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By J. C. Bokros, A. S. Schwartz

The irradiation-induced densification of pyrolytic carbon has been shown to take place by a simple first-order rate process. The values of the densification constant, kd, for isotropic carbons are 1.0 x 10-22, 1.4 X 10-22 and 2.8 X 10-22 (nut)-1 at irradiation temperatures of 520o, 670°, and 1000oC, respectively. The apparent activation energy obtained from the temperature dependence of kd for isotropic carbons is about 0.2 ev. Estimates of the maximum stresses that develop in isotropic carbons owing to shrinkage onto an unyielding support show that stresses in excess of 15,000 psi may be avoided during irradiatian at 600" and 1000°C if the initial coating density is kept above 1.5 and 1.9 g per cu cw, respectively. If a carbon coating on an unyielding support is not completely isotropic, stresses may continue to build up at high neutron exposures after densification is complete because of continued anisotropic distortion. Stresses in excess of 15,000 psi from this source may be avoided during irradiation at 1000°C if' the Bacon anisotropy factor is kept below 1.3. A variety of applications of carbon and graphite in nuclear technology has stimulated numerous studies of the effect of neutron irradiation on these materials One of the most interesting problems associated with the use of carbons and graphites in the high fast neutron fluxes of nuclear reactors arises as a consequence of the neutron-induced dimensional changes that occur during irradiation. Energetic neutrons displace car- bon atoms from their lattice positions; and, depending on the temperature, the interstitials and vacancies produced migrate to form clusters, recombine, or are annihilated at dislocations or crystallite boundaries. The competition of various sinks for the point defects results in structure-sensitive bulk-dimensional changes that vary with temperature in a complicated way. This paper deals with the neutron-induced dimensional changes in turbostratic carbons that are being used as coatings on nuclear fuel particles. Details of the structure of these carbons and the variations of their structure with deposition conditions have been reported.'-3 It has been shown in previous work that the neutron-

Jan 1, 1968

By Frank K. Mattson

The Minerals Processing Section of Surface Combustion is currently engineering and erecting a plant designed to produce 400,000 LTPY of 95% metalized pellets from raw magnetite concentrate, This venture is the first domestic commercial facility that will manufacture pre-reduced pellets as an integral part of a process to produce steel. Surface Combustion has developed the methods that will be used. Midrex, a division of Surface Combustion's parent company, Midland-Ross, will own and operate this plant. The site is adjacent to the City of Portland, Oregon on a 15 acre hydraulically-filled area on the east bank of the Willamette River. Either filter cake or concentrates in slurry form will be purchased from Marcona in Peru, delivered to the dock facility by ocean vessels and distributed to a pond for wet storage. Reclamation from the pond will be with a conventional dredge delivering concentrate to a thickener.

Jan 1, 1968

By R. W. Armstrong, P. C. Jindal

TABOR1 has indicated for a number of polycrystal-line materials that their hardness should be directly related to their yield strength. For a material showing zero work-hardening, the Meyer hardness, MH, may be calculated in terms of the yield stress, sy, by utilizing slip line theory and the result is: The Meyer hardness corresponds to indenting the surface with a spherical indenter and specifying the ratio of load and projected area of the indentation. The correlation indicated by Eq. [I] is not well-established. It has been verified to some degree by performing hardness tests on materials strained to the maximum nominal stress and taking this stress as the (new) yield stress of a nonwork-hardening material. The dependence of hardness on yield strength for an annealed material capable of showing work-hardening has not been theoretically evaluated but, presumably, the hardness should be greater than that specified above. Marcinkowski, Fisher, and szirmae2 measured the dependence of the Vickers Diamond Pyramid hardness, H,, on yield strength for an annealed Fe-Cr alloy which shows work-hardening and found:

Jan 1, 1968

By J. C. Williams, M. J. Blackburn

In recent years examination of thin foils of metals and alloys has been widely used in studies of deformation and phase-transformation mechanisms. Applications of this technique to studies of titanium and titanium alloys have been infrequent. Therefore, as a large number of titanium alloys have been investigated in this laboratory, it is proposed to give an account of methods used. Particular emphasis will be placed on some of the artifacts introduced in thin foils of titanium and titanium alloys during preparation. Experimental Procedure. It has been found that a large number of titanium alloys can be electropolished in a solution consisting of 30 cu cm perchloric acid (60 pct), 175 cu cm n-butyl alcohol, and 300 cu cm methyl alcohol. Thin foils are prepared using the window method and the electropolishing conditions listed in Table I. Although this solution is not unique, it is attractive because of its low concentration of perchloric acid and the wide range of alloys for which it can be used. Electropolishing is conducted at below -25°C as above this temperature a brown anodic film is produced on the specimen surface. Temperatures above -25°C also accentuate preferential attack of the 0 phase in the two-phase alloys, which unfortunately occurs at all temperatures. Contamination. It is advantageous to reduce the specimen to a thickness of 25 to 50 p prior to electropolishing, since the low-temperature electropolishing technique results in a low rate of metal removal. Both chemical polishing and grinding have

