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By Harold Margalin, Elmars Ence

M. H. Mueller, M. V. Nevitt, and H. W. Knott (Argonne National Laboratory)—We have reported1 the crystal structure of Ti2CU as body centered tetragonal with a. = 2.944A and co = 10.786A, six atoms per unit cell, and space groupl4/mmm(MoSi2 type). This cell is larger but definitely related to the unit cell reported by the authors. It permits definite positions for the titanium and copper atoms in the cell located as follows: 2 Cu (a) 0 0 0; 1/2 1/2 1/2 4 Ti (e) 0 0 z; 1/2 1/2 1/2 + z; 0 0z; 1/2 1/2 1/2- z where z = 0.341 The face centered tetragonal cell reported by the authors can be transformed to a small body centered tetragonal cell with flo (small bet) = ao(fct)v2 Both unit cells have the same CO. Neither the face centered tetragonal cell with four atoms per unit cell nor the small body centered tetragonal cell with its two atoms per unit cell lend themselves conveniently to an orderly arrangment of the 2 to 1 ratio of titanium to copper atoms. When the co of this small body centered cell is tripled, however, a large body centered tetragonal cell results with six atoms per unit cell as described above. We had also noted that the X-ray patterns of Ti2Cu indicated that the structure could be approximately described by the face centered tetragonal cell as reported by the authors; how- ever, there was evidence for a few additional very weak lines whose positions indicated a larger unit cell. Since the X-ray scattering amplitudes of titanium and copper are nearly equal, it is evident that it is difficult to distinguish their positions especially from X-ray powder patterns. It was therefore decided to look at a powder pattern obtained by neutron diffraction since the scattering amplitudes of the two elements are considerably different in magnitude and opposite in sign. The sample used for neutron diffraction was selected from a group of three alloys prepared by arc melting using crystal bar titanium of 99.92 pet nominal purity and 99.999 pet pure Cu. The alloys designated as A, B, and C had the following respective compositions: Ti-32.8 at. pet Cu, Ti-33.3 at. pet Cu, and Ti-33.8 at. pet Cu. On the basis of the melting losses incurred, it was established that the actual concentration of either component in any of the alloys probably did not deviate from the intended value by as much as 0.1 at. pet. The alloys were annealed for 5 days at 700°C in evacuated Vycor capsules and quenched in tap water. The metallographic structures of these alloys are shown in Fig. 1. None of the alloys contained sufficient second phase to permit its positive identification. Since alloy B contained the least amount of second phase and since its composition placed it closest to the ideal stoichiometry, it was chosen for the neutron diffraction study. The oxygen content of alloy B was found by chemical analysis to be 0.06 at. pet. This particular intermetallic compound is especially suitable for investigation with neutron diffraction since if the titanium and copper atoms have a random statistical distribution, a near null-matrix would result in which there would be practically no coherent scattering of neutrons, and hence no Bragg diffraction peaks. Such a condition could come

Jan 1, 1962

By G. H. Bishop

The kinetics of the inter granular penetration and embrittlement of [100] tilt boundaries in 99.998 pct pure nickel upon exposure to bismuth-rich Ni-Bi liquids have been determined in the temperature range from 700° to 900°C. The kinetics of penetration are parabolic in time at constant temperature over most of the temperature range. In a series of 43-deg bicrystals the rate of penetration is anisotropic with respect to the direction of penetration into the grain boundaries. In lower-angle bicrystals the penetration rate is isotropic. The rate of penetration decreases with tilt angle at 700°C. The activation energy for penetration in the 43-deg bicrystals is 42 kcal per g-atom independent of direction. It is concluded that the intergranular penetration and embrittlement in the presence of the liquid proceeds by a grain boundary diffusion process and not by the intrusion of a liquid film. This was confirmed by a determination that the kinetics of penetration and embrittlement were the same in the 43-deg bicrystals upon exposure to bismuth vapor under conditions such that no bulk liquid phase would be thermodynamically stable. WhEN solid metals are exposed to a corrosive liquid-metal environment, the grain boundaries are sites of preferential attack. Depending on the temperature, the composition of the liquid, and the composition, structure, and state of stress of the solid, a number of modes of attack are possible. This paper reports a study of the kinetics of intergranular penetration and embrittlement of high-purity nickel bicrystals upon exposure to bismuth which, together with an earlier study by Cheney, Hochgraf, and Spencer,&apos; demonstrates that there are at least two modes of intergranular attack possible in the Ni-Bi system. In the study by Cheney et al., columnar-grain specimens of 99.5 pct pure nickel were exposed to liquid bismuth presaturated with nickel in the temperature range 670" to 1050°C. They found that the majority of the boundaries, which were predominantely high-angle boundaries, were penetrated by capillary liquid films, the attack proceeding by a process which will be termed grain boundary wetting. This process occurs in a stress-free solid when twice the liquid-solid surface tension is less than the surface tension of the grain boundary,* i.e., when 2yLs < YGB In this case the penetration of the grain boundary by the liquid occurs at a relatively rapid rate, resulting in the severe embrittlement of a polycrystalline solid. Grain boundary wetting is a common mode of intergranular attack in systems in which the lower melting component is relatively insoluble in the solid, but the solid has an appreciable solubility in the liquid, for example, the Ni-Bi system, Fig. 1. In systems of this type at temperatures above the range of stability of any intermetallic phases, once the liquid is saturated with respect to the solid so that no gross solution occurs, chemical gradients are small, and surface tensions become major driving forces for attack, provided the solid is stress-free. The results of Cheney et al. appear to be typical of those encountered when grain boundary wetting occurs.&apos; Capillary films were observed in the boundaries after quenching from the exposure temperature. The mean depth of penetration increased linearly with time, and the activation energy for the process was found to be 22 kcal per g-atom. In a study of the Cu-Bi system Yukawa and sinott4 found that the depth of penetration of bismuth into high-purity copper bicrystals of orientations from 22 to 63 deg of tilt about (100) at 649°C ranged from 0.05 to 0.25 in. after a 12-hr anneal. This corresponds to a linear rate of 6 to 15 X 10~6 cm per sec. At the same reduced temperature of 0.68 the rate for the Ni-Bi system&apos; was 7 x lo-&apos; cm per sec. In another study of the Cu-Bi system, Scheil and schess15 determined the kinetics of grain boundary wetting in hot-worked commercial rod. While there were several complicating factors present in this study, there is general agreement with the above results. The kinetics of penetration were linear, the activation energy was 20 kcal per g-atom, and at 650°C the rate of wetting was 2 to 5 x 10-6 cm per sec. The rate of wetting in the A1-Ga system6 is somewhat

