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By H. C. Carpenter

This literature study of methods for desulfurizing residual fuel oil was conducted by the Bureau of Mines at the request of the Department of Health, Education, and Welfare. The sulfur compounds in residual fuels are believed to consist chiefly of condensed thiophenes and other polycyclic sulfur compounds. Hydrodesulfurization appears to be the most promising method for desulfurizing these oils and is the only method applicable to all types of sulfur compounds. There are indications in the literature that hydrodesulfurization without hydrocracking of residual oils may require higher pressures than used in present desulfurization processes, but no cost data and little experimental data are available on the higher pressure operation. Literature proposals for hydrogenating residual oils and heavy crude oils are exclusively for hydrocracking the oils to lower boiling products with accompanying partial desulfurization of the residual fuel fraction. Costs of the hydrocracking operations appear the closest available to probable costs of hydrodesulfurizing the oils, and have been reported (in 1955 to 1957) as $500 to $840 investment cost per daily barrel of capacity, with total operating costs of 70 cents to $1.10 per barrel.

Jan 1, 1963

By L. Adler

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

Jan 1, 1963

By J. G. Faller, L. P. Skolnick

The distribution of cobalt and vanadium over non-equivalent crystallographic sites in C14-type Zr(VCo), alloys has been investigated. An anomalous X-ray scattering technique developed by Skolnick, Kondo. and lavine7 by which the separation in the scattering factors of two similar atoms can be enhanced was employed. Six alloys spanning the pseudobinary section ZrV1.6Co0.4-ZrVO.6CO1.4 at 10pct steps showed a nonrandom compositionally dependent distribution. Specifically, at high vanadium content cobalt preferentially occupied sites of type (6h) and vanadium, sites of type (2a; at low vanadium content the reverse was observed. In addition to the distribution fraction the structural parameters x and z were obtained. There was no significant deviation of these parameters from those obtained in the ideal C14 structure. Certain suggestions are made to account for the observed nonrandomness in the distribution of atoms on the two types of sites. INTERMETALLIC compounds of formula AB2 iso-morphous with MgCu2, MgZn2, and MgNi2 are known as Laves phases. Because Laves phases exhibit high symmetry and coordination numbers, the highest possible for an AB2-type compound,1 they are among the most frequently observed compounds in nature. In recent years interest has centered about the purely transition metal Laves phases2-' in efforts to understand the function of atomic size and electronic structure in the formation of these compounds. It has been observed that pseudobinary Laves phase systems often show a variation of structure across the phase diagram. Such a system is the ZrV2-ZrCo2 in which the structure varies from cubic MgCu2 to hexagonal MgZn2 to cubic MgCu2.4 Some understanding about the conditions under which the second modification is stable can perhaps be gained by studying the distribution of cobalt and vanadium atoms on lattice sites in the MgZn2 modification of the system ZrV2-ZrCo2. In both the MgZn2 and MgNi2-types there exist nonequivalent positions open to occupancy by the B element, whereas in the MgCu2 prototype all sites are equivalent. Skolnick, Kondo, and La-vine7 have developed an anomalous scattering technique suitable for this type of investigation. Whereas the influence of size on the formation of a Laves phase is well recognized, no substantial evidence has been put forth in support of the size ratio dependence of a particular prototype. Berry and Raynor8 suggested that RA /RB ratio does indeed affect the type of structure that is chosen, MgZn2 compounds tending to cluster about 1.225 while MgCu2 compounds were found at larger deviations from this ratio. Dwight,3 however, from a study of 164 Laves phases does not believe this generalization to be justified. Electronic effects are certain to play a part in the stability of Laves phases in general and in the choice of a structure type in particular. For example, size along would favor the formation of Laves compounds of Ti, Zr, Hf, Ta, or Nb as the A element with nickel or copper as the B element. The absence of such is attributed to an unfavorable electron : atom ratio by Elliott and rostoker.4 Early experiments of Laves and witte9 with pseudobinary and pseudoternary systems of the three prototypes established the dependence of crystal structure upon electron: atom ratios. They observed that the MgCu2 structure dissolved elements of higher valency until the electron: atom ratio of =1.8 was reached; the MgZn2 likewise dissolved elements of lower valency replacing zinc. witte,6 from calculations of the electron : atom volumes of Brillouin Zones, obtained limits of stability for the prototypes MgCu2 and MgZn2. Elliott and Rostoker4 used these limits with considerable success in the all-transition element Laves phases they investigated. According to witte,6 compounds between the electron :atom ratios of 1.80 and 2.32 were of the MgZn2 type; those above and below exhibited the MgCu2-type structure. On the basis of these limits and an assumed valency of zirconium based upon the near tetra-valence of titanium, Elliott and Rostoker obtained valencies for the first transition series elements. For the Laves phases with which this investigation is concerned, ZrV2 and ZrCo2, the authors calculated electron :atom ratios of 2.54 and 1.56, respectively. These ratios are for the MgCu2-type structure and straddle the stability band of the MgZn2 modification. One could, therefore, predict that a pseudobinary system ZrV2-ZrCo2 should pass through the MgZn2 modification in traversing the composition diagram from one end to the other. Implicit in this assumption is a smooth change of the electron: atom ratio from 2'54 to 1.56. MOSS10 states that his finding the low temperature structure of ZrCr2 to be C15 instead of C14 alters greatly Elliott's valency of zirconium and hence the assumed valencies of the other metals. Such a quantitative correlation of structure with electron : atom

