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By J. A. Bailey, J. H. Tundermann

The dihedral angles of the solid-liquid interfaces were measured at various temperatures above the solidus and the interfacial energies calculated when small additions of copper, indium, lithium, magnesium, antimony, and silicon were made to an aluminum alloy containing 3 pct Sn. When the results were compared with those of the Al-Sn alloy some differences were found which could be interpreted in terms of the ability of the added element to enter into solution or form intermetallic compounds with the aluminum and tin. It was shown that in some cases considerable changes in the shape of intergvanular liquid films can be brought about by comparatively small compositional changes in the alloy. DURING the melting or solidification of an alloy a temperature range is usually found where the presence of a liquid phase may be detected at the grain boundaries of a solid. It is believed that the presence of this liquid phase is responsible for hot tearing in castings and welds and hot shortness in the working of some alloys at elevated temperatures. Rosenberg, Flemings, and Taylor1 in a study of the solidification of aluminum castings have indicated the importance of intergranular liquid films and shown that their shape and distribution at the end of solidification effect the hot tearing characteristics of the material. The shape of such intergranular liquid films are determined largely by the ratio between the solid-liquid interfacial energy (yLS) and the grain boundary energy (ySS). A measure of this ratio (yLS/ySS , relative interfacial energy) is the dihedral angle 8. The dihedral angle 0 is related to the relative interfacial energy by the following expression: Rogerson and Borland 2 have also suggested that the shape of the intergranular liquid is an important factor in determining the susceptibility of a material to hot shortness. They showed that on a comparative basis materials having the lowest dihedral angles at a given temperature gave the greatest severity of cracking. They stated that liquid in the form of globules should be less harmful than liquid in the form of extensive films as more intergranular cohesion should be possible. Rogerson and Borlland 2 also showed that the susceptibility of an A1-Sn alloy to hot cracking can be reduced by small additions of cad- mium. It was found that the cadmium gave an increase in the dihedral angle at all temperatures. Ikeuye and smith3 investigated changes in the dihedral angle and relative interfacial energy with temperature for a number of ternary alloys formed when small additions of bismuth, cadmium, copper, lead, and zinc were made to an A1-Sn alloy. They found that in most instances changes in the dihedral angle were caused by compositional changes in the liquid phase; as the composition of the liquid approached that of the solid the dihedral angle decreased. They noted that the addition of a third element which was soluble in both the liquid and solid phases at a given temperature may decrease the dihedral angle (e.g., the addition of copper or zinc) but otherwise the ternary alloys formed exhibited dihedral angles between those of the A1-Sn binary alloy and those of the binary alloy of aluminum with the added element. Dwarakadasa and Krishnan4 investigated the changes in dihedral angle and relative interfacial energy with temperature when small additions of magnesium, iron, silicon, manganese, sulfur, cobalt, and silver were made to a copper alloy containing 3 pct Bi. They found that in all cases the added elements gave an increase in the dihedral angle and relative interfacial energy when compared with the values obtained for the simple binary alloy at the same temperature. It was noted that an increase in temperature gave a decrease in dihedral angle and relative interfacial energy in each of the ternary alloys studied. Similar results have been obtained by Ramachandran and Krishnan5 for the addition of small quantities of lead. This paper describes the application of dihedral angle measurement to the determination of the shapes of liquid phases at various temperatures above the solidus when small additions of copper, indium, magnesium, lithium, antimony, and silicon are made to an aluminum alloy containing nominally 3 pct Sn. An attempt is made to correlate the measurements with the relative solubility of the added elements in tin and aluminum. The work was undertaken to provide more data concerning the effects of temperature and composition on the shape of liquid films above the solidus. EXPERIMENTAL PROCEDURE In the present work ternary aluminum alloys containing nominally 3 pct Sn and small additions of high-purity copper, indium, lithium, magnesium, antimony, and silicon were made. The alloys were melted in a graphite crucible under an inert atmosphere of argon and cast into ingots 6 in. long by 0.5 in. diam. The ingots were then cut into rods 1.5 in. long, given a 50 pct cold reduction, and machined into test pieces 0.5 in. long by 0.5 in, diam for heat treatment. The alloy samples were annealed at the various test temperatures between the liquidus and solidus for approxi-

Jan 1, 1967

By Charles M. Brinckerhoff

Everyone -- especially the engineer -- is aware of the great technological and social changes taking place in our world today, We realize that changes have been taking place since man's beginnings on earth, but the element we now face is the speed of change, rather than change itself. Developments in medicine, in transportation, in space exploration, in global communications, and in many other fields, are constantly being made known. These developments are affecting the lives of each of us, although some may appear remote and unrelated to us as individuals. New developments, almost on a daily basis, affect our work as well as our social, religious and educational lives. The effects are immediate and permanent.