Jan 1, 1969

By M. G. Nicholas

The influence of deformation, relative movement and surface cleanliness on the strength of room -temperature "interparticle" bonds between copper surfaces has been studied. No bonding resulted when clean surfaces were merely pressed together, even under pressures of 50,000 psi. Bonding resulted, however, when clean surfaces were simultaneously pressed and moved relative to each other, some bonding occurring no matter how small the pressure or relative movement. Exposure of the clean surfaces to various chemicals inhibited bonding, none at all being produced by small relative movements. The size of the movements which first produce bonding between exposed surfaces depends on the nature of the chemical, being less than 0.002 in. for cleansing reagents and greater than 0.004 in. for lubricants, water and hydrogen sulfide. It is concluded from the experimental data that the prime requirement for bonding is the dispersal of surface films such as oxides and adsorbed contaminants. THE formation of interparticle bonds during the room-temperature compaction of powder metallurgy components greatly increases the ease of handling in subsequent production operations prior to sintering. The strength of unsintered compacts follows the same general trends as their density and hardness, but quantitative data are extremely Scarce. Quantitative correlation of the data on the overall strength of a compact with that of the individual interparticle bonds is virtually impossible due to the extremely complex geometry of powder compacts. Qualitatively, however, the strengths of unsintered compacts can be correlated with variations in parameters known to influence the extent of cold bonding, and hence interparticle bonding, such as surface cleanliness, relative movement, and deformation of the mating surfaces. Kuzmic and seelig4 found that contamination of powder particle surfaces with lubricants reduced the strength of unsintered iron and copper compacts. Interparticle shear has been shown to promote bonding by Train and Hersey7 while Gregory has shown that die rotation is beneficial. Eilender and schwalbe6 concluded that most bonding occurred during the early stages of pressing iron powder compacts when interparticle shear is one of the principal processes occurring. mile there can be little doubt that these and other factors, such as particle size and shape, affect the extent of interparticle bonding produced by compaction, evaluation of the influence of individual factors is not easy. Particle deformation and relative movement, for example, occur simultaneously during compaction, making any precise measurement of their relative influences difficult. Because of these and other difficulties encountered in studying interparticle bonding in actual powder compacts, the approach adopted in this study was to

Jan 1, 1963

By P. E. Busby, C. Wells

FURTHER study of data used in determinations of 1—rates of diffusion of boron in austenite and 2—solubilities of boron in the a and phases of iron and steel&apos; has provided an equation for the diffusion of boron in a iron. In brief, the previously published data were accumulated from the results of deboron-izing (and decarburizing) experiments carried out in the range of 700° to 1300°C. Diffusion coefficients (D?) for boron in austenite were calculated using the Grube solution of Fick&apos;s law. However, only solubility values were estimated from the discontinuous concentration-penetration curves, Fig. 1, which are characteristic of diffusion in two phases. Dr. Carl Wagner&apos; has recently provided a solution for calculating D values from penetration curves of this type as follows: Cl1.1 —C8/C8- C11.1 = vp ? e ? erf (?) and D = ?/4?2 t where C11,12, C8, C11, and E have the values shown in Fig. 1. D is the diffusion coefficient, sq cm per sec; t is time of deboronizing anneal, see; and ? is a di-mensionless parameter. For a given diffusion experiment, the value of ? can be readily obtained by graphical solution from a plot of y vs the right-hand part of Eq. 1. D may then be evaluated from Eq. 2. The avplication of this solution to previously re-ported results, of which excerpts are given in Table I, permits the calculation of diffusion coefficients for boron in a iron. On the basis of these meager data, it is tentatively concluded that the diffusion of boron in a may be represented by the equation Da = 1011 e-92,900/RT where R is the gas constant, cal X 0C-1 X mol-1; and T is the absolute temperature, OK. Although the frequency factor, 106 sq cm per sec, is admittedly several orders of magnitude higher than expected, the value of Q, 62,000 cal per mol, appears reasonable and is, in fact, very similar to that for the self-diffusion of iron. It is pertinent to mention at this point that the value of Q obtained for the diffusion of boron in austenite by means of the Wagner solution is 19,000 cal per mol and is in excellent agreement with the value previously reported1 in the equation DT = 2xl0-3 e-21,000/RT [4] which was determined by the application of the Grube solution to other data. The fact that determined constants A and Q in the equation D? = A e-Q/RT were practically the same, independent of whether the Wagner or Grube solutions were used in determinations of D values, strengthened the authors&apos; belief that the computed values of D (Table I) using the Wagner solution are reliable. The relative values in Eqs. 3 and 4 for the diffusion of boron in the a and ? phases, respectively, suggest that boron forms a substitutional solid solution in a iron and an interstitial solid solution in ? iron. The same tentative conclusion has been reached by McBride et al.3 on the basis of relative solubilities, atom diameter, and the size of the interstitial hole in a and ? iron. In connection with the data for test 14 listed in Table I, it is of interest to calculate the solubility of boron in a iron using the D value given by Eq. 3. As might be anticipated from the small movement of the interface in test 14, proper substitutions in Eqs. 2 and 1 give a low value, approximately 0.0004 pct B, at 850°C. Apparently at 835°C (test 13) it is possible to obtain 0.0018 pct B, and at 850°C only 0.0004 pct B into solution in the a phase before a second phase appears. These observations are consistent with the Fe-B constitution diagram proposed by McBride, Spretnak, and Speiser.3 References P. E. Busby, M. E. Warga, and C. Wells: Diffusion and Solubility of Boron in Iron and Steel. Trans. AIME (1953) 197, p. 1463; Journal of Metals (November 1953). &apos;W. Jost: Diffusion in Solids, Liquids, Gases. (1952) pp. 69-71. New York. Academic Press Inc. "C. C. McBride, J. W. Spretnak, and R. Speiser: A Study of the Fe-Fe2B System. Trans. ASM (1954) 46, p. 499.