Jan 1, 1963

By A. C. Rice

Aminopolyacetic acid chelating agents were added to separatory-funnel-scale solvent-extraction systems to determine the effect on separating rare-earth elements. Average values for separation factors between adjacent elements obtained with Primene JM-T2 increase 36 percent when EDTA is added to the aqueous phase. Adding HEDTA or DCTA also improves separation factors for certain rare-earth elements. Percentage of extraction and the separation factors exhibit marked sensitivity to concentrations of amine, chelating agent, and hydrogen ion. The chelating agents improved separation in Primene JM-T, BHDA, and Primene 81-R extraction systems.

Jan 1, 1963

By Ross W. Whipple

Applying geophysical techniques in potential geothermal areas has received: little attention in the United States, though it is widely used and accepted in New Zealand and Italy. In those countries it has been demonstrated that geophysical surveys can be useful in locating new geothermal areas and in directing test drilling programs. Geophysical studies in a thermal region can provide structural information and, if conditions are right directly; locate subsurface hot waters. They can give indications of sub-alluvial rock types and of the thickness of alluvial cover. In certain cases they can be used to estimate the power potential of a hydrothermal system.

Jan 1, 1963

By Lowell Stroud

A windowed-cell phase equilibrium apparatus was used to obtain equilibrium vapor- liquid data for a helium-bearing natural gas (Hogback) at temperatures from -100 to -250° F and pressures to 500 psia. Anomalous phase behavior resulting in the formation of two stable liquid phases occurred at tmperatures below -200° F and pressures above 200 psia. A review of the published literature on the occurrence of multiple-liquid phases included in the report indicates that the experimental results with Hogback gas are the first substantiated evidence of a vapor-liquid-liquid equilibria in a helium-containing natural gas.

Jan 1, 1963

By Alfred Wild

The Kraftile Co. plant, Fremont, Alameda County, Calif.--the largest producer of glazed, structural wall units west of the Rocky Mountains-- maintains modern processing facilities to evaluate and blend a wide variety of clays from several sources to produce quality products. The report desribes the prospecting, exploration, and test methods used to locate raw material sources and covers processing methods, cost factors, and trends. Also, the geologic and ceramic factors are considered in a general discussion of the economics, potentials, and requirements of clays as raw materials for ceramic tile manufacturing.

