealized model which was "tailored" to the fingering mechanism as observed in transparent models under scaled conditions. This approach was the more attractive, as a highly simplified model had already yielded an adequate description of the process. Though we are aware our theoretical approach can be extended in several ways, it is given here in its simplest form to explain the fundamental principles and to avoid complicated formulas. SIMPLEST CASE OF A LINEAR DRIVE Observations and Theoretical Model In Fig. 1 a series of photographs shows how water penetrates into a formation saturated with an oil which is considerably more viscous than the water. The technique for obtaining these photographs, using transparent models, has already been described?. The fingers can be clearly observed and are seen to be mainly parallel to the flow direction. Note that the contours of these fingers are not smooth but show protrusions of water enclosing oil pockets.

By J. L. Lytton

The flow-stress recovery of high-purity aluminurn following a 10 pct tensile prestrain was studied in terms of a fractional flow-stress recovery parameter fr. The flow-stress recovery behavior was related to the dislocation arrangements using transmissiort electron rnicvoscopy. During recovery at 120° and 160°C, nearly stable strength levels were attained, the strength level for 120°C recovery being greater than that for 160°C. This stabilization of flow stress was related to the formation of meta-stable dislocation networks bounding nearly perfect cells. Both network formation and the annealing of dislocation loops were found to be recovery mechanisms, and the stronger metastable strength level joy 120°C recovery was related to a smaller average cell size. Analysis of the networks was consistent with the reaction of sets of dislocations with a/2 (110) Burgers vector to give product Burgers DURING isothermal annealing of cold-worked metals, a degree of softening occurs without re-crystallization, and the processes responsible for this change are termed recovery processes. During recovery annealing, the dislocations generated during cold work become rearranged into low-energy configurations, and as much as 50 pct of the stored energy is released."' The relationship between this rearrangement of dislocations and mechanical behavior is of considerable importance, since the dislocation substructures formed during recovery provide a significant degree of low-temperature strength3j4 and can favorably alter the course of primary creep at high temperatures.4 The purpose of the present study was to relate the flow-stress recovery behavior of high-purity aluminum to the substructural modifications that occur. Electron transmission microscopy was therefore employed for direct observation of dislocation substructures at various stages of recovery following 10 pct prestrain. Several investigators5-' have proposed that dislocations can become rearranged or lost during the preparation of thin foils. It was found early in the present study that the dislocation structures in the thicker regions of the foils changed in a systematic way during the course of recovery. Therefore, it is unlikely that substantial losses or rearrangements occurred during thinning. This point will be discussed in more detail later. The results of various investigators indicate that recovery processes in fcc metals can result in release of 50 pct or more of the total energy stored in the as-prestrained metal, this percentage decreasing with increasing prestrain.' Alloying elements or impurities tend to increase this percentage. The release of stored energy of fcc metals during recovery appears to occur by 1) annealing of point defects if the deformation occurred at sufficiently low temperaturesg and 2) rearrangement of dislocations into low-energy Configurations.1,2In bcc metals, the annealing of dislocation loops has also been observed during recovery after prestrain,10-12 and it has been proposed that this is a recovery mechanism for unidirectionally strained fcc metals.' The density of dislocations in bcc metals has not been observed to decrease appreciably during recovery,10 although the formation of regular dislocation networks has been observed. has shown that the formation of such networks can result in elimination of long-range stresses and can lead to significant release of stored energy without dislocation annihilation. It might thus be expected that network formation is a significant recovery mechanism in fcc metals, although extensive network formation has apparently not been reported in controlled recovery experiments. The formation of sub-boundaries in aluminum has been observed by various investigators13'17 during recovery studies of aluminum, but the structure of these boundaries was not resolved. In this regard, it is significant to note that Bailey and Hirsch,' using transmission electron microscopy, detected no network or sub-boundary formation during recovery of 99.99 pct Ag. Furthermore, Clarebrough et al.2 found no such rearrangements during recovery of copper. EXPERIMENTAL PROCEDURE The high-purity aluminum used in this investigation was obtained in the form of 0.125-in.-thick sheet. Spectrographic analysis revealed that the sheet was 99.995 pct A1 with the following weight-percent impurities: 0.001 Cu, 0.002 Fe, 0.001 Si, and 0.0004 Mg. The as-received sheet was in the heavily cold-rolled condition. The as-received sheet was cold-rolled at room temperature to 0.040-in.-thick sheet in the longitudinal direction, which was the original rolling