Jan 1, 1955

By M. R. Geer, H. F. Yancey, P. S. Jacobsen

Two growing problems confront the preparation engineer—still further restrictions on stream pollution and a greater proportion of fine coal as more and more continuous miners come into use. The de-watering screens, centrifuges, and settling ponds that sufficed a few years ago must often be supplemented by more effective equipment, and in some instances the finest solids are now being recovered by vacuum filtration, once considered too costly in many coal washeries. Unfortunately not all slurries can be readily filtered. Some are virtually unfilter-able, and others do not permit the high cake rates needed to hold costs within reason. Often, however, these difficult slurries can be rendered filterable by flocculation. Starch and lime have long increased settling rate in thickeners and can also aid filtration. More recently there have been other flocculants, primarily synthetic polymers or gums. Reports of their great effectiveness prompted the U. S. Bureau of Mines to test their use in filtration as part of its program on recovering and cleaning fine coal. The object of the present work was to compare some of the newer flocculants with starch and lime and to test the reaction of different types of slurries to flocculation. Three natural slurries, three synthetic coal-clay mixtures, and five flocculants were tested, all with a laboratory filter leaf. Slurries and Flocculants Tested: First of the slurries was the thickener feed from the washed coal section of the Michel colliery of Crow&apos;s Nest Pass Co. Ltd., Michel, B.C. As shown by the screen and ash analyses in Table I, practically all this slurry was finer than 28 mesh, and about half the solids were finer than 200. Substantially all material coarser than 200 mesh was clean coal, but the ash content of 20.7 pct in the finest size indicates a moderate amount of impurity. This coal is medium-volatile bituminous in rank. Slurry was also obtained from the Black Diamond washery of Palmer Coking Coal Co., King County, Wash. This underflow of a 1/2-mm vibrating slurry screen is a waste product discharged to a settling pond. As shown by the data in Table I it contained about 20 pct material finer than 200 mesh, which analyzed 77.5 pct ash, indicating a high proportion of clay. The coarser sizes were also high in ash content because of the presence of bone and shale. Black Diamond coal is on the dividing line between bituminous and subbituminous rank. The third slurry, from the washery of Roslyn-Cascade Coal Co. in Kittitas County, Wash., was the underflow of a battery of 8-in. cyclones that is wasted with the coarser refuse from the plant. In both size and ash content this slurry was similar to the Black Diamond, but since it was a cyclone-underflow product, the fraction finer than 200 mesh undoubtedly contained a much smaller proportion of finely divided clay than was present in the Black Diamond slurry. The Roslyn-Cascade coal is high-volatile A bituminous in rank. Initially the slurry samples were stored in the laboratory at a concentration of 40 pct solids. A progressive change in filtration and flocculation characteristics during storage was noted, however, presumably because of progressive disintegration of the clay. After careful testing demonstrated that the slurry solids could be dried and then repulped without changing the original filtration characteristics, this procedure was adopted. The flocculants used were Separan 2610, Kylo 27, Jaguar MD-A, Idaho potato starch, and lime. The lime was used as a slurry, the Separan 2610 as a 0.10 pct aqueous solution, and the other flocculants as 0.50 pct aqueous solutions. The starch was causti-cized with sodium hydroxide before use. As some of the flocculants are reported to deteriorate on storage, new batches of flocculants were prepared every two days. Test Procedure: Fig. 1 diagrams the filter leaf apparatus employed. This consists of a test leaf having an effective area of 0.10 sq ft., a 60°, 8 1/2-in. diam cone to hold the slurry sample, a variable-speed electric stirrer, vacuum gage, bleed line for controlling vacuum, filtrate flask, moisture trap, and vacuum pump. Two filter cloths were selected—Saran SA 603, a monofilament, coarse-weave cloth, and polyethylene PO-801 HF, a monofilament, fine-weave cloth. The Saran was selected to provide maximum cake rate without regard to clarity of filtrate and the polyethylene to provide the best quality of filtrate without regard to cake rate. The test charge for the filtering vessel consisted of 800 g of solids (previously soaked for 24 hr) and

Jan 1, 1960

By Walter L. Crow

MUCH has been published on highly technical phases of grinding. Very little has been written on how a mill man can improve his operations by determining the optimum size assortment of grinding balls that should be added as a makeup charge. This ball rationing is not to be confused with the ball ration used as an initial charge when the mill is started up. Ball rationing is considered for one or more of the following purposes: 1) to increase throughput of the mill, 2) to reduce the power required per ton of ore ground to the desired size, 3) to reduce steel consumption per ton of ore ground, 4) to improve product size, and 5) to lower retention time of ore in the mill.