Jan 1, 1963

By W. R. Hansen, F. W. Boulger

Twenty-nine laboratory steels were studied to determine the effects of composition and ferrite grain size on drop-weight and Charpy V-notch transition temperatures. The experimental steels covered the following ranges in composition.. 0.10 to 0.32 pct C, 0.30 to 1.31 pct Mn, 0.02 to 0.43 pct Si, md nil to 0.136 pct acid-soluble Al. Although most of the data were obtained on hot-rolled samples, some plates were heat-treated in order to cover a wider range in ferrite grain size. The experimental data were used for a multiple-correlation analysis conducted with the aid of an electronic computer. The study showed that carbon raises and that manganese, silicon, aluminum, and finer ferrite grains lower both drop-weight and Charpy transition temperatures. Quantitatively, variations in composition and grain size have a more marked effect on V15 Charpy transition temperatures than on the drop-weight transition temperature. Useful correlations were found between transition temperatures in drop-weight tests and those defined by seven different criteria for Charpy tests. Evidence was accumulated that the conditions ordinarily used for drop-weight tests are more severe for 1-1/4-in. -thick plate than for 5/8- to 1-in. -thickplate. PROJECT SR-151, to study quantitatively the effects of metallurgical variables on performance in the drop-weight test, was established by the Ship Structure Committee late in 1958 on recommendation of the National Academy of Sciences, National Research Council. This project was initiated as a result of the increasing use of the drop-weight (nil-ductility) test in predicting the ductile-to-brittle behavior of steel. Qualitative data indicated the drop-weight was not as sensitive to metallurgical variables as the Charpy V-notch test. Furthermore, the available information indicated that the drop-weight test did not show the superiority of killed steels over semikilled steels reflected by Charpy tests. This difference in sensitivity to brittle fracture is considered important because the drop-weight transition temperature has been reported1 to correlate better with service-temperature failures than the V-notch test does at a constant energy level. Therefore, this project was concerned with establishing quantitatively the effects of metallurgical variables in the drop-weight test. For comparison, Charpy V-notch data were obtained for the steels investigated. This paper summarizes the results of the investigation. Most of the steels used for the study were made and processed in the laboratory. However, some tests were also made on commercial killed steels available from Project SR-139 (SSC-141). During the course of the investigation, data were obtained on the effects of carbon, silicon, manganese, and aluminum on transition temperatures of drop-weight and Charpy specimens. In addition, the effects of heat treatment which changed the ferrite grain size and the transition temperatures were also investigated. Finally a few exploratory studies were made on commercial killed steels to evaluate the effects of plate thickness, grain size, and heat treatment on the performance of drop-weight specimens. EXPERIMENTAL PROCEDURES Preparation of Materials. A total of twenty-nine 500-lb induction-furnace heats were made and processed in the laboratory for the investigation. Carbon, manganese, silicon, and aluminum contents were systematically varied. Melting and rolling techniques proven satisfactory in a previous project2 were used as a guide for the current investigation. Composition. The composition of the twenty-nine laboratory heats made for this project are given in Table I. The steels are divided into three groups. The first group consists of ten aluminum-killed steels similar in composition to Class C ship-plate steel. The second group consists of ten semikilled or Class B type steels. In both of these groups the carbon and manganese contents were intentionally varied over a wide range. This wide range in composition was helpful in obtaining quantitative data from a limited number of steels. The primary purposes of these two groups of steels was to determine the effects of carbon, manganese, and deoxidation practice. In addition, one steel in each group (Steels 2-2 and 9-2) were made about 1 year after the start of the program in order to check consistency of melting practice. The third group of nine steels listed in Table I was intended for studies on the effects of silicon and aluminum. In eight of these steels carbon and manganese were held relatively constant at levels of about 0.2 and 0.8 pct, respectively, while silicon and

Jan 1, 1963

By W. Evans, C. E. Ells

The agglomeration of hydrogen in pure aluminum and A1-Mg alloys has been studied through use of hydrogen introduced into the metal by cyclotron proton irradiation. Both the growth and dispersal of the agglomerates have been followed by metal-lographic techniques. During the cyclotron irradiation, agglomeration occurs at temperatures i 100°C for hydrogen concentrations as low as 1 ppm. On heating at elevated temperatures, 300°C to 600°C, intragranular agglomerates first coarsen and then disperse. The agglomerates formed at grain boundaries are much larger than the intragranular agglomerates; with hydrogen concentra- tions > 10 PPm, heating for 1 hr at 500°C results in extensive grain-boundary cracking. The hydrogen agglomerates have been shown to inhibit grain growth, but no inhibition of recrystallization has been observed. The ability of hydrogen to enter aluminum at a free surface, combined with its high-diffusion rate at elevated temperatures, accounts both for growth and dispersal of the agglomerates. Irradiations at elevated temperatures give results consistent with the explanation proposed for agglomerate behavior on post-irradiation heating. 1 HE formation of hydrogen-filled bubbles, or blisters. in aluminum and its alloys has been studied for over' thirty years. The work up to 1952 has been reviewed by Kostron' and since then Ransley and