Jan 1, 1967

By R. E. Miner, J. K. Jackson, D. F. Gibbons

Internal-friction measurements were made during isothermal aging treatments of 18 pct Ni maraging-steel wires between 420° and 612°C. A sharp initial drop in the internal-friction level was interpreted in terms of a rapid dislocation recovery reaction. The rate of the recovery was found to be independent of temperature. Truncation of the recovery reaction was apparent in those systems that exhibited the rapid age-hardening characteristics of the maraging steels. It is proposed that this initial hardening response is the result of a low activation energy preprecipitation reaction involving molybdenum. A gradual rise in the internal-friction level at longer aging times was associated with the precipitation of a molybdenum-containing precipitate. CONSIDERABLE research effort has recently been devoted to the mechanisms responsible for the high strength and toughness of 18 pct Ni maraging steels. These bcc martensitic alloys are found to harden during aging at temperatures between 400° and 600°C. The aging response is very rapid with more than half the total hardness increase occurring within the first few minutes of aging, Fig. 1. Precipitate particles have been observed in the later stages of aging by a number of investigators.'-' While the identity of the precipitates remains the subject of some controversy, one or more of the intermetallic compounds, Ni3Mo, Ni3Ti, and Fe2Mo, are almost certainly involved. Heterogeneous nucleation of precipitates at dislocations has been noted8 and cobalt is believed to enhance the formation of fine, homogeneously distributed particles by lowering the solubility of the alloying elements in the martensitic matrix.3,7 Transmission electron microscopy studies of the initial hardening behavior have not been fruitful. Strengthening mechanisms based on atomic ordering have not been generally supported by X-ray and neutron-diffraction experiments.9 In the present investigation, the aging reaction was studied using isothermal-aging internal-friction measurements. The marked sensitivity of internal friction to short-range diffusion and precipitation processes has provided a convenient tool for the elucidation of the strengthening mechanisms operative in the maraging steels. EXPERIMENTAL PROCEDURE An upright torsion pendulum was used to measure the internal friction of several maraging steels during isothermal aging. The pendulum was placed in an atmosphere of helium at a pressure slightly less than atmospheric. To permit measurement of internal friction during the first minutes of aging, the specimens were rapidly heated by passing a current through them in a manner similar to that described by Ang and Wert.10 Thermal gradients in the specimen were largely eliminated by using specially designed specimen grips11 which produced temperature variations of less than 1 pct over 90 pct of the specimen length and less than 3 pct over the entire length at aging temperatures up to 620°C. A proportioning strip-chart program controller was employed to maintain constant specimen temperature during treatments of up to 36 hr duration. A number of vacuum-melted laboratory heats having compositions near that of a typical commercial 18Ni-7Co-5Mo-0.4Ti alloy were investigated. The amount of cobalt was varied from 0 to 7 wt pct in five of the heats. Either molybdenum or titanium was omitted in the remaining two heats. The alloy desig-

Jan 1, 1967

By J. J. Bailey, R. C. Dean

Dr. Maurer has reviewed the large and confused field of rock mechanics and drilling. We have focused our attention on advance drilling and the disengagement of rock. To understand drilling in greater detail is certainly desirable, but such understanding does not necessarily hold any certain promise of near-term practical advancement. In the longer term, it is probably essential. Present work on drilling and our understanding of drilling falls roughly into three separate classes (and, indeed, these are in no way peculiar to drilling): 1) we have knowledge of certain (scientific) topics which seem to be relevant to the process, 2) we have knowledge of the drilling process in both qualitative and quantitative terms from observation of the actual process, and 3) we have certain modeling procedures, by which we bridge the gap between these two previous areas. The usefulness of our scientific knowledge depends critically upon this last item. In all our following remarks we shall consider only those problems of drilling and the disengagement of rock in which the rock behavior is essentially brittle. Let us start by examining some of the problems of constructing an even moderately detailed theoretical model of the drilling process in the small. The prospects of any near-term success in that direction seem extremely meagre; nor is it clear that any great advancement in the practical art of drilling is even likely to result from the construction of such a detailed model. On the other hand, as we shall suggest later, considera-

