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By R. G. Wheeler, J. W. Goffard

The Larson-Miller parameter was used to correlate time, temperature, and indentation creep of magnesium, aluminum, and some of their alloys. In the temperature range 300" to 450°C, the short-time Meyer hardness of pure magnesium was less than that of the magnesium alloys tested, but for long times the pure magnesium has greater indentation creep resistance. Aluminum (1100 alloy) had 1.5 to 2.5 times more indentation creep resistance than magnesium at 300" and 450oC, respectively. Hardening of aluminum with a dispersion of Al2O3 was effective in the time and temperature ranges studied. New technologies have required the development of new materials and the utilization of the more familiar materials for new and unusual applications. The use of magnesium and aluminum and some of their alloys, because of their desirable nuclear characteristics, light weight, low cost, and ready availability, has been extended to the 300" to 450°C temperature range. In this temperature range the basic consideration of these materials must be their rate of plastic flow rather than offset yield strengths. The indentation testing reported here arose from a need for design data for the load-holding ability of supports made of these materials. Test Procedure—Hardness indents were made with a 0.275-in.-diam quartz indentor and a 10.65-lb load. The indentor was made by fire-polishing a spherical surface on the end of a fused quartz rod. The samples were held at temperature in a graphite crucible controlled to ±2°C. A thermocouple was attached to the sample and test temperatures were recorded. The diameter of the spherical indentation was measured at the end of a test period and the compression stress (Meyer Hardness) was determined by: H___________load__________ m = projected area of indent Samples were 1 in. in diam and at least 1/4 in. thick. It was observed that at the higher temperatures and longer times, the quartz indentor would stick to the magnesium sample. The quartz indentor was, therefore, frequently inspected and fire-polishing repeated when necessary. The area of sticking was always a small fraction of the area of indent and was therefore considered to have an insignificant effect on results. Correlation of Hot-Indentation Test Data with Time-Temperature Parameter—Sherby and Dorn' have correlated creep or tensile data of a' solid solutions of aluminum with a temperature and strain-rate parameter suggested by Zener and Holloman. underwood2 used this parameter to correlate creep properties of some steels with hot hardness, and upon the basis of this correlation a means of obtaining creep properties from short-time (and inexpensive) hot hardness tests has been demonstrated. Since the validity of the correlation of creep properties with a time-temperature parameter and the correlation of creep properties with hot hardness have been shown, it follows that hot hardness may correlate with the time-temperature parameter. The hot-indentation data obtained was expressed as Meyer hardness, and was shown to be time and temperature dependent. Correlation of Meyer hardness, time, and temperature with the parameter was made using the relationship: Hm = Meyer hardness t = time, hours T = absolute temperature, OK K = constant A value for the constant K was calculated by equating In l/t + K/T at different temperatures and times but at the same hardness. The correlation was tested by plotting Hm vs the parameter, In 1/t +K/T. Since materials are being sought which have high hardness at low indentation creep, i.e., a high Meyer hardness for long time at high temperatures, low values of the parameter are ofthe most interest. TEST RESULTS Magnesium—Pure magnesium (99.98 pct) cut from extruded rod was indentation tested perpendicular to the rod axis at temperatures of 300°, 350°, 400°, and 450°C for times ranging from 6 sec to 112 hr. Fig. 1 shows the time dependency of Meyer hardness at the four constant temperatures. Fig. 2 shows the correlation of the Meyer hardness of pure magnesium with the time-temperature parameter using a K of 22,720 in Eq. [I]. At the bottom of Fig. 2, the effect of doubling the time of indentation t2 = 2(t1), on the abscissa for any time is shown graphically. This effect is of constant magnitude. Also shown graphically are the magnitudes of the effects on the

Jan 1, 1960

By J. Nutting, J. W. Cahn

WITH the development of thin film techniques for the direct examination of metals in the electron microscope some new problems in quantitative metallography have become apparent. In order to obtain certain contrast effects in the electron optical image when examining thin films from alloys containing dispersed phases, it is essential to use films of a thickness at least two or three times greater than that of the mean particle diameter of the dispersed phase. From micrographs of such specimens it may be desired to obtain the volume fraction of the dispersed phase and the number of particles of the phase in a unit volume of the matrix. Under these conditions the particles sectioned by