Jan 1, 1963

By W. Hume-Rothery

RECENT interest has been shown in utilizing solid-state techniques for obtaining large oriented grains in the Alnico Alloys.1-4 Unfortunately, due to the inherent brittleness of these materials it is difficult to introduce sufficient imperfections by deformation to support the nucleation and growth of new, recrystallized grains. As a result, recrystal-lization methods for obtaining large grains, such as the strain-anneal technique, do not appear to be feasible. Steinort et a1.2 used a combination of a thermal gradient and internal strains to obtain large single crystals of Alnico 5 from a poly crystalline casting by annealing at temperatures above 1200°C. It was suggested that the strains were the result of the precipitation of the y phase which exists between -850° and 1200°C. The purpose of the present study was to determine if the grain size of the cast Alnico alloys can be markedly increased by solid state techniques involv-

Jan 1, 1963

By W. H. Herrnstein, J. B. Clark, E. C. Utley, A. J. McEvily

The ratio of the endurance limit (10' cycles) to tensile strength of age-hardened aluminum alloys is approximately 0.3, whereas the ratio for annealed alloys is about 0.5. The lower value for the age-hardened alloys has been associated with the instability of coherent precipitate during cyclic loading, but it has not been definitely established whether this instability is due to overaging or reversion during cyclic loading. The results of the present investigatzon support the reversion viewpoint. In this work specimem of 2024-T4 aluminum alloy were aged for 16 hr at 150°C after cycling for 10 pct of the life at 25.000 psi. These specimens were then tested to failure and exhibzted a marked increase in fatigue life. It is proposed that during the early stages of fatigue in this alloy dislocations cut through the coherent precipitate and bring about the reversion of the precipitate. Subsequent aging at 150ºC induces reprecipitation in the precipitate-free zones so that the weakened regions are strengthened and the fatigue life is extended. It Is recognized that the fatigue strengths of precipitation hardened aluminum alloys are unusually low relative to their tensile strength.'-= This feature is illustrated in Fig. 1 where it can be seen that age-hardened alloys have lower fatigue ratios (the ratio of the fatigue strength to the tensile strength) than those in the annealed or cold worked state. Further, as shown in Fig. 2, the more an alloy is dependent upon precipitation hardening for its total strength, the lower is the ratio of the fatigue strength to the tensile strength. This state of affairs has been associated with an instability of the metastable metallurgical structure of precipitation hardened aluminum alloys during cyclic loading. Evidence2 in support of this view is that the fatigue ratio increases in these alloys as the test temperature is lowered, thereby indicating that thermo-mechanical instability, rather than some other factor such as a non-uniform distribution of precipitate, is the factor responsible for the low fatigue ratio at room temperature. Two mutually exclusive proposals have been ad- vanced to account for this instability. Hanstock has proposed that overaging takes place during cyclic loading, and in support of this view, Broom et a1.2 have indicated that an overaging process might be promoted by the large numbers of vacancies which are created during cyclic loading. The creation of vacancies by radiation4 has been shown to lead to rapid overaging. Hanstockl obtained visual evidence of overaging in an aluminum alloy after cyclic loading, but in this instance it has been pointed ou? that because of the high frequency used (60,000 cpm) the observed effect may have been due to normal high temperature precipitation around energy dissipating cracks. Efforts to discern visual evidence of overaging in this alloy at lower test frequencies were not successful.3 The alternative postulate3 is that reversion takes place during cyclic loading and leads to localized soft spots at which fatigue cracks are readily initiated. Evidence for this process has recently been provided by Polmear and Bainbridge5 who demonstrated metallographically that regions depleted of precipitate were created during cyclic loading of an aluminum alloy. Inasmuch as precipitate particles bordering the depleted region had not grown in size, it was concluded that the solute atoms which had constituted the missing particles had gone back into solution. No mechanism for the reversion process was presented. The present study was undertaken to investigate further the conditions leading to instability during cyclic loading, and to determine whether reversion or overaging had taken place as a result of cyclic loading. BACKGROUND AND TEST PROCEDURE In order to differentiate between the processes of reversion and overaging, rest periods at an elevated temperature, which ordinarily would insure additional precipitation, were used in this investigation. It was expected that after a period of cyclic loading an elevated temperature rest period would result in a decrease in the remaining life of the specimen if overaging were occurring during cyclic loading, whereas in the case of reversion, reprecipitation would occur and the fatigue life would be extended. Such an expectation is based on the assumption that the crack-nucleation phase is a significant portion of the total fatigue life, and that such a treatment is of influence in the crack-nucleation stage and is relatively unimportant thereafter.