Jan 1, 1967

By John A. Reeves

The Coal Creek Preparation Plant is the coal cleaning facility of Mid-Continent Coal and Coke Company. Located three miles west of Redstone, Colorado, and at an elevation of 8,040 feet the preparation plant cleans coal produced at the company's Dutch Creek Mine and L. S. Wood Mine. (See Fig.1.) Current production is at the rate of 2500 tons per day clean coal. Plant capacity is rated 350 TPH raw coal. Reject rates vary with mining conditions from 8% to 25%. Factors which influenced the design of the coal cleaning facility were the characteristics of the coal, the location in a tourist oriented resort area, and the extreme winters of the area. Lack of areas suitable for settling ponds and the necessity of keeping effluent waters out of the fishing streams dictated a closed circuit plant. Severe winter conditions, which last six to seven months out of the year and temperatures which have dropped to 40° F. below zero on occasions demanded that the plant be totally insulated and enclosed indoors.

Jan 1, 1967

By H. I. Aaronson, H. A. Domian

ELectvon-probe analgsis has been used to in7:estigatr the partition ot alloying- elements between aus-tenite and proeutectoid ferrite (or the Jerritic component of bainite) in high-purity Fe-C-X alloys, lsuully at tzco levels of carbon content fca 0.1 and 0.4 pct in ntost steels) at temperatures between the M, and the Ae3 in Si, mn, Ni, mo, Co, Al, Cr, Cu, and PI steels. No partition ous found during the early stages of transformation at any temperature studied in the Si, ,mo. Co, Al, Cr, and Cu steels. Partition did take place, Jrowel'er, in Ihe Mn, ATi, and Pt steels, occurring in lewtperature. regions below the Ae3 of ca 130°, 65", UNDERSTANDING the mechanisms through which alloying elements influence the kinetics of austenite decomposition reactions which proceed by nucleation and 35c respectively. A break was discovered in the TTT curve for the initiation oj the proeutectoid ferrite reaction in the latter steels at the temperature at which partition began. The alloy content in ferrite at the a:y bondavy remained at constart lecels, shown experimentally to be significantly above those corresponding to eqiilib+iu??l, e'en at the longest reaction times investigated (ca 1o6sec). The partition and the TTT curve observations foere rationalized on the basis of the thermodynamic treatment developed in an accompany ing paper. and diffusional growth has been a major research objective of physical metallurgy since the latter part of the 19th century. The measurements made on the dif-fusivities of carbon and of substitutional alloying elements in austenite during the 1930's and 1940's seemed to provide a useful clue as to the nature of these mechanisms. These measurements showed that the diffu-sivity of carbon is several orders of magnitude higher than that of the alloying elements at a given tempera-