Jan 1, 1968

By O. D. Gonzalez, R. A. Oriani

The migration of hydrogen and of deuterium dissolved in a iron and in nickel induced by an applied electrical potential has been measured over a range of temperature. In all cases the intevstitial solute migrates to the cathode. The deduced charges of transport are positive, independent of or slightly dependent on temperature, and markedly larger for the beavier mass. These results are interpreted as showing predominating momenlum transfer between electron holes and the acticated complex of the elementary diffusion act. THE migration of components of a metallic system under the action of an applied electrical potential is called electromigration or electratransport. This phenomenon has been known since 1861 and is becoming of increasing interest to metal scientists because of the opportunity it offers to explore the connections between mass transport and electron transport. Until recently, reliable data have been very scarce because of the difficulties inherent in the measurements. In addition, theoretical understanding has been either nonexistent or rudimentary and at present this situation is only moderately improved. Whereas the prevalent notion had been (and is still widely held) that electromigration directly reflects the state of ionization of a component in its equilibrium state in the metal, it is now becoming clear that the major, if not the sole, factor is the momentum transfer between the charge carriers, themselves in motion because of the applied field, and the metallic components in their activated state. It becomes important therefore to obtain reliable data over a range of temperature on electrornigration in systems where only one component moves, that is, either in pure metals (vacancy motion) or in interstitial solid solutions. Our choice of systems was dictated by our measurements' of the Soret effect in solid solutions of hydrogen and deuterium in iron and nickel. Indeed, the main reason for making measurements on electromigration at all is that we suspected a mechanistic connection between thermal diffusion and electromigration. In our former paper' we proposed that what is common to both phenomena is the momentum transfer between the charge carriers in the metal and the atom as it jumps from one equilibrium position to another. In Soret diffusion, however, there is in addition the dissipation of the energy of the jumping atom via pho-nons. We have since found that similar ideas for this interconnection have been developed by Fiks.2 In the present paper we will discuss in more detail our understanding of the mechanism of electromigration itself, but we turn first to a presentation of the experiments and results. EXPERIMENTS AND RESULTS Let us consider a metallic system in which only one component, m , can diffuse at the temperature in question, and to which are applied simultaneously an electrical potential gradient, grad cp, and a chemical potential gradient, grad p,. One may write3 for the material flux Jm and the electronic charge flux Je by applying the condition, grad = 0, to Eq. [I] and evaluating grad(um/T) for the isothermal case and for activity coefficient independent of composition over the relevant composition range. ere, c is the concentration and D the diffusivity of the mobile component. The experimental technique that we have used to measure Z* for the isotopes of hydrogen individually dissolved in each of two transition metals has been developed from a method used by Wagner and Heller.4 (A somewhat similar method was also used by Herold.5) A wire or thin rod of the metal under study connects two volumes of gaseous hydrogen at identical pressures; hence grad um = 0. A direct current is made to pass through the specimen, serving to maintain the specimen at the desired temperature and also to produce the electromigration of the hydrogen dissolved in the metal in equilibrium with the gaseous hydrogen. Under these conditions, the flux of hydrogen from one volume to the other is given, from Eq. [I] for grad( um/T) =0by

Jan 1, 1968

By B. A. Donahue

The results of a survey of 46 West Virginia coal samples, employing the Office of Coal Research-Band coal sewage treatment process, indicated that the Freeport coal and Bakerstown coal from Preston County, Pittsburgh coal from Harrison and Ohio County and the Sewickley coal from Monongalia County offer outstanding potential for water clarification. Oxidation, steam treatment and acid and base washing of coal generally resulted in small positive or negative changes to the water clarification capacities of the coal while the employment of prepared coal fractions resulted in more significant benefits. Of the coals tested, those fractions with high ash, high sulfur and low Btu generally possessed the highest adsorption capacities.

Jan 1, 1968

Reports by researchers in government, industry, and universities of the United States are given for various projects on basic coal research concerning, the metamorphism, physical and chemical properties, and reactions of coal, and how many of these studies can lead to better utilization of coal.