Jan 7, 1957

By P. Wynblatt, J. E. Dorn

The effect of strain rate, temperature, and interstitial impurity concentration on the flow stress was investigated in a poly crystalline Fe-2 pct Mn alloy. The temperature dependence of the flow stress was found to be independent of the interstitial impurity concentration, removal of interstitials merely decreasing the atherma1 stress level. Below 160%, the large temperature dependence of the flow stress was interpreted in terms of the Dorn-Rajnak theory of the Peierls mechanism of plastic deformation. Above 160"K, some other thermally activated intrinsic meckanisln seems to be operating. The strong temperature dependence of the flow stress of bcc iron at low temperatures has been studied by numerous investigators and interpreted in terms of several different thermally activated dislocation mechanisms. The following mechanisms have been proposed: a) interaction of dislocations with interstitial impurity atoms1 or with solute atoms in general; b) interaction of dislocations with clusters of impurity atoms;3 c) resistance to the motion of dislocations due to jogs on screw dislocations;* d) resistance to the motion of dislocations due to the Snoeck effect;&apos; and e) interaction of dislocations with the intrinsic resistance of the bcc lattice or Peierls "hills". In previous work: it was found that the plastic behavior of polycrystalline iron containing 2 wt pct Mn (and 100 ppm C + N) is in good agreement with predictions based on the Peierls mechanismlo from 77" to 160°K whereas from 160" to about 370°K another as yet unidentified thermally activated mechanism is operative. The purpose of the present investigation was to determine the effect of interstitial impurities on the temperature dependence of the flow stress, by purifying the previously investigated alloy with respect to interstitial impurities. The investigation revealed that removal of the interstitial impurities to a level that eliminated Cottrell locking and the Portevin-LeChatelier effect (i.e., serrations in the stress-strain curve due to dynamic strain aging) affects neither the strong temperature dependence of the flow stress at low temperatures nor the general characteristics of the higher-temperature behavior. Such purification, however, lowered the athermal yield stress. I) EXPERIMENTAL PROCEDURE AND RESULTS The material used in this investigation consisted of an Fe-2 wt pct Mn alloy having the following additional elements present: 0.004 pct C, 0.006 pct N, 0.05 pct 0, 0.004 pct S, 0.003 pct P, and 0.001 pct Si. This was the same material as that studied in the previous investigation and will henceforth be referred to as the "impure material". The as received -jr by 2 in. hot-rolled bars were cold-rolled to 0.08-in. thickness, recrys-tallized under argon for 30 min at 80O0C, and further cold-rolled to 0.053-in. thickness. Flat tensile specimens 3 in. wide having a 1.625-in.-long gage section were machined from the sheet and then purified. The first stage of purification consisted of holding the specimens at 850°C for 24 hr in a stream of hydrogen saturated with water vapor at room temperature. Material prepared in this fashion will subsequently be referred to as "wet hydrogen purified material". It has been estimated that this type of treatment reduces the carbon content of iron to less than 5 ppm.&apos; The second stage of purification consisted of holding the specimens in a closed system through which hydrogen was circulated past the heated specimens as well as a zirconium hydride getter. The specimens were held at 850°C and the getter at 800°C. The process was continued for 212 hr. The starting material for this process was wet hydrogen purified material. Material prepared in this manner will be referred to as "ZrHz purified material". The technique used was substantially the same as that described by Stein et al.&apos; who have shown that the carbon level at the end of the process is reduced to about 5 parts per billion. The mean grain size of the three materials was found to be -60 C( for the impure material and -160p for the wet hydrogen and ZrHz purified materials. All tensile testing was carried out on an Instron Testing Machine either in controlled-temperature baths or at fixed-point baths such as boiling liquid nitrogen, and so forth. When fixed points were used the temperature was kept constant to better than *1°C whereas in all other tests the temperature variation was less than *2°C. Test of Purity. It was not possible to determine the purity achieved at each stage of the purification because the resulting level of interstitial impurities was near or below the limit of sensitivity of standard analytical techniques. It was possible, however, to obtain a qualitative measure of the extent of purification from the appearance of the stress-strain curves for the three materials. Fig. 1 shows the stress-strain curves for the three different materials tested at 300°K. It can be seen that the effect of wet hydrogen

Jan 1, 1967

By V. A. Phillips, M. Safdar Ali

The tensile properties of Cu-0.20 pct Al, Cu-0.45 pct Mg, Cu-0.27 pct Cr, and Cu-0.22 pct Be solid-solution alloys were studied at -196°, 18°, 2509 and 500°C on wires internally oxidized at 900°and 1000°C. Internal oxidation produced marked increases in yield strength relative to pure copper, particularly at low temperature. The yield strength decreased with increase in temperature to a much greater extent than predicted by current theories of dispersion hardening. The strengthening effect of internal oxidation persisted throughout the entire stress-strain curve, but since a marked loss of ductility occurred at all test temperatures, only modest increases in tensile strength were realized. INTERNAL oxidation involves the preferential oxidation of a baser solute in a relatively noble solvent by diffusion of oxygen into the solid. Since the process is diffusion controlled, it is expedient to carry it out at a high temperature often approaching the melting point. The amount of solute is limited and the oxidation conditions adjusted so that oxygen diffuses inwards to meet the solute causing reaction to progress inwards and form subscale instead of only sur face scale. The reaction can be made to occur throughout the thickness of thin material producing a fine dispersion of oxide inside the metal. C. S. Smith1"3 appears to have been the first to recognize the true nature of the process of internal oxidation. Although extensive kinetic and metal-lographic studies followed by Rhines and coworkers,4-5 Chaston7 andMeijering and Druyvesteyn8 working independently were the first to report hardening effects due to internal oxidation. These results prompted detailed studies of the effects of internal oxidation on the hardness, tensile, creep, and fatigue properties of a number of alloys by G. C. Smith and coworkers9-12 in England, on hardness by Gottardi13 in Italy, and on hardness and tensile properties by wood14 in the U.S.A. Publications dealing with other aspects of internal oxidation will not be reviewed here. Internal oxidation of solutes having a high affinity for oxygen provides a means of obtaining very fine dispersions stable in a suitable atmosphere at temperatures well above those at which most age harden ing precipitates coalesce. The process therefore offers a method of producing thin sheet and wire of possibly outstanding creep resistance. The size limitation might be overcome by internally oxidizing porous powder compacts made from alloy powder before final sintering. PREPARATION OF ALLOYS The alloy ingots, which were approximately 5 1/2 in. long by 1 in. diam, were made up in a high-frequency furnace, using as raw materials OFHC copper, 99.99 + pct Al, high-purity magnesium, and master alloys of Cu-4.19 pct Be and Cu-10 pct Cr. The alloys containing aluminum and magnesium were melted ii closed high-purity graphite crucibles and solidified in the crucible which was lowered partly Out of the coil to give a hot-top effect. The alloys containing beryllium and chromium were made by melting in vacuo in alumina-lined sillimanite crucibles. The magnesium, chromium, and beryllium