Jan 1, 1967

By G. R. Love, M. L. Picklesirner

THE use of color adds a new beauty, power, and versatility to metallography. This has been amply demonstrated in a number of public exhibits and on the walls of corporate, government, and university metallographic laboratories around the world. Indeed, in a number of cases, the color not only is of esthetic value but is scientifically essential to the competent examination of particular samples and systems. Optical strain analysis,' determination of true grain size in U-A1 alloys: phase identification in Nb-base alloys,3 analysis of transformation rates in heat-treated Nb-Zr alloys,4 measurement of solidification segregation in cast Nb-Zr alloys,' study of the intermediate phases in Nb/Sn diffusion couples,6 investigation of the oxidation kinetics at various surface orientations in single crystals,7'8 and a number of other research efforts9'10 would have been vastly more difficult without the extra clarity and distinction introduced by color—either the colors resulting from particular polarized light techniques or the interference colors obtained by oxidation. It is unfortunate that the beauty of colored micro-structures cannot be shared more widely, but the economics of publishing a technical magazine apparently prohibits color plates except under extraordinary circumstances. It is doubly unfortunate that no convenient, general method exists for communicating the information available in colored microstructures to the scientific community. True, in some instances the color changes observed are dramatic enough that direct black and white photography is adequate. In photoelastic stress analysis, several orders of interference fringes may be produced and it is frequently desirable to suppress the color effects (use monochromatic light) to simplify interpretation. On the other hand, relatively minute color variations may be readily detectable by eye, be of considerable assistance in interpreting a structure, and yet be enormously difficult to reduce to an unambiguous black and white print. In order to illustrate a possible compromise or solution to the above problems, we wish to show three black and white photographs of the same region of an Nb/Sn diffusion couple whose interpretation depends heavily upon use of color techniques. These micro-structures were obtained from a section through a rod consisting of commercial-purity niobium tubing filled with 99.995 pct Sn (melt-filled in 10"6 Torr vacuum). The composite rod, measuring 500 mm long, was bent into a hairpin shape and inserted into water-cooled copper grips in a vacuum high-temperature furnace. The rod was outgassed for 2 hr at a furnace temperature of 800°C and was further heated by self-resistance using a 2.2-kva ac power supply. The rod was raised to 1910°C over a 4+-hr period, held for 15 min, slow-cooled to 1500°C over a -hr period, and free-cooled to room temperature (all temperatures were measured with W5Re/W26Re thermocouple). Throughout the heat treatment the ambient pressure was kept below 8 x lo-' Torr. Metallographic preparation of the sample was completely conventional except that it was necessary to extend the grinding steps to remove damage in the brittle NbsSn phase introduced by sectioning. No satisfactory chemical or electrochemical etch has been found for these diffusion couples; of those which have been tried, any that attack the niobium-rich phases at all attack the tin-rich phases disastrously. However, the final polishing steps did produce a slight relief effect and this, coupled with anodizing, yielded excellent clarity in the microstructures for direct observation. The anodizing voltage was chosen to give maximum change in color per unit change in composition. In this case, indeed normally, this maximum sensitivity occurred in the blue-to-red color range. The pure niobium tube wall anodized to a relatively bright blue

Jan 1, 1967

By W. M. Aubrey

The use of solid fuel in shaft furnaces to indurate iron ore pellets was originally considered a necessary evil, which the industry worked long and hard to eliminate. Since then changes have taken place in furnace design and operating practices that have led us to our suggestion that solid fuel additions could again be used. In essence, what has happened is that the developments which made it possible to operate without solid fuel have also created new operating conditions favorable to the effective use of solid fuel. Because these new conditions* were brought about in part by the desire to eliminate solid fuel and because the development was a gradual one, the industry failed to reassess its position and for years neglected the possibility of returning to solid fuel.

Jan 1, 1967

By R. F. Neider, W. R. Bain

"Expanding upon one aspect of a recent paper on ""Fluid Column Roasting at Sherbrooke Metallurgical Co. Ltd.,"" the present paper deals with the operation of the fluid column process to achieve substantial elimination of cadmium and lead during the roasting of pelletized zinc concentrates. Designed to meet the need for additional feed for Matthiessen and Regeler Zinc Company's vertical retort zinc smelter in West Virginia, without recourse to a sintering operation, the plant is capable of simultaneously attaining very low lead and cadmium levels on demand, through operation in the manner described. Fluidizing air admitted via the wind box is supplemented by natural gas admitted via a tuyere bank 15 ins. above the hearth, in quantities adjusted to maintain a reducing atmosphere within the interstices of the bed. In addition, careful attention is paid to bed temperatures, which run from 1,080° to 1,100°C. Under these reducing conditions, 90 per cent of the cadmium and 92 per cent of the lead in the feed are eliminated, the sulphate sulphur content is decreased by 0.5 per cent, sulphide sulphur is held at 0.6 to 0.08 per cent, and the zinc content correspondingly in-creases. The fuel value of the natural gas is recovered as extra steam, which carries a credit. There are some added difficulties with fume accretions, gas conditioning and gas -cleaning, some of which have yet to be overcome."

Jan 1, 1967

By W. H. Engelmann

The electrokinetic (zeta) potentials of a charcoal granite in an aluminum chloride (AlCl3) solution and in an oleylanunonium acetate (C18H35NH3+ -OCOCH3) solution have been correlated with the specific damping values as measured by the pendulum sclerometer. This investigation shows that the pendulum specific damping attains a minimum at the isoelectric point for the charcoal granite-aluminum chloride and charcoal granite-oleylammonium acetate systems, and thus indicates that the penetration of the diamond points is a maximum at the isoelectric point.