Jan 1, 1968

The Precambrian Eastern Creek Volcanics comprises spilitic basalts with interbedded sediments and tuffs which were extruded and deposited during Middle Proterozoic time. The rocks have undergone low-grade regional metamorphism.The Eastern Creek Volcanics are approximately 17,000 ft thick and have been divided into four units.The rocks were laid down in a geosynclinal basin elongate to the north. The main structural features are the northerly trending Mount Isa and Gorge Creek-Quilalar fault systems.Major east-west faults cause repetition of the sequence.Copper and uranium mineralization is known within the formation. Copper mineralization is confined to quartz-filled shears anp basalts. Nothing of economic importance has been found in the area though ore deposits have been found elsewhere in this type of environment.

Jan 1, 1968

By Earl R. Johnson

Ore broken at the mine or quarry face generally is loaded by power shovels into large trucks or rail cars and hauled to a primary crushing plant where it is reduced to a more workable size for ease in handling. The primary crushing plant is customarily located as close as possible to the center of gravity of the ore body and the projected limits of the mine pit to minimize the cost of hauling and to increase safety from flying rock as a result of blasting operations. A belt conveyor is used to transport the crushed product to a nearby ore treatment plant or, should this plant be located some distance away, the ore is loaded directly into cars and hauled by rail. Between trips the crusher product is accumulated in bins or stock piles. In all open pit mining and quarrying operations, the power shovel, the transportation equipment, and the primary crushing plant should work as a team, complementing each other. When establishing the design and selecting the equipment for these closely integrated operations, capital and operating costs for each unit operation must be weighed to achieve an optimum balance. Rising labor costs have given impetus to the universal trend toward greater efficiency, higher speed and larger equipment, and higher degrees of automatic control. The result is that power shovels have increased in size, haulage trucks are larger and faster, and only coarse crushers with feed openings adequate to receive run-of-mine lumps of ore with a minimum of secondary blasting are selected for new installations. These coarse crushers also have large through-put capacities, even when adjusted to produce a 6- to 10-in. size of product, thus making it possible to use a single stage of coarse crushing at the average mine. The use of a single crusher results in a compact crushing plant layout consisting of a dumping pocket for receiving loads of run-of-mine ore, a coarse crusher followed by a surge chamber for the crushed product, and a feeder to withdraw the ore at a uniform rate to deposit it on a belt conveyor. A

Jan 1, 1968

During fiscal year 1966 the Bureau of Mines published 99 scientific and technical papers and engaged in 67 research projects on petroleum, natural gas, and oil shale. A basic appropriation of $3.4 million was supplemented by $1 million in cooperative funds from other Governmental agencies and industry groups. Petroleum conservation was advanced by development of scientific knowledge and improvement of technologic methods in both the extraction and utilization of petroleum, natural gas, and oil shale. Experimental work was carried out at research centers in Bartlesville, Okla., and Laramie, Wo., and in laboratories in Morgantown, W. Va., and San Francisco, Calif. ACHIEVEMENTS IN FISCAL YEAR 1966 Bureau of Mines--Petroleum Research in fiscal year 1966 (July 1, 1965- June 30, 1966) was involved in many public issues--air pollution, peaceful uses of nuclear explosives, utilization of oil-shale resources, computerization of recovery-stimulation techniques, and fuels for supersonic airplanes. Scientific contributions included compositional studies of petroleum and oil shale, determination of thermodynamic properties of petroleum compounds, development of analytical techniques, and correlations of petroleum properties with geologic occurrence. Technologic advances included rock-fracturing research, in situ combustion studies, waterflood techniques, use of radio-tracers to study stability of petroleum fuels, and hydrogenation as a tool to prepare shale-oil products.