Jan 1, 1960

By A. C. Johnson

This report is one of a series being prepared by the Bureau of Mines on exploration, development, mining methods, and costs at various mines in the United States. It describes operations at the Black Rock mine, Wah Chang Mining Corp., Mono County, Calif. The purpose of these reports is to promote development and conservation of our mineral resources by disseminating technologic information on mining methods, practices, and costs. The Black Rock tungsten mine of the Wah Chang Mining Corp. is 33 miles north of Bishop, Calif., in the Benton Range, Mono County, Calif. The property was acquired in August 1950 and a well-planned program of exploration, development, and exploitation resulted in a good production record with low costs. Operations were halted in July 1957, about 6 months after suspension of the tungsten purchase program by the Federal Government.

Jan 1, 1960

By H. E. Powell

A laboratory mineral-dressing investigation was conducted by the Federal Bureau of Mines on four limonitic and four sideritic iron ores from the North Basin of the east Texas iron-ore district. The samples, composited from drill cores, were considered representative of the iron-ore reserves of the area. The objectives of this research were twofold: (1) To devise a mineral-dressing method whereby the yield from currently mined east Texas iron ores might be increased and the grade improved, and (2) to extend such treatment to include the lower grade ferruginous materials that are not amenable to beneficiation by simple washing and, therefore, are not being exploited. Of the mineral-dressing methods used in this investigation, magnetic separation of roasted are was shown to be the most effective. Results show that, by this method, a laboratory recovery of 82 percent of the iron is attainable at a grade surpassing that obtained by current plant practice and that both limonite and siderite are amenable to concentration by the process. The existence of large deposits of iron are in eastern Texas has been recognized for over 100 years. These ores were first exploited during the Civil War and were mined intermittently until about 1911. From that time until 1944 when the Defense Plant Corporation financed the erection of three blast furnaces to use these east Texas ores, production was almost at a standstill.4/

Jan 1, 1960

By Thomas J. Blalock

The volumetric determination of uranium according to the method of Sill and Peterson (6),3/ which uses cerate oxidimetry after the separation of interferences such as sulfides and cupferrates, has been used for some time by the Bureau of Mines and gives satisfactory results for many of the samples tested. However, in those instances where the uranium content did not exceed a few tenths of 1 percent and iron was present in the range of 10 to 40 percent (as Fe203),4/ the method was cumbersome and unreliable. The need for a more accurate procedure for the determination of small amounts of uranium in the presence of large amounts of iron, such as in shale or black sands, prompted this investigation. The Bureau desired that materials containing as little as 60 p.p.m. of uranium be assayed within reasonable limits of accuracy. One of the primary aims of this work has been to eliminate, as far as possible, the necessity for repeated cup ferron extractions.

Jan 1, 1960

By A. J. Miller

Estimates of interstitial water saturation derived from capillary pres-sure data are compared with residual water saturations found by the analysis of cores out in oil-base drilling fluid. A theoretical explanation for the high-rate of water production from the Bellshill Lake Field is proposed, based on the interpretation of the capillary pressure data.

Jan 1, 1960

By I. L. Feld

This report describes an attrition-grinding process and equipment for grinding coarse kaolins to the 2-micron particle-size range. The research was undertaken by the Bureau of Mines to devise an acceptable method for converting coarse kaolins, such as paper-filler-grade clays, to paper-coating-grade clays, thereby increasing the value and extending the life of the southeastern paper-clay deposits. The attrition-grinding process is basically the intense agitation of a slurry composed of the material to be ground, a granular grinding medium, and a suspending fluid. This process gave better particle-size reduction than that obtained by several other grinding methods. Results of batch tests in 5-and 10-inch-diameter attrition grinders demonstrated that a coarse kaolin containing about 13 percent minus 2-micron, equivalent spherical diameter (e.s.d.) particles was readily ground to give a product with 88 percent minus 2-micron e.s.d. material. Power consumption was reasonable in view of the increased value of the ground material. Comparison of particle-size reduction with power-consumption data for the two units indicated that better performance was obtained with the larger machine.