Jan 1, 1963

By F. G. Tahmoush, N. J. Grant, E. P. Abrahamson

The effect of grain size on the brittle -ductile transition temperature of pure iron and three dilute Fe-W alloys has been investigated by slow bend tests. The brittle-ductile transition temperature for pure iron increased with increasing grain sizes from 8000 to 500 grains per sq mm where the transition temperature then decreased with further increase in grain size. The dilute additions of tungsten lowered the transition temperature for fine grain sizes, suppressed a reversal of the curve in the coarse grained portion, and raised the transition temperature for this region. The frequency of twin occurrence increased with increasing grain size and decreasing temperature. The object of the present investigation was to re-examine the effect of grain size on the brittle -ductile transition of pure iron and several dilute Fe-W alloys. Current literature normally presents a simple relationship between grain size and the brittle-ductile transition temperature, namely, that the transition temperature increases with increasing grain size. Heslop and etch' have studied the transition temperature of mild steel by V-notch Charpy impact tests for the grain size range between 200 and 6000 grains per sq mm. The result was a linear plot of In 1-1/2 vs brittle-ductile transition temperature, where 1 is the grain diameter. Recent experiments by sipos2 revealed the possibility of a reversal in the slope of the grain size vs transition temperature plot for pure iron; however, his investigation was limited in scope, and the data obtained were insufficient to permit a definitive curve. The present investigation was undertaken in an effort to confirm or extend the grain size effect observed in iron by Sipos. PROCEDURE All alloys were vacuum induction melted, using 99.95 pct Fe containing 0.03 pct 0 and 0.004 pct C. Four ingots were made, ranging from pure iron to iron with 0.035 pct W. The chemical composition of each alloy, after processing, is given in Table I. The four alloys were prepared as 45 lb heats and cast into 4 in. diam by 16 in. molds. They were then extruded into 3/4 in. rods at 1800oF. Specimens for chemical analysis, taken from various positions along the rods, revealed no variation in tungsten content along the length. The extruded rods were reduced to 0.156 in. diam stock by a series of cold swaging operations involving intermediate vacuum annealing treatments. This procedure yielded a final cold reduction in area ranging from 10 to 90 pct. The swaged rods were chemically cleaned, cold pressed to a cross section of 0.10 by 0.18 by 1.0 in. long (2.54 by 4.73 by 25 mm). The specimens were wrapped in iron foil and vacuum sealed (10-4 mm Hg) in quartz. Various heat treatments at temperatures from 700" to 1300oC were utilized to produce grain sizes from 8000 to 1 grain per sq mm. Grain sizes were determined by measuring the average area of grains in a polished section. In specimens with grain size greater than 20 grains per sq mm, the total number of grains in the cross section was counted and then divided by the area to yield grains per sq mm. Grain size was measured both for longitudinal and transverse cross sections. The average of the two measurements was plotted vs transition temperature. An Instron Table Model testing machine was used to determine the transition temperature of specimens tested in three point horizontal bending. The specimen was supported by two 1/4 in. dowels one in. apart. Bending was accomplished with a push rod, the end of which had an 1/8 in. radius. The head speed was 50 in. per min. Temperatures were established through the use