Jan 1, 1967

By M. R. Louthan, C. L. Angerman

In polycrystalline Zircaloy-2 the orientation of zirconium hydride precipitates is influenced by an applied stress during hydride precipitation; hydride platelets are oriented nearly parallel to a compres-sive stress and perpendicular to a tensile tress. 1,2 A similar effect has been observed in the Ti-H system, where precipitation of the low-density hydride platelets occurred on habit planes made energetically favorable by the application of stress. 3 Recently, stress activation of hydride habit planes in zirconium and Zircaloy-4 was also demonstrated. The hydrides precipitated on {101l), {112l} and (2131) planes in both zirconium and Zircaloy-4; however, no platelets were found near the prism-plane positions in the Zircaloy-4 samples. Investigations at the Savannah River Laboratory, using polycrystalline Zirc_aloy-2 samples, have confirmed the (101l) and (1121) habit planes but also showed that the prism planes were active hydride habit planes. Using single-surface stereographic analysis and back-reflection Laue techniques, most of the previously reported habit planes for a zirconium were observed.4"1 and one additional plane, the (1013) plane, was noted, Table I. All the habit planes observed had the form (101l) or { 112l) indicating that these planes are the habit planes for hydride precipitation in poly-crystalline Zircaloy-2. The specimens used in these studies were cut from large-grained weld areas of seam-welded tubing and were hydrided in either a static steam autoclave at 400°C and 1500 psig or in a modified Sieverts apparatus at 400°C.

Jan 1, 1967

By R. V. Higgins

The Bureau of Mines investigated the use of electronic computers for obtaining more information about relative permeabilities of reservoir rock to oil and water. It was found that there are many possible combinations of relative permeability curves that will result in virtually the same recovery versus injection) but they require different times and rates to recover the oil even with different mobility ratios. Permeability curves obtained by the use of non-viscous oil and employed for calculating the waterfloods of viscous oils can lead to serious inaccuracies. For viscous oils) the wettability characteristics in the middle portion of the permeability curve affect recovery nearly as much as other portions of the curve; this) however) is not true for non-viscous oils in water-wet reservoir rock.

Jan 1, 1967

By P. G. Barnard

The Bureau of Mines investigated the effects of various additions of rare-earth metals or rare-earth oxides on the mechanical properties of cast and wrought plain-carbon steels. Rare-earth metals, as misch metal, were added to medium-carbon steel in amounts to 0.70 weight-percent; rare-earth oxides, as a commercial mixture, were added in amounts to 1.50 weight-percent. The melting and casting of conditioned steels were done in a vacuum-induction furnace, to avoid formation of oxides from the melting atmosphere and to pro-vide better control over chemical composition. At room temperature, data for tensile strength, yield strength, elongation, and hardness of cast and wrought steels were obtained by standard testing equipment and procedures. Impact tests were conducted on as-cast steel specimens. The greatest amount of tensile ductility and impact strength was obtained in as-cast steel with 0.50 to 0.70 weight-percent misch metal additions. No significant improvement on mechanical properties was indicated in wrought steels containing rare-earth metal additions in the range from 0.10 to 0.70 weight-percent. In general, the rare-earth oxide additions up to 1.50 weight-percent had little effect on the tensile properties of steel in the cast, wrought and annealed, or wrought and normalized condition.

Jan 1, 1967

By Donald W. Petrasek

The effects of selected alloying elements on the elevated-temperature tensile properties of copper alloy -tungsten fiber reinforced composites were invcstigated. A cornparison of the elevated-temperature tensile properties of copper alloy - tungsten fiber reinforced composites, representing soluble systems. was made with copper - tungsten fiber reinforced composites, representing a mutually insoluble system. A linear relation between tensile strength and volume percent fiber content existed at elevated temperatures for all the systenzs investigated. The copper alloy composites were weaker in tension at high volume percent fiber contents than copper composites in which alloying with the fiber did not occur. The tensile strength of the alloyed tungsten fiber decreased with increasing penetration of the alloying element into Ihe tungsten fiber. THE technique of combining strong fibers with relatively weak matrix materials so that the fibers are load-carrying members has been utilized for many years in the reinforcement of plastics with glass fibers. This type of strengthening is currently being extended to include the reinforcement of metals with metallic fibers. Investigations of the room-temperature tensile properties of metal-fiber-reinforced metallic composites have been numerous,'-" but the study of tensile properties at elevated temperatures has been limited. In previous work done at the Lewis Research Center' composites consisting of mutually insoluble constituents were investigated. Composites were made of copper reinforced with uniaxially oriented tungsten fibers. The stress-strain behavior and tensile properties of the composites were related to the tensile properties of the base materials. The tensile strength of the composite was directly proportional to the volume percent of tungsten fiber present, and the full strength of the fiber was realized. Few metal fiber - metal matrix systems exist that are mutually insoluble, and those that do exist are not generally practical. An extension of this work was an