Jan 1, 1960

By Y. A. Rocher, J. E. Dorn, L. A. Shepard

Creep activation energies for single aluminum crystals favorably oriented for shear by (010) [101] glide were detemined over the temperature range from 78" to 900°K. Observations of slip bands on the specimen surface were made in conjunction with the investigation. From 78" to 780°K, the activation energies obtained in this imestigation agreed closely with those previously found for creep by (111) [101] slip. Between 78" and 140°K, the activation energy was identified with the Peierls process, while between 260°and 780°K the activation energy was close to that for cross-slip. The coarse wavy slip bands nominally parallel to the (010) plane observed above 260°K were attributed to fine cross-slip. From 800" to 900°K, unusually high apparent activation energies ranging from 28,000 to 54,000 cal per mole were obtained. These apparent activation energies were attributed to re crystallization. AS illustrated in Fig. 1, a recent investigation1 has shown that creep of aluminum single crystals by the (111) [i01] mechanism is controlled by three unique processes, each of which is characterized by a single activation energy which is independent of the applied stress and the creep strain. A comparison of the observed activation energies with theoretically calculated values permits a fairly clear identification of the three operative creep processes. Below 450°K, where the activation energy for creep is 3,400 cal per mole, the deformation is controlled by the Peierls process, the activation energy for creep agreeing well with that calculated by seeger2 for the energy required to nucleate the motion of a dislocation loop against the atomic forces of the lattice. Between 590° and 750°K, the observed activation energy for creep of about 28,000 cal per mole agrees well with the energy necessary to induce cross-slip. Seeger and schoeck3 estimate that the activation energy is about 24,000 cal per mole whereas Friedel4 recently calculated this activation energy to be 28,000 cal per mole. Above 800°K the activation energy of 35,500 cal per mole that was observed for creep agrees well with that estimated for self-diffusion in aluminum.= In this range the operative rate-controlling slip process has been clearly identified as that arising from the climb of edge dislocations. The objective of this investigation is to ascertain whether a single crystal of aluminum favorably oriented for simple shear in the [loll direction on the (010) plane might exhibit uniquely different activation energies for creep from those obtained previously for (111) [101] slip. Whereas the exis- tence of such unique activation energies would constitute incontrover table evidence for new mechanisms of slip, the absence of any new activation energies might suggest that slip of aluminum is confined to the (111) [loll mechanism. Several factors prompted the selection of the (010) [101] orientation for study. First, there are more reported observations of (010) [loll slip than of any other nonoctahe-dral mechanism.8-10Secondly, Chalmers and Martius1l have concluded from considerations of the energies of dislocations that (010) slip is the second most favored mechanism in face-centered-cubic metals. Finally, favorable orientations for simple shear by the (010) [loll mechanism provide the least favored orientation for slip by the (111) [101] mechanism. EXPE-RIMENTAL PRO-CEDURE The high-purity aluminum stock, specimen preparation, shear fixture, extensometry, and experimental technique used in this investigation were the same as those previously reported.' Single-crystal spheres grown from the melt of 99.995 pct pure Al* were _ *The high-purity aluminum used in this investigation was graciously given by the Aluminum Company of America. oriented, carefully machined into dumbbell-shaped shear specimens, annealed, and chemically polished. The finished specimen had a central reduced section 0.190 in. wide and 0.590 in. in diam and 1/4-in. grip sections at both sides, 0.690 in. in diameter. The specimen was oriented in the stainless steel grips of the shear fixture with the (010) plane perpendicular to the dumbbell axis and the [loll direction parallel to the stress axis within 2 deg. Creep activation energies were calculated in the previously described manner1 from determinations of the instantaneous change in shear strain rate produced by an abrupt 15 to 20 deg increase or decrease in test temperature. If is the instantaneous strain rate at strain y and temperature T1, and ?2 the instantaneous rate at y and T2,

Jan 1, 1960

By J. Duby

"A description is given of a series of tests performed to determine the comparative effects which dynamic and static straining, in compression, have on the physical strength properties of mild steel and an aluminum alloy. The dynamic deformation was imposed during the passage of single stress pulses of about 100 micro-second duration. These pulses were recorded with strain gauges mounted near both ends of the specimen. The resulting records were analysed using a simple wave theory; there from the dynamic stress-strain curves for the respective metals were deter-mined and were then compared with the static stress-strain relation. The respective hardnesses of the metals after deformation are evaluates by means of static stress-strain curves in compression. The micro-structures of the metals before and after deformation are also shown. It is observed that dynamic de-formation considerably modifies the rate of strain hardening. This modified hardening appears to be persistent. The observed differences in physical strength properties and micro-structures are discussed in the light of the accepted dislocation theory for metals."