Jan 1, 1963

By G. R. Speich

The age-hardening of Fe-18 to 21 pct Ni marten-sites containing small amounts of titanium, aluminum, copper, or molybdenum has been studied by hardness measurements, transmission electron microscopy, extraction replicas, and X-ray and electron diffraction. Electyon-probe microanaly-sis of the extracted precipitates was also performed. The effects of temperature and composition on the aging kinetics have been studied in detail for Fe-20 pctNi-Ti martensites. All the martensites hardened on aging at 400" to 500 "C with a single aging peak. In the Fe-20 pct Ni-Ti martensites hardening was associated with the formation of a fine dispersion of NisTi. No precipitation was observed in an Fe-21 pct Ni-2.6 pct A1 alloy, although the hardness increased from 327 to 545 Dph during aging at 500°C. Copper was precgitated from an Fe-20 pct Ni-10.7pct Cu alloy, at least during the later stages of age-hardening. Hardening in an Fe-18 pctNi-5pct Mo alloy was associated with the precipitation of an intemzetallic compound tentatively identified as NisMo. The formation of austenite and the recovery of the defect structure of the martensite occur simultaneously with the normal precipitation processes &ring aging of these alloys. THE age-hardening of substitutional iron-base martensites is an important subject for study since age-hardening is one of the principal means of strengthening the substitutional iron-base martensites in precipitation-hardening stainless steels1 and maraging steels.a~4 In contrast to Fe-C martensites, these martensites are relatively soft and ductile in the as-quenched condition, due to the low solid-solution hardening effect of the substitutional elements as compared to carbon. Also, these martensites are hardened by aging at low temperatures in contrast to Fe-C martensites which generally soften on tempering. Titanium and aluminum, singly or in combination, as well as copper and molybdenum, have been the principal alloying additions to stainless steels to obtain an age-hardening reaction.' Ti-A1 or Co-Mo-Ti combinations have been used in the case of maraging steels.3"4 The present work has been confined to a study of the age-hardening characteristics of an Fe-18 to 21 pct Ni martensite to which small amounts of titanium, aluminum, copper, and molybdenum were added in order to study the effects of each alloying element separately. The age-hardening characteristics of these alloys were studied by hardness measurements, transmission electron microscopy, extraction replicas, and X-ray and electron diffraction. Electron-probe micro-analysis of the extracted precipitates was also performed. The types and dispersion of precipitates, the formation of austenite, and the recovery of the defect structure of the martensite all were studied. EXPERIMENTAL PROCEDURE Alloys. The compositions of the alloys studied are listed in Table I. The level of 18 to 21 pct Ni was chosen to assure complete transformation to martensite on quenching and is the same nickel level used in maraging steels. The concentrations of titanium, aluminum, copper, and molybdenum were chosen after a study of the and Fe-Ni-MO' ternary diagrams indicated how much of each alloying element could be dissolved in austenite. Alloys with 2 and 4 pct Cu were also studied, but these did not show precipitation hardening at the nickel levels studied and will not be discussed further. The alloys were prepared from electrolytic iron and high-purity* nickel, titanium, aluminum, copper, and molybdenum by vacuum melting of 20-lb heats. These were vacuum-cast into two 8-lb ingots. The ingots were hot-rolled at 1100°C to 1/2-in. plate and subsequently cut into 3/8-in. cubes. The cubes were sealed in evacuated quartz capsules and solution-treated for 16 hr at 1100°C, except for the Fe-20 pct Ni-10.7 pct Cu alloy and Fe-21 pct Ni-2.6 pct A1 alloys which were solution-treated for 16 hr at 1300" and at 1250"C, respectively. Metallographic examina-

Jan 1, 1963

By D. I. Bardos, A. M. Bardos, Paul A. Beck

The approximate effective silicon radii in ternary Laves phase alloys with transition elements and silicon were found to range between 1.16 and 1.21A, i.e., considerably smaller than the atomic radius calculated for elemental silicon. The atomic radii were found to increase with the size of the transition element atoms in the structure. It has been noted by Aronsson1 that silicon in solid solution in iron, cobalt, and nickel has an effective CN 12 atomic radius of approximately 1.20Å, a value very much smaller than the CN 12 radius of 1.34Å derived from the interatomic distances in elemental silicon.7 The unusually short metal-silicon interatomic distances in transition element monosilicides and disilicides have been also pointed out by various investigators.1 A similar tendency was observed by Nevitt in Cr3O type silicides.2 Recent work on Laves phases in ternary systems of silicon with transition elements4"8 suggested that extensive Laves phase fields may occur in such systems.8 It has been pointed out by Laves7 that the MgCu2 and MgZn2 type structures lend themselves particularly well for the determination of the effective radii of the component atoms. In these AB2 phases the B atoms are arranged in close packed straight lines, and their distances are related in a simple manner to the lattice parameters.8 The present work was undertaken in order to find out whether or not the B transition element in such AB2 Laves phases can be replaced to an appreciable extent by silicon. In cases where extensive substitution proves to be possible, the "average atomic radius for the B site" at various silicon contents was to be determined, and the effective atomic radius of silicon calculated by extrapolation to complete replacement of the B component by silicon. The following ternary systems were studied: Ti-Mn-Si, Ti-Fe-Si, V-Co-Si, V-Ni-Si, Nb-Fe-Si, Nb-Co-Si, Ta-Fe-Si, Ta-Co-Si, and Mo-Fe-Si. In all of these alloy systems, the Laves phase solid solutions were found to extend over a considerable range of silicon content. As previously reported,4"8 in the V-Co-Si, V-Ni-Si, and Mo-Fe-Si ternary systems Laves phases do occur, even though there are no corresponding binary Laves phases. In stabilizing the Laves phase, silicon acts as if it were decreasing the effective electron concentration of the alloy.8 A more detailed study of the boundaries of the Laves phases in the V-Co-Si and V-Ni-Si systems has been made and will be published elsewhere. In both cases, the elongated Laves phase fields extend parallel to the B-Si side of the composition triangle, clearly showing that silicon is substituting for cobalt, respectively, nickel over a wide range of compositions. The binary Laves phases NbCo2 and TaCo2 have the cubic MgCu2-type structure. It was found that, in both ternary systems with silicon, again the MgZn2-type hexagonal Laves phase is stabilized and that this phase extends to high-silicon contents. In each ternary system at least three Laves phase alloys of the composition A(B1_xSix)2 were used, x here denoting the fractional substitution of the B-transition element atoms by silicon. The alloys, listed in Table I, were prepared by arc melting in argon. Each specimen was water quenched after a homogenizing anneal of 3 days at 110(FC, except for the Mo-Fe-Si alloys, which were annealed at 1200°C. Metallographic examination showed that most of the homogenized alloys consisted of a single phase, although some had minor amounts of a second phase, as shown in Table I. X-ray diffraction patterns were prepared using an asymmetrical focusing camera of large resolution and Fe Ka radiation. The patterns were indexed, and the lattice parameters of the hexagonal Laves phases were determined from the available diffraction lines of highest indices: (213), (205), and (313). The lat-