Jan 1, 1968

By M. F. Burr, F. V. Lenel, G. S. Ansell

The mechanism of materials transport was studied in a model experiment in which a silver sphere was sintered to a silver plate under an applied external stress near 800° C. For this purpose the rate of growth of the neck between the sphere and the plate which is proportional to the strain rate of the creep process involved in a neck growth was determined by measuring the change in electrical resistance of the away. This rate of neck growth will depend upon the magnitude of the applied external stress. By measuring the rate just before and just after a change in the external load and therefore the applied stress, the relationship between strain rate and stress can be derived. For material transport by slip in a pure metal it is expected that the strain rate should be proportional to the 4.5th power of the stress, while for transport by diffusional flow the strain rate should be proportional to the first power of the stress. It was found that for stresses above 5 X 10' dynes per sq cm (70 psi) the exponent in the stvain rate-stress relationship was near 4.5 while for a stress of 0.7 x 108 dynes per sq cm (10 psi) an exponent of 1.8 was determined indicating that under the conditions of the experiment the transport mechanism for creep in silver shifts from diffusional flow to slip in the region of 0.7 x 106 dynes per sq cm (10 psi). The importance of these findings for an understanding of the mechanism of material transport in conventional sintering (without an external load) is pointed out. In a paper by Early et al.,' the mechanism of material transport during sintering was treated as a creep process. It was pointed out that two possible types of creep processes could operate during sintering. In one of these material transport takes place by vacancy diffusion due to a gradient in chemical potential. The vacancy sinks in this diffusion process may be either grain boundaries, as in Herring-Nabarro microcreep, or regions beneath a surface of small radius of curvature. The diffusive transport may be by volume, grain boundary, or surface diffusion. In the other mechanism, creep takes place by slip, i.e., dislocation motion with its rate generally controlled by dislocation climb. One method of distinguishing between these two modes of materials transport is to investigate the creep rate, i.e., the rate of material transport as a function of stress. For material transport by vacancy diffusion, the creep rate is proportional to the stress.' For creep by slip, controlled by dislocation climb, the creep rate is proportional to a power of the stress. For pure metals this power is 4.5;374 for dispersion-strengthened material a fourth power relationship can be derived.5 This difference in the stress dependence of the strain rate is illustrated schematically in Fig. 1, in which the logarithm of strain rate is plotted vs the logarithm of the stress for material transport in a pure metal by vacancy flux and by dislocation climb. The stress range in which the two types of material transport overlap would be expected to be relatively small. In the experiments described by Early and coworkers compacts pressed from spherical copper powder were sintered isothermally under an applied axial external load in a dilatometer. During sintering the magnitude of the applied external load was changed and the rate of axial shrinkage of the compact before and after the load change determined. In order to find the stress dependence of the strain rate the magnitude of the stress acting on the neck area between the spherical particles before and after the load change had to be calculated. This stress is the resultant of the stresses due both to the externally applied load and to surface tension. The stress due to surface tension is a function of the geometry of the powder compacts. It can be determined, at least for simple geometrical arrays,'76 but it is difficult to obtain exact values of the stresses for actual powder compacts when only average values of particle diameters and of neck diameters between particles are available. The calculation of stress and the strain rate-stress relationship is therefore only very approximate.

Jan 1, 1968

By W. Blake McCullogh

It is often written that the purpose of any mining operation is to produce efficiently, safely, and profitably, and always to search for more efficient, safer, and more profitable methods. To provide for continual improvement, an attitude that is not only reasonable but also imperative, there is an obvious need for a high standard of competence among the ranks both of supervision and of those being supervised. It naturally follows that, to achieve this standard, planned training in every level of an organization is a definite necessity. There are many factors involved in the need for training, and the scope of a program is influenced by answers to such questions as: "What is the geographic location of the project?" "What are the duties of each job?" "What is the source of the working force and supervision?" "What are the hiring standards for various jobs?" "What is the availability of trained personnel?" "What is the availability of outside training facilities?" The approach in this chapter will be to consider a need for a maximum of training, and it may be applied by the reader to whatever extent is considered necessary in each individual situation. 14.2-1. Administration. It is a basic responsibility of every supervisor at all levels to train those who work for him. However in a very extensive training program, which involves supervisors and the working force, includes both compulsory and voluntary participation, uses outside and in-plant methods, and where the increasing complexity of jobs requires more specialization, the establishment of a training department is definitely war- ranted. This will consist mainly of instructors for related classroom training and preparation of manuals, etc., and the necessary clerical help. A training staff does not relieve the various departments of their responsibility to train, but it does have facilities, experience, and contacts that are inval-