Jan 1, 1965

By E. P. Abrahamson II

The effect of transition elements which form binary solid solution upon the recrystallization temperature of zirconium has been investigated. All additions raised the recrystallization temperature. A correlation is obtained between the logarithm of the rate of change of recrystallization temperature with atomic percent solute and the free atom ground state electron configuration of the solute element. ThE work of Abrahamson, et al., on dilute binary solid-solution alloys indicated a correlation between the free-atom ground state electron configuration of the solute and either the brittle-ductile transition or recrystallization temperature. These studies were carried out on bcc base materials. The implication is that the outer s and d electrons of the solute are the prime determinant of the absolute rate of change of recrystallization or transition temperature. Furthermore, the limit of linearity has been shown to be a function of solute electron configuration for recrystallization in iron and vanadium. To date no Complete systematic recrystallization study of dilute binary zirconium base alloys has been made. It is the purpose of this study to note whether the change in solvent structure from bcc to hcp will influence the correlation. It was also desired to learn more of the role of the electron configuration of the solvent on recrystallization temperature. PROCEDURE All alloys were made using 99.87 pct Zr with 0.01 Cr, 0.04 Fe, 0.006 Hf, 0.003 Mg, 0.003 Mn, 0.003 N, and 0.080 0 (132 BHN). The solute elements were 99.9 pct pure. According to the published binary phase diagrams6 and metallographic examinations at X750, all alloys used were solid solutions. The alloys were arc melted and remelted six times in the form of cubic 200-g buttons under an argon atmosphere. They were then hot pressed at 950°C to 0.450 in., upset pressed to 0.350 in., and annealed at 800°C for 1 hr. The specimens were then Blanchard ground to 0.250 in., removing 0.050 in. from each side. The grain size of the material at this stage was found to be 8000 100 grains per sq mm. The specimens were then cold rolled to 0.130 in. and cold pressed to 0.125 in., yielding 50 1 pct cold work. All alloys were then chemically analyzed for the principal addition. The interstitial contents remained at the values of the starting material when checked on random alloy specimens. The rolled sheet was cut into 6.75 by 0.25-in. lengths and heat treated in a gradient furnace for 1 hr. The gradient was 250o to 900°C over the 6-in. length, recorded continuously by six thermocouples resting on each specimen. Control was 3oC, accomplished at the hot end. The recrystallization temperature was determined metallographically using polarized light. The criterion chosen was the point on the specimen showing the first recrystallized grain at a constant magnification, X200. Specimens were repeated, and the agreement was found to be 3°C. RESULTS Three different pure zirconium specimens were tested, and the recrystallization temperature was

Jan 1, 1962

By H. E. Cline

Solidification of Pb-Sn alloys ranging in composition from 1.2 to 56 at. pct Pb ws observed with polarized light. Lamellar structures were observed over a larger range of compositions in alloys containing excess tin than excess lead, as expected from constitutional supercooling. The occurrence of pools of supercooled liquid surrounded by lead is explained by the difficulty in nucleating tin. Cells and dendrites weve observed in tin-rich alloys. Evidence was found that the degenerate structure formed at low growth rates, the formation of faults, and abrupt changes in composition and structure can be attributed to non-steady-state growth. The apparent interface shape was observed to have deep grooves at the interphase boundaries. HUNT and Jackson have observed the shape of the interface during growth of organic eutectics. They observed the formation of lamellar faults and shape instabilities upon changes in growth rate. The lamellar structure in these organic eutectics was not restricted to the eutectic composition. Recent work by Mollard and Flemings2 indicated that Pb-Sn alloys from 12 to 26 at. pct Pb could be solidified with a lamellar or rodlike structure if a sufficiently steep temperature gradient was used at a slow growth rate. Observations of the solid liquid interface of the Pb-Sn eutectic were made by Davies3 using polarized light. Photographs were at too low a magnification to determine the interface shape, but he has concluded that tin was the leading phase. In the following experiments, solidification of a range of Pb-Sn alloys from 1.2 to 56 at. pct Pb was observed using polarized light, to determine the factors controlling stability of the lamellar structure. EXPERIMENTAL Procedure. One hundred-gram ingots of alloys prepared from 99.999 pct pure Pb and Sn were cast into graphite molds under argon. The compositions of the alloys were 1.2, 6, 12, 26, 36, 46, and 56 at. pct Pb. Two-gram pieces were melted between two cover glass slides which were squeezed into a 1-mm separation. Samples were then observed under polarized light in a hot stage shown in Fig. 1. A long working distance objective designed for viewing at 500 times was used. Photography was made difficult by the lack of illumination and contrast at these high magnifications. By using an elliptical polarization compensator, as suggested by A. Holik, the contrast and illumination could be optimized. Photographs could be taken only at slow growth rates to avoid excessive interface motion during the 15-sec exposure used. The solidification rate was varied by increasing or decreasing the power to the heater. It was found that insulation was necessary to avoid undesired growth rate fluctuations. The temperature gradient, as measured with two thermocouples 1 cm apart, was 80" ± 20°C per cm during all the experiments reported here. The advantage of this procedure is in being able to observe solidification while it is occurring. However, the observations are restricted to the glass-metal surface and may be influenced by this surface. Also, one has no knowledge of the interior of the sample, in contrast to studies of the freezing of transparent organic eutectics.' Observations. The alloy near the eutectic composition (26 at. pct Pb) solidified in a lamellar structure when the growth rate was uniform. If the growth