Jan 1, 1963

By Wingham DW

Based upon the previous work of Norman and Loeb, a method, was used, to assess-the comparative wearing properties of ten different alloys being used, or being considered for use, as mill liners and grinding media at Mount Isa. The materials to be tested were obtained in the form of large diameter balls and were run, along with the regular ball charge, in a large ball mill operating-under normal grinding conditions. At selected. intervals, the test balls were removed from the mill, weighed and identified, and their relative wear rates determined.

Jan 1, 1963

By E. C. Olsen

This paper describes the unusual hazardous conditions encountered in mining thick, inclined coal beds under heavy cover in Carbon County, Utah. This description includes heavy roof conditions, sloughing ribs, steep pitches, and severe bouncing experience. Emphasis is placed on the top bench system of mining and development in the top half of a 16-ft seam, under the roof rock, which is bolted, and the recovery of the bottom coal on retreat; success of bolted roof and ribs; and shuttle car haulage on pitches up to 25%. The use of protective cages for operators of face equipment, the guarding of belt conveyor systems to prevent injury associated with deliberate entry, and the positive lockout of electrical equipment is described and illustrated. Most coal mining areas of the Western United States are characterized either by thick beds, steep pitches or heavy cover. Individually, each of these may present inherent safety hazards that in- fluence mining. When all are met at one location, the combined effect is to make the safe operation of the mining property a challenge to management. These combined conditions are met in the coal mines of the Columbia-Geneva Steel Div. of the United States Steel Corp., in southeastern Utah. This coal bed measures up to 16 ft in thickness, the pitch is as much as 25% and mining is under a cover approaching 3000 ft. The Sunnyside coal bed is found in the Book Cliff Mountains, a great escarpment extending from west of Castle Gate, Utah, some 180 miles to Grand Junction, Colo. West of Green River, Utah, the Book Cliffs swing sharply to the north because of the domelike uplift of the San Rafael Swell to the southwest. It is in this northerly extension of the Book Cliffs that the Sunnyside coal in the Blackhawk Formation of the Mesa Verde Group, Upper Cretaceous Age is found. The strata are transected by numerous faults with from a few inches to as much as a hundred feet of displacement. All of these faults have had some effect on the mining operation, either in roof control or, in the case of major faulting, the pattern of mine development. MINING PRACTICES Mining has generally been confined to the Lower Sunnyside Seam which measures from 7 to 16 ft in