Jan 1, 1960

By H. T. Clark

NO previous determinations of the deformation or recrystallization textures of titanium or of titanium-base alloys have been reported in the literature. The room-temperature structure of titanium is hexagonal close-packed with a c/a ratio less than 1.633. It would be expected, therefore, to have a rolling texture similar to that of other hexagonal close-packed metals, namely (0001) [1010]. Burgers and Jacobs1 have shown that zirconium, a metal isomorphous with titanium in its structure and similar in many of its properties, has such a texture with a scatter of the basal plane toward the transverse direction. This scatter is in the opposite direction from that found in magnesium by Bakarian2 but similar to that reported by Smigelskas and Barrett3 or beryllium. The rolling and annealing textures reported here for high-purity iodide titanium are significantly different from the . textures of any other hexagonal close-packed metal. All titanium used during this investigation was prepared by the iodode process." The annealed hardness of this material varied from 73 (material used for sample No. 2) to 97 Vickers hardness number. An estimate of the chemical composition of this grade of titanium has been reported by Finlay and Snyder.5 With one exception, shown in table I, the as-deposited titanium was cast into 10 to 20 g ingots in an electric arc furnace in purified argon before being rolled to sheet. The cast ingots were forged and ground until their cross-section was approximately rectangular, annealed 1 hr at 700°C in vacuum and cold rolled. Rolling was carried out in a two-high, 4 in. diam mill, using reductions no greater than 10 pct per pass. The direction of rolling was reversed after each pass, and, in order to avoid temperature effects, the sheet was allowed to cool after each pass. Unless the rolled sheet was sufficiently thin for X-ray penetration (about 0.004 in.), it was reduced to this thickness by pickling. Because of the possibility of introducing twinning or other deformation during grinding, no attempt was made to maintain uniform thickness of the sample during pickling by intermediate grinding or sanding operations. Those samples to be used for determining the annealed texture were recrystallized by vacuum annealing the cold-rolled sheet for 1 hr at 500°C. These thin samples were held between thick titanium sheets during annealing to prevent distortion. Table I outlines the rolling and annealing schedule of those samples for which photograms or texture patterns are shown. X-ray Techniques The usual techniques for determining textures were employed during this work. Molybdenum radiation was used for the transmission exposures and copper radiation for the glancing angle ones. Since titanium fluoresces under these conditions, it is necessary to employ a filter between the sample and the film. The Kß radiation filters are very satisfactory for this purpose. Sufficient grains having favorable orientation were present in both the cold-worked and in the cold-worked—500°C annealed samples to provide satisfactory patterns with the samples stationary. Because of the difficulties of comparing intensities of transmission photograms with those obtained

Jan 1, 1951

Jan 1, 1931

By H. I. Smith

CONTENTS [PAGE Problems of Mining and Processing Mineral Aggregates (TP 1649, by NATHAN C. ROCKWOOD, Min. Tech., Nov. 1943. Discussion by H. I. SMITH, IRVING WARNER and the author) t Mica in War (TP 1749, by RUSSELL G. WAYLAND, Min. Tech., July 1944. Discussion by H. S. SPENCE) 3 Three Roofing-granule Plants in Pennsylvania (TP 1787, by RICHARD M. FOOSE, Min. Tech., Jan. 1945. Discussion by H. I. SMITH)5 Methods of Prospecting and Mining Optical Calcite in Montana (TP 1896, by E. W. NEWMAN, Min. Tech., Nov. 1945. Discussion by W. C. STOLL and FRANK C. ARMSTRONG, and the Glass Sand and a Glass Industry in Puerto Rico (TP 1939, by HOWARD A. MEYERHOFF and J. EARL FRAZIER, Min. Tech., Nov. 1945. Discussion by A. M. SHORT, the author and PHILIP The "Bonanza" Mica Operation of Purdy Mica Mines, Limited, Mattawsn Township, Ontario (TP 2154, by HUGH S. SPENCE, Min. Tech., March 1947. Author&apos;s supplement and discussion by JOHN A. BAKER, E. J. LINTNER, and the author) 7 Process for Manufacture of Dead-burned Magnesite and Precipitated Calcium Carbonate from Dolomite (TP 2155, by ROBERT D. PIKE, Min. Tech., March 1947. Discussion by 0. C. RALSTON and the author) 9] Problems of Mining and Processing Mineral Aggregates H. I. SMITH*-Mr. Rockwood has presented a very interesting paper on problems of the mineral aggregate industry in meeting specification requirements, which apparently are ever decreasing in tolerance. May I call attention to a method of mineral separation that may be of value in separating the flat aggregate particles from the more angular ones and possibly the soft particles from the hard. The method is the old Pardee spiral coal separator, extensively used many years ago in the anthracite region for separating rock and bone from anthracite coal.1 The success of the process depends on the relative coefficient of friction of the aggregate particles to be separated rather than on their relative specific gravity. The flat and the soft particles normally will slide more slowly and stay on the inner spiral until they reach the delivery spout at the bottom whereas the round and the angular pieces will work to the outer edge and fall off into a spiral of larger diameter. The capacity of the separator is increased materially by having three inner spirals, with a separate feed for each, on which the particles travel more slowly, and one outer spiral from which the more rapidly traveling pieces slide to the bottom. IRVING WARNER*-I have long been convinced that much of the equipment and methods developed for mineral dressing might be advantageously employed in the mineral aggregates industry, and more particularly in the production of sand and gravel. The two industries are not well acquainted with each other or their problems. They have separate trade publications. The difficulty with the situation is that there are few large sand and gravel plants and few provided with technical services in their own organization or by retainer. This does not refer to engineering organizations but rather to improvement of plant technic in processing.