Jan 1, 1968

By F. C. Wagner, E. P. Klier, D. E. Nulk

The presence or absence of plastic strain at a cleavarage surface is a question of much importance, and upon its answer depends future possible theoretical work. To investigate this question back-reflectinn X ray patterns were obained on the cleavage facets of ferrite grains. The test set-up consisting of FeK colli- mated radiation, single grain material and stationary cassette and specimen will not lead to a diffraction pattern, in general, but is an ideal arrangement for the exami-nation of surface effects. A pattern taken on hydrogen purified

Jan 1, 1949

By L. L. Seigle

Free energies, heats, and entropies of mixing of solid Fe-Au alloys have been measured by the galvanic cell method between 800° and 900°C. A positive deviation from Raoult's law and a large excess entropy of mixing were observed, both attributable to lattice distortion caused by the disparity in component atom sizes. Since the terminal solid solutortiontions are not regular, thermodynamic properties computed from the location of the mis-cibility gap do not agree well with measured quantities. The electromotive force data suggest some changes in the existing Fe-Au phase diagram. ALTHOUGH a considerable amount of information has been accumulated about the thermodynamic properties of metal solid solutions which exhibit negative deviation from Raoult's law, particularly those in which ordering occurs, relatively few experimental measurements have been made on solutions with positive deviation. This is due to the infrequency of broad homogeneous regions suitable for experimental measurement in solutions of this type, since any marked positive deviations from ideality lead to restricted solubility and the formation of miscibility gaps. Thermodynamic data reported in the literature for such systems have usually been calculated from the location of the miscibility gap boundaries under the assumption that the entropies of mixing are ideal, i.e., the terminal solutions are regular.' One of the few binary systems with both positive deviation and a wide homogeneous range in the solid is the Ni-Au system. A recent investigation of solid Ni-Au alloys' revealed that the entropies of mixing were much larger than ideal and consequently thermal data computed from the phase boundaries assuming regular solutions were seriously in error. Theoretical considerations put forward by Zener indicated that high entropy values should generally be associated with systems possessing a miscibility gap in the solid, when this is due to differences in the size of component atoms. These facts suggest that the regular solution assumption is a poor approximation for many solid solutions with positive deviation and that reliable thermodynamic data generally cannot be obtained by conventional methods from the location of miscibility gap boundaries. The Fe-Au system, Fig. 1, resembles the Ni-Au system in certain respects. The presence of a miscibility gap in the solid indicates a large positive deviation from ideality, but there is nevertheless an extensive single phase region suitable for experimental measurement. The following investigation of solid Fe-Au alloys was carried out in order to obtain additional data on the thermodynamic properties of metal solid solutions with positive deviation from Raoult's law and to further compare thermodynamic data computed from miscibility gap boundaries with those measured experimentally. Experimental Method The thermodynamic properties were derived from measurements of the potential developed between pure solid iron and Fe-Au alloys in a high temperature galvanic cell. The experimental apparatus and technique were the same as those used for the Ni-Au alloys and described in a previous report.' Cell electrodes were 1/16 in. diam rods swaged from chill-cast ingots and annealed for one week at 850°C. The alloys were prepared by melting fine gold granules under argon with pure iron obtained from the National Research Co. The cell electrolyte was

Jan 1, 1957