Jan 1, 1963

By D. Weinstein, F. C. Holtz

AS a possible method of improving the elevated temperature strength properties of zirconium, an investigation was initiated on the feasibility of producing a dispersion-strengthened material. Because of the high reactivity of zirconium, its high solubility for oxygen, and the stability of the Zr-0 solid solution, the major problem in such a development is choice of a suitable dispersant. Thus, in the present investigation we were concerned primarily with the stability of various dispersants in the zirconium matrix. The experimental procedure consisted of blending powders of zirconium and a dispersant, followed by cold compaction and extrusion. The best available source of -325 mesh zirconium powder contained between 1500 and 3500 ppm Oz; to this material, powders of zirconium carbide (5 p max), vanadium carbide (5 p max), alumina (0.03 p average), lan-thana (0.8 to 2 p), ceria (0.8 to 2 p), yttria (0.8 to 2 p), calcia (44 p rnax), or thoria (0.6 to 0.8 p) were added in amounts of 7 vol pct and compacted at 65 tsi. A cylindrical compact having a density between 70 and 80 pct of theoretical and dimensions of 1 in. diam by 1-114 in. high was thus produced. After canning in copper, these billets could be extruded (5: 1) on a 54-ton capacity, slow-traverse hydraulic press with the billet temperature at 1550°F and the extrusion die at 900°F. However, lack of densifica-tion of some of the extruded billets necessitated ratios of at least 23 :1. Ultimately, all billets were successfully extruded at 1500°F to 0.190 in. diam (32 :I), fully dense rods using a 200-ton capacity press and a ram speed of 90 ipm. The microstructures of as-extruded Zr-7 vol pct LazOS and Zr-7 vol pct Y2Os are shown in Fig. l(a) and (c), respectively. These structures are similar to all the as-extruded materials and consist of an elongated, single-phase zirconium matrix dispersed with oxide or carbide particles. Very little porosity is observed, and the interface between matrix and particles appears satisfactory. The size and distribution of particles, however, are not ideally of the type desired for dispersion strengthening. Since the primary study was of particle stability with respect to zirconium, no attempt was made to overcome agglomeration during powder blending and fabrication. Some areas exhibit fine, well-distributed particles; undoubtedly, a small proportion is submicroscopic and has the

Jan 1, 1963

By Paul M. Price

The Mouat mine, Nye, Mont., was reopened in 1953 by the American Chrome Co. under a Defense Minerals Production Administration contract. Operations were terminated in 1961 after completion of the contract. Mining methods employed during this period are described in detail, and cost data are presented by years for 1953 through 1959. Ultramafic rocks of the Stillwater complex in Montana contain the largest domestic resource of chromite, and the Mouat mine has been the largest producer. Mine reserves were estimated in 1960 to be about 4.4 million tons containing 22.5 percent Cr2O3. The chromite deposits occur as a series of overlapping bands or lenses roughly paralleling the steeply dipping layers of the complex. Only two of the chromite layers have proven to be of economic importance. One layer is 2 to 16 feet wide; the other is 3 to 8 feet wide. Shrinkage stoping was generally used throughout the mine, but various methods of ore breaking, stope drawing, chute construction, etc., were tested to improve output and lower costs. Long-hole stoping proved to have limited use. Breasting down benches, developed outward from the center of the stope with air-leg drills, was satisfactory only in wider stopes. At the close of operations, the company had standardized the use of lightweight stopers to advance a flat back by breaking from a centrally located face. Mining costs were reduced 47 percent during 7 years of operation.

Jan 1, 1963

By W. Julian Parton

General Crushed Stone Co. operates a dozen quarries in such rock types as gabbro, basalt, granite and limestone. Drilling characteristics and problems vary from one operation to another so that a variety of equipment and methods must be employed. In addition, it has been found that equipment improvements make it advisable to continuously look for and experiment with new machines and accessories. This article discusses drilling progress at some of the Company's more interesting operations.

Jan 1, 1963

By T G. Callcott

Australian coking coals are either class 434<tlj534<2l, at Port Kembla, or 634<3> at Newcastle. The former yield good blast-furnace cokes; the latter yield poor ones. However, increases in conventional strength indices, by methods applicable with normal coking ovens, seem unlikely to be economically attractive. Characterization of the coals has enabled an "economic" blend to be developed in the Newcastle area, and this has affected mining, preparation and handling operations. Coking studies have led to a specification for the making of strong coke, especially from the high-volatile Newcastle coals. Continuous coking studies, developed from the efforts to make very strong coke, have taken two directions. Firstly, coking thin layers of coal on strands; secondly, coking, in various types of vessels, compacts of coals with or with-out the inclusion of non-coking coals, iron ores or other inert materials. Gas, "sand" and hot metal coking have been tested for use in compact coking. Particular attention has been paid to pellets of coal and ore. The probable industrial problems in adopting any of the ideas are presently being examined.

Jan 1, 1963