Jan 1, 1947

By Nicholas J. Grant, David S. Bloom

An investigation of the Cr-Ni system has revealed that there exists a eutectoid transformation at about 1180°C. &apos;The transformation in chromium implied by the eutectoid reaction was detected at about 100°C below its melting point. Associated with the eutectoid transformation, a metastable transition structure has been found. THE Cr-Ni phase diagram is shown in current literature to be a simple eutectic system in which the high chromium end of the diagram is incompletely determined, Fig. 1. The last investigation of this system was undertaken in 1936.&apos; Because of limitations in metal purity, especially of chromium, and temperature measuring techniques, the diagram should be accepted with some reservations, as was indicated by Hansen.V or examwle.-, the wresence of the compound Cr²Ni, with a tetragonal structure," remains unverified and incompatible with the simple eutectic diagram. The work reported here began because of discrepancies that appeared in experimental studies in the binary alloys Cr-Ni and in the ternary system Cr-Mo-Ni. The existing binary Cr-Ni diagram failed to provide a complete explanation of observations made by microscope, X-ray, and thermal analyses. Experimental Methods The materials employed were of a higher degree of purity than were available to previous investigators. The Mond nickel used had a nominal purity of 99.87 pct, while the electrolytic chromium analyzed 99.03 pct with the major impurity being 0.5 to 0.7 pct oxygen with some iron. All alloys were melted in a vacuum furnace to remove dissolved gases, sufficient carbon was added to the charge to combine with all the oxygen as CO. Final analysis determined the carbon as about 0.02 pct and the oxygen around 0.06 pct or slightly more. Stabilized zirconia crucibles and thermocouple protection tips were used throughout and contributed no detectable impurity to the melts, as long as the oxygen in the chromium was kept low. Heats averaged about 250 g, which permitted about 2 in. of the thermocouple protection tips to be submerged. The temperature drop across the thermocouple protection tip was determined to be about 3°C, a minor source of error. The alloys, after removal from the vacuum furnace, were placed in a furnace operating in a purified argon atmosphere for the thermal analyses. An- nealed wolfram-molybdenum thermocouples provided the primary means of temperature determination, though a Pt-Pt-10 pct Rh couple was employed for a check when possible. A sensitive, high-speed Leeds and Northrup Speedomax recording potentiometer indicated the thermocouple output. X-ray diffraction patterns were obtained primarily on a Norelco unit, which permitted diffraction angles only up to 45" (28 = 90"). In general, either rotated or stationary solid samples were used, because it later evolved that many samples were susceptible to transformation resulting from the cold working involved in pulverizing. It was also noted that rotating a sample sometimes suppressed weak lines, so, usually, samples were not rotated. Later a high temperature camera was adapted for use at temperatures up to 1400 °C on the Norelco unit utilizing both solid and powdered samples. Unless otherwise noted, all X-ray patterns were made with a chromium tube and a vanadium filter. Further-

Jan 1, 1952

The visitors to the October meeting will be given opportunity to visit the coal fields in Illinois, adjacent to St. Louis, the steam-shovel operations near Pittsburgh, Kan., and the Oklahoma oil fields. The coal mines of Illinois, Missouri, Kansas, Oklahoma and Arkansas furnish fuel over all of the central region of the country. Especially at this time, this district is of importance because of the necessity of producing enormous quantities to meet the country&apos;s demand. Some of the mines produce as much as 5,500 tons in 8 hr., and. the total output of Illinois, alone, in 1916, was 63,000,000 tons. Visitors may see elaborate underground electric tram systems, large underground machine repair shops, surface plants equipped for rapid loading, and some of the most modern coal-washing installations. The conditions for mining here are somewhat simpler than in the east.