Jan 1, 1967

By A. C. A. Howe, J. C. Rowntree

"The Bernie Lake pegmatite near Lac Du Bonnet in southern Manitoba is a complexly zoned pegmatite containing several lithium-bearing units in addition to the western world's largest known reserve of cesium. The pegmatite forms a flat-lying ellipsoidal body within an east-west-trending Precambrian amphibolite. The pegmatite enclosed by this vertically schistose amphibolite lies near the eastern tip of a granitic intrusive. The relationship of this intrusive to the pegmatite is obscured by Bernie lake. To date, the pegmatite body has been delineated aver an area of approximately 80 acres; it attains a maximum thickness of 280 feet. Several distinct zones, including three assemblages of economic importance, comprise the pegmatite itself. The combined spodumene and lepidolite assemblages provide a recoverable defined lithium ore reserve of almost 5 million tons averaging more than 2 per cent lithium oxide. The recoverable cesium ore of the pollucite assemblage provides 300,000 tons averaging more than 20 per cent cesium oxide; this represents more than half of the western world's pollucite reserve. The Bernie Lake pegmatite deposit, owned by Chemalloy Minerals Limited, is well located with respect to the growing United States markets, and its reserves of cesium are large enough to enable it, under favourable economic circumstances, to become the major producer of this metal in North America."

Jan 1, 1967

By D. Cox, M. J. Duggin, L. Zwell

The carbides of approximate composition and Mn have been studied using X-ray diffraction techniques. Those carbides of the type (Fe,Aln)zC ave isostructural with cementite. The cell pararmeters a and c have minimum values at approximately 10 at. pd substitution of manganese for iron; no satisfactory explanation has yet been found for this phenomenon. The carbide fFeMn4)C has a monoclinic unit cell whose dimensions are close to those of ,11,15Cz A neu-troip-dij~ractiot~ study of (F'eAlrz4)C~ reveals that, like MnsCZ, it is isostructural with Pd5Bz. The iron and manganese atoms occupy the palladium atom sites, while the carbon atoms were found to have the same atomic coordinates as the hovon atoms. A neutrorr-diffraction study of indicates that the carbon-atom positions are very close to those occupied in (Fez.,ll/lr~,.3)C. In both carbides studied, tlre iron and manganese atomzs were found to be essentially randomly distributed, although, in the case of (Fe,.811fn1.2)C, it is possible that there may be a slight preference of manganese atoms for- the general (d) positions and a corresponding slight preference of iron atoms for the special (c) positions. It has been found that a complete range of solid solution exists between Fe3C and Mn3C at 1050°C,I although Mn3C becomes unstable when the temperature is reduced to 95O0C,' and can only be retained by rapid quenching. It is also known that a complete range of solid solution exists from Fe5Cz to M~SC~,~ although the stability range of carbides of the type (Fe,Mn)sCz as a function of the relative proportions of iron and manganese is not known. X-ray examinations of Oh-man's carbide3 and Spiegeleisenkristall,~ which have the approximate compositions (Fe3.67Mnl.33)C2 and (Fe3-,Mn,)C, where x lies between 0.4 and 1, respectively, have been made. The following carbides have also been studied: ] The lattice parameters determined during these investigations are listed in Table I. It is seen that carbides of the type (Fe,Mn)sCz have a monoclinic unit cell while carbides of the type (Fe,Mn)3C have an orthorhombic unit cell. It is evident that the variation of lattice parameters with manganese content is not linear for carbides of the type (Fe,Mn)3C. The coordinates of the atoms in (Fe2.7Mno.3)C have recently been determined by single-crystal analysis., The fractional atomic coordinates have been shown by Fasiska and jeffrey to be in good agreement withj those deduced from an earlier analysis of Fe3C by Lipson and etch.' However, it was impossible to determine whether iron and manganese atoms occupied ordered positions because of the small difference between the atomic scattering factors of iron and manganese. The atomic positions in Mn5Cz (Refs. 8 and 9) and Fe5C2 (Refs. 7 and 8) have been obtained only by comparisons made with the isostructural compounds P~SB~.' Since X-ray diffraction techniques were used in these investigations, accurate positioning of the carbon atoms, which have a low atomic scattering factor, was difficult. No attempt has been made to determine the atomic positions in the other carbides previously studied. It was felt that an investigation of the lattice parameters of a number of intermediate carbides of the types (Fe,Mn)sCZ and (Fe,Mn)& would be of interest. It seemed likely that a neutron-diffract ion study of such carbides would indicate whether ordering occurred between the iron and manganese atoms because of the large difference between the neutron-scattering cross sections of iron and manganese. It also seemed probable that such an investigation would provide a determination of the atomic coordinates of the carbon atoms. I) EXPERIMENTAL DETAILS Specimens, each weighing approximately 20 g, were carefully prepared according to the following proportions: The components were 500-mesh powders of 99.995 pct purity iron and spectroscopically pure carbon and a 200-mesh powder of 99.995 pct purity manganese. The component powders were intimately mixed by prolonged shaking, then each specimen was inserted into a spot-welded cylindrical container of tantalum foil, whose end was closed but not sealed. Each specimen in its envelope was then sintered at 1050° C for 24 hr in a thin-walled evacuated quartz capsule, such a time having been previously found sufficient for equilibrium to be attained.' Each specimen was then quenched in order to attempt to retain the high-temperature phase, as the literature indicates that transformations may occur on cooling. Debye-Scherrer X-ray photographs were taken of each specimen using a 114.6-mm-diam camera, Fig. 1, patterns 2 to 6. The exposure time was 6 hr using filtered iron radiation at a tube voltage of 40 kv and a tube current of 12 ma.