Jan 1, 1960

By Clifton W. Livingston

So many factors influence blasting results that theories and rules are usually dismissed as impractical; the practice prevailing today is arrived at by cut and try. Usually the first step is to experiment with drillhole patterns and spacing until an arrangement is found that gives best results. The next step is to experiment with different types of explosives and sequences of blasting until the most satisfactory degree of fragmentation is achieved and until no further reduction in cost is immediately apparent. Improved fragmentation is generally attributed to the type of powder used, the sequence in which the holes are blasted, or the use of millisecond delays. Various types of drill rounds have been evolved in tunneling operations, underground development headings, and stoping, and various patterns of blasting in open pit mines and quarries. These practices usually are carried from mine to mine or from district to district, and great skill is exercised by those experienced in the art of blasting.

Jan 1, 1960

By J. W. Eckerd

This report describes an investigation of the technical feasibility of using a conventional commercial-size (10-ft. i.d.), rotating grate, dry-ash-removal type gas producer to make producer gas from chestnut-size bone anthracite. Test instruments were installed, and some minor changes were made in the equipment to handle the large quantities of materials expected. Extensive tests, lasting about 4 weeks, were planned, using 35 to 50 percent ash chestnut anthracite bone. However, operations were suspended after 8 days when it became apparent that to use this type of fuel satisfactorily substantial changes in equipment and operating procedures would be required. Nevertheless, enough data were obtained to indicate that gas could be produced continuously and routinely from bone coal in this type of producer whenever conditions justified the necessary development work.

Jan 1, 1960

By C. W. Taylor, F. L. Martin

"THE DICTIONARY defines Metallurgy as the ""science or art of separating metals from their ores and refining them for use"". In these days, however, such a definition is not detailed enough.The modern science of metallurgy is based on two fundamental sciences, physics .and chemistry, and is sub-divided into two major fields: Process Metallurgy and Physical Metallurgy. These fields of metallurgy are now so comprehensive and involved that even the graduate metallurgist has to specialize in one or the other.In recent years, the relatively new science or technology of non• destructive testing has also entered the industrial scene, with tremendous impact and ramifications. So much so that, certainly, no .discussion on metallurgy can be complete without including some reference to it.Obviously, one paper cannot hope to cover in detail the relationship of the whole science of metallurgy to the mining industry. Consequently, only a very brief reference will be made to the field of Process Metallurgy, our major concern being with Physical Metallurgy and Non-Destructive Testing."

Jan 1, 1960

By D. Bienstock

The Fischer-Tropsch synthesis is practicable in a reactor where the exothermic heat of reaction is removed by circulating large quantities of recycle gas through a catalyst bed of high-voids content. At an hourly space velocity of 1100, the feed gas, a mixture of 1.5 parts hydrogen to 1 of carbon monoxide, was converted 90 percent, producing hydrocarbons predominantly in the gasoline range. At these conditions a recycle-to-fresh gas ratio of 40:1 was enough to give excellent temperature control with a pressure drop of 1.5 p.s.i. per foot of bed using a steel catalyst in the form of lathe turnings. Steel parallel plates, although offering lower resistance to gasflow, were less reactive and less durable. INTRODUCTION The Federal Bureau of Mines has been engaged in a research and development program since 1944 on the synthesis of gasoline from coal. Gasification of coal with steam and oxygen to yield a synthesis gas--a mixture of carbon monoxide and hydrogen--is being investigated at Morgantown, W. Va.; and the synthesis of gasoline by catalytically reacting the carbon monoxide and hydrogen over iron by the Fischer-Tropsch reaction is being investigated at Bruceton, Pa.