Jan 8, 1917

By Bryan J. Travis, Thomas L. Cook

INTRODUCTION Our growing concern for adequate and secure sources of energy and minerals has stimulated vigorous exploration for new sources, research toward a better understanding of geological processes, and development of new extraction technologies. The need for control, or at least prediction, of subsurface fluid flow is important for many of these technologies for example: primary, secondary and tertiary recovery of oil; ground water and waste management; in-situ fossil energy extraction (oil shale, coal, tar sands); and solution mining of uranium, copper and other minerals. These technologies, especially the last two, are characterized by highly complex systems. A partial list of the physical processes occurring would include flow in porous/fractured media, multi-phase and multi-component flow with heat transport, chemically active fluids and soils, tracers, diffusion and dispersion, fracturing and dissolution. A great deal of understanding of how these processes behave and interact can be obtained from models. MODELS Theoretical models are valuable because they: 1) provide a frame of reference for interpreting results of laboratory and field experiments; 2) once validated by experiments, allow a variety of geometries, injection/production strategies, etc., to be examined (at relatively low cost) for efficiency and stability; 3) can provide guidance to the design of experiments and field operations. Most models are based on the fundamental principles of mass, momentum and energy balance. But from this starting point, many paths can be taken. For example, there is the theory of Payatakes (1973) which concentrates on the microscale dynamics. In this approach, the rock or soil matrix is represented by a complex of characteristic channels (such as periodically constricted smooth tubes). Detail of flow within the characteristic channel is calculated very accurately. A difficulty with this model is that description of a representative channel can require several parameters which may not be easily measured. Also, it is not clear how the channels can be combined practically to model a large scale flow. Another type of model is the "global" one described by Bear (1972). Here, the continuum equations for conservation of mass, momentum and energy are averaged over a distribution of pore channels, resulting in a set of conservation equations in which the small scale structure of the medium is replaced by quantities such as porosity, permeability, dispersion coefficients and tortuosity. This approach allows computation of large scale flows. However, additional constitutive equations are needed which relate averaged quantities such as permeability to observables such as local saturation, particle size distributions, and others. An important difference between models is the way they handle the momentum equation. Payatakes&apos; model solves the full equation. In others, it is replaced by a simpler relation such as Darcy&apos;s law (valid for slow flow rates) or by Forchheimer&apos;s equation which extends Darcy&apos;s law to higher flow rates. These simple relations can nevertheless match a great deal of experimental data (Dullien 1975). The permeability term which appears in Darcy&apos;s law and in Forchheimer&apos;s expression has been related to other quantities such as porosity and particle surface area. The Kozeny-Carmen equation is a well-known example, valid for some ranges of porosity and particle sizes and for some materials. Several other semi-theoretical, semi-empirical formulations have been devised, none of which are entirely satisfactory. One goal of researchers has been the ability to predict permeability of a porous material from basic measurable quantities such as grain size distributions without recourse to adjustable parameters. This effort has proceeded from consideration of distributions of idealized, non-intersecting channels, to intersecting channels, to consideration of both distributed pore radii and pore neck radii. This last approach has been used successfully to predict permeabilities (ranging over several orders of magnitude) in sandstones (Dullien 1975). Additionally, studies on explicit networks of channels (e.g., Fatt 1956) and percolation theory (e.g., Larson et. al. 1981) have been used to examine interconnectivity effects in porous media with the hope of eventually being able to predict permeability accurately. To be of more than theoretical interest, a model must be compared s controlled laboratory conditions where boundary and initial conditions and relevant material properties can be accurately determined. Also, extraneous forces can be eliminated so that the interactions between processes of interest can be clearly seen and flow models can be vigorously tested. In contrast to the well-defined environment and

Jan 1, 1982

All the TECHNICAL PUBLICATIONS and CONTRIBUTIONS published in 1939 are available at Institute headquarters, unless otherwise noted. They are also on file in many public, university and technical libraries and, when so indicated in the list, may be found in the TRANSACTIONS. TECHNICAL PUBLICATIONS in Classes A-Metal Mining, B-Milling and Concen-tration, H-Industrial Minerals, and ;I-Mining Geology are distributed in MINING TECHNOLOGY, which is issued every other month. Technical Publications in Classes C-Iron. and Steel Division, D-Nonferrous Metallurgy and E-Institute of Metals Division are distributed in METALS TECHNOLOGY, which is issued twice quarterly. TECHNICAL PUBLICATIONS in Class G-Petroleum Division are distributed in PETRO-LEUM TECHNOLOGY, which is issued quarterly. TECHNICAL PUBLICATIONS in Classes F-Coal Division, J-Mineral Industry Education Division, K-Mining Administra-tion, and L-Geophysical Methods of Exploration are issued as separate pamphlets. An Institute member is entitled to one copy of any TECHNICAL PUBLICATION or CON-TRIBUTION. Copies of TECHNICAL PUBLICATIONS listed have been mailed to members of the Institute according to their registration by classes. CONTRIBUTIONS and Other TECHNICAL PUBLICATIONS will be sent upon request. A member relay purchase an additional copy of a TECHNICAL PUBLICATION Or a CONTRIBUTION at One cent a page; minimum charge, 25¢. Nonmembers may purchase any CONTRIBUTION or a TECHNICAL PUBLICATION Of the F, J, K, or L classes at the same rate, but the nonmember price per copy for METALS TECHNOLOGY, MINING TECHNOLOGY or PETROLEUM TECHNOLOGY is $1. TECHNICAL PUBLICATIONS (separate pamphlet form), $2 per annum; Canadian and foreign postage 50 cents extra. METALS TECHNOLOGY, $7 per annum; Canadian and foreign postage 50 cents extra (Iron and Steel Division and Institute of Metals Division ferrous and nonferrous papers). MINING TECHNOLOGY, $6 per annum; Canadian and foreign postage 50 cents extra (metal mining, milling and concentration, Industrial Minerals Division, and mining geology papers). PETROLEUM TECHNOLOGY, $4 per annum; Canadian and foreign postage 50 cents extra. Bound volumes have been mailed to members that have requested them, and MINING AND METALLURGY is mailed each month. A member is entitled to one volume a year on his membership and lie may purchase for $2.50 one copy of a volume not already received; additional copies of &apos;the same volume, $5. Nonmembers may pur-chase the volumes listed, at $5 each, plus 60 cents for Canadian or foreign postage. Extra single copies of MINING AND METALLURGY, 25¢ current issue, back numbers 500 each to members; to nonmembers 50¢ current issue and $1 each, back issues. Subscription price to nonmembers and to members for extra copies, $3 per annum plus $1 for Canadian or foreign postage.

Jan 1, 1939

By W. W. Svendsen, J. F. Hoffmeister, W. C. Larson, R. E. Cozad

The paper presents the background, history, and current development of the retractable core bit for the wireline drilling system. Design criteria, concept development, and system design of the retractable bit system are discussed, including laboratory test results.