Jan 1, 1967

By Walter E. Kramer

The advantages derived from the use of pellet burdens in blast furnaces are so great, that hematite ores are being converted into pellets in greater quantities each year. The conversion of these ores into pellets appears on the surface to be relatively simple. In reality, this is not so. Serious difficulties are encountered in drying these pellets that do not exist in the drying of taconite concentrate pellets. The ores that present problems are goethite and earthy hematites. Green pellets prepared from these ores have very law shock temperatures, 200-600° F. The shock temperature of a green pellet according to our definition is the highest initial temperature to which a green pellet may be exposed without suffering decrepitation. Decrepitation may involve spalling, fracturing or total disintegration. The poor shock properties of these green pellets result from the inability of the vaporized water to escape freely and easily as it is formed with¬out affecting the integrity of the pellet. As a consequence, the pellets must be carefully dried prior to induration. This careful treatment is costly. The slow drying process restricts productivity and requires larger furnaces than desired. The use of an additive to elevate the shock temperature of the green pellets would increase productivity. Bentonite is used in some pellet plants to improve balling but it raises the shock temperature only slightly. Nalco became interested in the shock temperature problem because of its activity in the development of organic pelletizing aids for taconite concentrates. The findings reported here are an outgrowth of our experimental work on the development of shock temperature additives.