Jan 1, 1960

By Louis C. Brichta

This report summarizes the progress made by the Federal Bureau of Mines in assembling and compiling a catalog of available logs of drill holes and maps of mine developments in the Tri-State Zinc-Lead District in northeastern Oklahoma, southeastern Kansas, and southwestern Missouri. It supplements an interim report (11)3/ published in 1955, and for convenience of the reader repeats much of the general descriptive matter pertinent to the district contained in that report. The work of procuring and recording the data was begun in August 1949 and was recessed in May 1959. The catalog preserves the records of accomplished explorations and mine developments in the district and provides a readily available source of information for individuals and firms interested in planning mineral explorations, Government agencies estimating of reserves of mineral resources, and the mining industry for general use.

Jan 1, 1960

By E. G. King

THIRD-LAW entropy data for zirconium-containing compounds are sparse. Kelley a lists entropies at 298° K. for the oxide, tetrachloride, nitride, and silicate, as well as for the metal. The present paper presents heat capacities between 51° and 298° K. and entropies at 298.15° K. for the zirconates of the alkaline-earth metals-calcium, strontium, and barium. The authors believe magnesium zirconate does not exist as a stable compound at room temperature. Entropies of formation from the constituent oxides also are given. MATERIALS The materials used in this investigation were synthesized and analyzed in the Berkeley Laboratory of the Bureau of Mines. Calcium zirconate was prepared by heating an intimate mixture of reagent-grade calcium carbonate and pure zirconia for 30 hours between 1,200° and 1,300° C. and for 32 hours between 1,400° and 1,500° C. As part of the heating schedule, the sample was ground and mixed seven times. Periodic analyses and minor adjustments of composition were made. Analysis of the final product gave 31.19 percent calcium oxide (theoretically 31.28 percent) and 68.67 percent zirconia (theoretically 68.72 percent). The X-ray diffraction pattern agreed with that in the ASTM catalog.

Jan 1, 1960

By S. L. Ausmus

The work covered in this report is a continuation of an earlier feasibility study by the Federal Bureau of Mines and points out improvements in the skull-melting method for casting reactive metals such as titanium, zirconium, and hafnium. Machined graphite molds with laminated sections can be reused many times. Large tube sections can be produced by spin casting. Graphite powder is the best expendable mold material, but binders for this use must be compounded carefully. The effects of current and furnace atmosphere on the dependent variables of the casting technique are shown. Because of developments in casting technology for titanium which eliminate the basic problems of melting and pouring the metal, opportunities for improvement in the method have increased. The mold material and gate and riser configurations require particular attention. The limits of application of the casting method have yet to be defined. New knowledge in anyone of these areas could result in marked improvements and simplifications in casting methods.

Jan 1, 1960

By Virgil L. Barr

National income originating compared to physical production for an enterprise or an industry reflects its ability to strengthen the national economy. For a single industrial sector or for an industry this comparison can be useful to reflect changes that may occur in this ability to contribute because of changing supply-demand-income-investment equilibria. A favorable relationship can be postulated by specified economic incentive, and the accompanying technologic input required can be shown. The new index proposes the use of the Federal Reserve Board indexes of production divided by the constant dollar income originating in the petroleum industry which reflects increases or decreases in performance. When compared with other mineral industries and with, total industry, an approximation of relative strength is evident. By constructing three different hypothetical conditions for future petroleum imports, assuming a constant excess capacity requirement for domestic production, and providing an estimate for future domestic demand for petroleum, the impact on the performance index can be shown. Thus, a strong position for the petroleum and natural gas industry can be stated. If this is done, it becomes evident that because of restrictions on cost-price relationships, a drilling program that would provide enough domestic oil to meet demand may not be practicable. By difference, the amount of improvement in methods of production and processing through technologic advancements can be stated explicitly.