Jan 1, 1983

By L. D. Godshall

The latest revised edition of Mr. C. A. stetefeldt&apos;s book on the Lixiviation of Silver-Ores, which appeared very recently, contains no mention of the volatilization of silver in chloridizing-roasting—an omission which is the more remarkable in view of the fact that in former editions of the work this important subject was noticed. Moreover, Mr. Stetefeldt has discussed it to some extent in his paper on " The Stetefeldt Furnace," * in which he criticised certain statements made by me before the Colorado Scientific Society in May, 1893, in a paper entitled " A Review of the Russell Process;" ? and Mr. Morse, in his paper on " The Lixiviation of Silver-Ores by the Russell Process at Aspen, Colorado," $ has given statistics showing the loss of silver by volatilization (including the dustloss, which Mr. Morse estimates at not more than 1 per cent.) on more than 30,000 tons of ore roasted, to have been 9.16 per cent. The matter must certainly be deemed important enough to warrant me in returning to it, and offering, with the aid of the figures made public since my first paper, a reply to the criticisms of Mr. Stetefeldt. The passages of my paper which he deemed to be " ques-

Jan 1, 1897

By W. M. McKewan

A large amount of work has been reported in the literature on reduction of cubes, spheres, or regularly shaped particles of iron ore. Previously, it has been difficult to evaluate these data because no equation has been developed that would yield one or more constants for comparison of overall reduction rates. Iron ore in the process of gaseous reduction is a complex system. The reduction takes place through the series Fe2O3-Fe304-Fe0-Fe. Edstrom and Bit-sianesl have reported that the gas-solid type of reaction was found only at the FeO-Fe interface and that the internal reduction proceeded by elementary diffusion of iron. Therefore, during reduction oxygen is essentially removed from the system only at the FeO-Fe interface. Kinetically, it is reasonable to consider iron ore in the process of reduction as a

Jan 1, 1959

By J. E. Johnson

The general construction of blast-furnaces has undergone no radical change in more than a generation. When the old style of masonry construction was replaced by the steel shell, the masonry piers were simultaneously replaced by columns, never lese than 6 and frequently 12 or 16 in number, set under the mantle-ring. These columns were at first unvaryingly made of cast-iron, but in more recent years have frequently been made of structural steel. The furnace itself has recently been the subject of radical changes; in some cases the thin-lined construction has been adopted for the whole furnace, and in other cases it has been adopted for a zone immediately above the bosh, raising the mantle several feet to make this possible, but still the style of construction with columns set immediately under the mantle has been universally followed. In spite of the apparent fixity of this type of construction it is open to grave disadvantages from the operating point of view, which may be briefly outlined as follows: The slope of the bosh and size of the crucible are such as to leave scant room inside the columns for the necessary water-piping, etc. The bustle-pipe must necessarily be outside the columns and the penstocks have to pass between them, with the result that the columns are frequently much in the way when changing the tuyeres or otherwise handling the penstocks. Moreover, the hearth-jacket requires a diameter but little smaller than the circle of the inside of the columns, and as a result the cooling-water ditch for protection against breakouts is exceedingly limited in width. As a consequence of these conditions, when any work requires to be done around the furnace, such as changing a tuyere or working on the cooling-water pipes, the amount of room left between the columns, pen-

Jan 1, 1913

By Philip D. Anderson, Ralph Hultgren

Heat contents of extremely pure iron were measured over the range 300"to 1433"K, using a diphenyl ether calorimeter. Results from three samples containing widely differing impurities agreed with one another and with Previously reported results at higher temperatures (1184 ° to 1809°K) by Olette and Ferrier. From these data a table of heat contents of iron has been Prepared which is believed to be more accurate than those previously available. CP values have been derived which are consistent with these heat contents, with the best experimental Cp data, and with the thermodynamic conditions of equilibrium between bcc and fcc iron. The opinion is expressed that low-temperature extrapolations of presently known Cp values for y-Fe are not reliable. It would seem that the thermodynamic properties of iron, which is by far our most important metal, should have been well established long ago. This is not the case, however. As discussed by Olette and Ferrier,&apos; there is objection to every earlier heat content measurement. While the best true Cp determinations agree well at temperatures below the Curie point, there is wide divergence at higher temperatures. Several investigators have examined available data and attempted to calculate thermodynamic functions for iron that are consistent with the two equilibrium temperatures of bcc and fcc iron. The two primary efforts were those of Austin&apos; in 1930 and Darken and smith3 in 1948. The recommended values differ considerably; integration of Austin&apos;s Cp values leads to a heat content at 1100°K which is 300 cal per g-atom higher than the value recommended by Darken and Smith. The compilation of Fisher4 in 1949 was based on the selection of Austin. In 1956, Weiss and Tauer obtained yet another set of values by resolving Cp values into components due to dilation, lattice vibration, electronic excitation, and magnetism. The magnitude of contribution by each component and its dependence on temperature was estimated by semiempirical means. Their values are not self-consistent in that they do not form smooth curves when plotted vs temperature; moreover, their calculations cannot easily be repeated since they do not give the values of some of the parameters used. Clearly, experimental values for iron were in a most unsatisfactory state. The presently described measurements of the heat content of iron were therefore undertaken, covering temperatures as high as 1433°K. While the work was in progress, the high-temperature (1193" to 1789"K) heat content measurements of Olette and Ferrier&apos; were published; in the region of temperature overlap the present results agree with Olette and Ferrier well within experimental accuracy. It is believed that the present results, combined with those of Olette and Ferrier, provide for the first time a reliable set of heat contents of iron from room temperature to the melting point. From these data, guided by available Cp measurements, it proved possible to derive Cp, entropy, and free energy function values for @-iron from room temperature to the melting point, and for y- iron in the temperature region of its stability. Exhaustive study led to the conclusion that extrapolations of y-iron functions to room temperature were not reliable enough to be useful; hence these have been omitted from the tables. EXPERIMENTAL Materials. Three samples of extremely high purity iron from different sources, containing widely different impurities, were measured. The first of these, designated "Chipman", was kindly supplied by Dr. K. K. Kelley of the U. S. Bureau of Mines from a lot which was made many years ago by Dr. John Chipman of the Massachusetts Institute of Technology. The second, designated6&apos;Teddington", was supplied by the National Physical Laboratory, Teddington, England, from a lot zone-refined by them. The third sample, designated "Irsid", was supplied by the Institute de Recherches de la

Jan 1, 1962