Jan 1, 1967

By M. S. Rashid, C. J. Altstetter

Allotropic transformations in cerium have been studied by dilatometric, resistometric, X-ray diffraction, and metallographic techniques. The dilatometric study indicated that, on cooling below O°C, the high-temperature fcc phase, y, transforms partly to the hexagonal phase, ß, and, on further cooling, to the collapsed fcc phase, a. The amount of $ phase present at room temperature is increased by repeated cycling through the a-y transformation. It has been shown metallograPhically that the y-ß transformation has many characteristics of a martensitic transformation. In contrast to the y-ß transformation the ?-a transformation does not give the manifestation of a shear transformation. Small cellular ? domains of random shape and size collapse to a in a short time with no apparent coordination with neighboring domains. The considerable confusion in the literature over the existence of more than one high-temperature fcc phase is discussed. Two such phases have been reported in the literature and an attempt is made in this study to clarify the situation. Twelve fcc and two hcp structures have been shown to be easily reproduced or eliminated. It is proposed that the two "additional" allotropes reported in the literature and fourteen of the phases detected here are not allotropes of cerium but are due to contamination. CERIUM exists in several allotropic forms, but there is some disagreement over what the forms are. Furthermore, the conditions favoring the presence of a particular allotrope and the nature of the transformations from one form to another are uncertain. The objectives of this research were 1) to ascertain the allotropic forms of cerium, 2) to establish the conditions under which the allotropes exist, 3) to study the effects of annealing and thermal cycling on the allotropic transformations, and 4) to study the transformation mechanisms. Dilatometric, resistometric, metallographic, and X-ray diffraction techniques were employed. The form of cerium commonly found at room temperature is fcc and is designated ?. A complex hexagonal phase, 8, forms when y is cooled to slightly below room temperature. At still lower temperatures the y fcc structure transforms to an fcc form with a much smaller lattice parameter, termed a cerium. A bcc form, 6, which exists just below the melting point (800°C), will not be considered further in this work. There is a substantial body of experimental evidence (reviewed by Gschneidnerl) which favors the acceptance of these four allotropes, though some investigators have tried unsuccessfully to observe the ß hexagonal form.'-' There is disagreement, however, over the phase-transformation temperatures, due, in part, to broad hysteresis and overlapping of the transformations between the a, ß, and ? forms. The transformations are also sensitive to prior thermal and mechanical treatment. The differing purity of cerium used by different investigators is undoubtedly a factor. Cerium is difficult to separate from other elements and is quite reactive, igniting spontaneously when it is filed in air. The highest purity of cerium to date is reported to contain several hundred parts per million by weight of impurities, and early investigations were carried out on cerium containing several percent of impurities. There have been reports of more than one fcc allotrope at room temperature. Gschneidner, Elliott, and McDonald5 obtained diffraction patterns of an fcc phase with a lattice parameter about 1 pct less than that of the ? phase, instead of the y phase, on slowly cooling cerium filings from 23° to -198°C and warming them back to room temperature. However, when the sample was heated to 447°C and cooled to room temperature it consisted of only the ? phase. They have designated this new fcc phase "a-? intermediate", and say it is quite sensitive to impurities. After prolonged high-temperature treatment of a powder specimen, Weiner and Raynor2 obtained a diffraction pattern of an fcc phase of lattice parameter about 1 pct less than the ? phase. This they called the y' phase. It could not be reconverted to the y phase and is claimed to be different from the a-? intermediate phase.5,6 Dialer and Rothe3 reported two fcc phases* after cycling their powder specimens between room temperature and -192°C. Gschneidner, Elliott, and McDonald5 suggested that one of the fcc structures obtained by Dialer and Rothe was equivalent to their "a-? intermediate" phase. Table I presents some pertinent data on the proposed allotropes. For the ?(fcc)-ß(hexagonal) transformation

Jan 1, 1967

By Jean Dugas, Roger Sirois

The Mineral Deposits Service of the Quebec Department of Natural Resources is engaged in the preparation of metallogenic maps as a contribution to the Canadian Sub-Committee of the Metallogenic Map of North America. The preliminary work is being done on large-scale maps. The main objective is to clearly represent information on ore deposits in a suggestive way. The design of the legend to meet these requirements is discussed. As these maps are still only descriptive, a further step will be the interpretation of data into metallogenic maps with Jess emphasis on the individual deposits and more on the metallogenic factors. Both types of map should prove useful in the search for ore deposits; the first by providing at once a large amount of information, the second by suggesting the ore controls.

Jan 1, 1967

By F. Harold Weber

On July 13, 1967 the San Bernardino County Planning Commission approved publicly a request by American Smelting and Refining Company for a zone variance to conduct a silver mining and milling operation in the Calico district, southern California, Coincidentally, on July 14 the U.S. Treasury halted its sales of silver, and the U.S. free market price quoted rose immediately from $1.30 to $1.77 per ounce. In its request to the commission Asarco stated that about 13,500 to 15,000 tons of rock would be moved daily by surface mining, including 7,000 tons of ore. The ore would be crushed to minus three-quarters inches and the silver recovered "by a chemical process." The grade of the ore was not given, but the company said that it might also recover barite as a byproduct, The operation would employ 150-160 people. Additional activity in the district includes exploration programs by Superior Oil Company and Calico Silver Mines, Ltd. History and production: In retrospect, as the price of silver began to rise in 1961 from 91 cents an ounce, and as Asarco began its exploration program in late 1964, a new era for an old bonanza silver district would seem to have begun. The Calico district has been mined for silver only on a very, very small scale since 1882 to 1896, when an estimated $12 to $20 million (perhaps 15 to 20 million troy ounces) of that metal was produced from the 50-odd mines of the district and vicinity. These mines include the Silver King, Oriental, Waterloo, Garfield, Odessa and Waterman (which is about 8 miles west of the district). Much smaller-valued amounts of barite, gold, lead, and copper also have been produced from the ore deposits of the district; and from 1884 to 1907 the region yielded about $9 million worth of borate minerals.

Jan 1, 1967