Jan 1, 1960

By F. Seitz

STAFF: Editor, Gerhard Derge Carnegie Institute of Technology Schenley Park Pittsburgh 13, Pa. Editorial Assistant, M. A. Redmerski Managing Editor, James J. Burke THE METALLURGICAL SOCIETY: John Chipman, President; W. R. Hibbard, Jr., Post-President; C. C. Long, Vice-President; T. D. Jones, Treasurer; R. W. Shearman, Secretary. PUBLICATIONS COMMITTEE OF THE METALLURGICAL SOCIETY: R. Maddin, Chairman; Dennis Carney, J. C. Fulton, J. H. Hollomon, T. B. King, C. C. Long, W. 0. Philbrook, J. D. Sullivan, David Swan, and F.L. Vogel. Review and selection of manuscripts is under the supervisian of the following Publications Committees: Extractive Metallurgy D ivis ion: T. 0. King, Chairman; S. J. Dick inson, R. P. Hermsdorf, R. Schuhmann, Jr., and H. H. Kel logg. Institute of Metals Division: F. L. Vogel, Choirmon; R. L. Smith, Vice Chairman; R.W. Balluffi, J. H. Bachtold, A Servi, C.D.Graham, Jr., C. G. Goetzel, F. E. Joumot, Jr., G. E. Pellissier, Paul Gordon, Jock Washburn, Harold Margol in, A. U. Seybolt, I. R. Kromer, R. A. Meussner, R. W. Guard, M. Harmon, J. N. Hobstetter, Dean Starr, P. Shewmon, R. Gordon, J. 0. Betterton, and E. Morgan. Iron and Steel Division: W. 0. Philbrook, Chairman; F. C. Langenberg, C. W. Sherman, J. Wagstaff, and E. J. Whittenberger. Published bimonthly by the American lnstitute of Mining, Metallurgical, and Petroleum Engineers, Inc., 29 West 39th Street, New York 18, N. Y. Telephone: PEnnsylvania 6-9220. Subscription $20 per year for non-AIME members in United States and North, South, and Central America; $25, foreign; $5 for AlME members. Single copies, $4.00, single copies foreign, $5.00. The AlME is not responsible for any statement made or opinion expressed in its publications . . . Copyright 1959 by the Americon Institute of Mining, Metallurgical, and Petroleum Engineers, Inc. . . . Registered cable address, AlME New York ... Indexed in Engineering Index, Industrial Arts Index, and Chemical Abstracts . . .Second class postage paid at New York, N. Y. , ond Ann Arbor, Mich. Volume 215, Number 3

Jan 1, 1960

By K. H. Kretzschmar, M. A. Smith

A brief review of the rapid growth of ACT in Western Canada is presented. It is remarked that this rap-id growth has been accompanied by a heterogeneous approach to design. A more rational and consistent approach is suggested, together with the assumptions on which this approach is based. The operating history of some existing installations is discussed briefly, and conditions necessary for the continued growth of ACT are outlined.

Jan 1, 1960

By Sandford S. Cole

Manganese compounds occur in many mineral forms widely distributed throughout the crust of the earth. The most important of these commercially are the oxides which are usually found as irregular masses, but in some places (notably U.S.S.R.) occur as extensive beds of varying thickness and purity. The principal sources of ore have been U.S.S.R., Ghana (the Gold Coast of Africa), India, Union of South Africa, Belgian Congo, French Morocco, Cuba, Brazil, and Mexico. New developments of ore are being conducted in Brazil, British Guiana, French Equatorial Africa, and Northern Rhodesia. The production of the United States normally meets less than 10 pct of domestic manganese consumption. Manganese ore (35 pct or more Mn) is used principally by the ferrous metallurgy industry for production of manganese metal, ferromanganese, and other manganese alloys for use in production of steel ingots and castings. Some manganese is used in the nonferrous industry as an alloying element and cleanser in aluminum alloys, aluminum bronze, constantan, manganese bronze, Monel, Everdur, nickel-chromium resistance alloys, and nickel-silver. The metallurgical uses consume about 97 pct of the total manganese ore requirements of the United States. The balance goes principally for the manufacture of dry cells and for chemicals, with limited amounts for ceramic products, plastics, welding rods and varnish. The Materials Survey on Manganese, compiled in 1952 for Materials Office National Security Resources Board by the Bureau of Mines and Geological Survey, provides an excellent review of resources, reserves, specifications, uses, mining, beneficiation, metallurgical processes and deposits, and is worth referring to for greater details. Mineralogy and Geology The more common manganese minerals with typical characteristics are listed in Table 1 in order of importance. [ ]

Jan 1, 1960