Jan 1, 1968

By B. B. Rath, Hsun Hu, R. S. Cline

FOLLOWING the techniques used by Beck and co-worker~ "~ the characteristics of selective growth in the recrystallization of a zone-refined aluminum single crystal, rolled 80 pct at -78°C in the (110)[112] orientation, have been studied. The material was 99.999+ pct pure. The as-grown crystal had a resistance ratio, R(298°K) /R(4,2°K), of approximately 5000. The method of preparation of the single crystals and the necessary precautions in handling them during rolling in order to avoid recrystallization in locally distorted regions were described in an earlier paper.3 The rolling texture of this zone-refined aluminum crystal is practically identical with that of less pure aluminum crystals rolle! in the same orientation, i.e., a very sharp (110)[112]. Random nuclei were provided by artificial nuclea-tion by abrading one face of the rolled crystal on 600-grit emery paper in a random fashion. The thin layer of disturbed metal recrystallized at room temperature into fine grains almost immediately. An X-ray diffraction pattern was taken from the abraded surface of the crystal, and the relative intensities of the various reflection peaks were compared with those obtained from a powder specimen. As shown in Fig. 1, the relative intensities of the various peaks from the recrystallized layer varied somewhat from experiment to experiment, depending presumably on the abrading technique. However, the texture of the recrystallized layer produced by this method is nearly as random as that of a powder specimen. Fig. 2 shows the texture determined from the "growth side" (face opposite the abraded surface) of the crystal after it was kept at room temperature for 100 hr. The specimen was only partially recrystallized, as shown by the remaining deformation texture. The new orientations are derived from the recrystallized grains grown through the thickness of the crystal from the "nucleation side" (the abraded surface). Fig. 3 shows the texture after complete recrystallization produced by annealing at 60°C for 1 hr. The arrows indicate 40-deg rotation around the (111) axes of the deformation texture. The microstructure of a completely recrystallized specimen is shown in Fig. 4. As shown in Figs. 2 and 3, the texture of the re-crystallized grains grown from the nucleation side to the growth side is essentially the same as that observed in less pure aluminum' (99.994 pct) and dilute alloyz crystals rolled in the same orientation. How-

Jan 1, 1968

By A. E. Jenkins, L. A. Baker, N. A. Warner

Rates oj decarburization of levilated Fe-C droplets conlaining 5.5 to 0 pct C have been measured at 1660°C. Gas mixtures of 1, 10, and 100 pct 0, with helium diluenl were used at velocities of 12.5 and 62.5 cm per sec. Rates were independent of carbon concentration in the mell and in good agreement with the calculated rule of oxygen diffusion through the gas boundary layer. The effects of flow rale and total pressure are as predicled and the rates are approxitnalely 2.5 times those with CO2 as oxidant. The mass-transfer correlation used incorporaled the efject of natural convection as well as forced conrection. Graphile spheres are shown to oxidize at the same rate as Fe-C droplets under the same experimental codlions. It is concluded that, for high carbon concentrations in the melt, the rate of- decarburizalion is controlled wholly by the rate of gaseous diffusion. Rate measurements with pure CO, are reported for low carbon concentrations where CO bubbles nucleate within the droplet. Under these circumstances the decarburi-zation decreased with carbon concentration and it is proposed that carbon diffusion is significant in conlrolling the decnvburization rate. In an earlier paper1 decarburization rate measurements were reported for levitated Fe-C alloys at 1660°C but with CO2 as the oxidant. The decarburization rate was found to be independent of carbon concentration in the melt but slightly affected by total pressure. The authors were unable to explain the slight pressure effect but in all other respects the results were consistent with control by diffusion in the gas boundary layer. Subsequent work has been directed at finding the reason for the slight pressure effect and whether the kinetics with oxygen as oxidant parallel those with CO2. Recently Ito and Sano2 have shown that with water vapor-argon atmospheres the decarburization rate is gaseous diffusion controlled until an oxide film appears on the surface. In this work the melts were contained in crucibles. MASS TRANSFER IN THE GAS PHASE In the earlier analysis1 only forced-convection mass transfer was considered. Subsequent recognition of the existence of some free-convection mass transfer explained the observed small effect of total pressure on the decarburization rate. Steinberger and Treybal3 and Kinard, Manning, and Manning4 have developed correlations involving the linear addition of the contribution of radial diffusion, free and forced convection. Steinberger and Treybal&apos;s correlation was chosen as the most applicable to the present work since it correlated most of the data available in the literature and handled the low Reynolds number region exceptionally well. The correlation for (Gr&apos;Sc) < 108 is where Nu&apos; is the Nusselt number for mass transfer based upon the total surface of a sphere in an infinite medium, G&apos; is the mean Grashof number for mass transfer defined by Eq. [2], Sc is the Schmidt number (µ/pDAB)f, Re is the sphere Reynolds number (dpu,pf/µf), p is the viscosity of the gas (poise), p is the density of the gas (g cm-3), Dab is the binary diffusivity for the system A-B (sq cm sec-&apos;), dp is the sphere diameter (cm), u is the approach velocity of the gas (cm sec-I), and subscript f denotes the property value is computed at the film temperature Tf defined by Tf = +1/2(To + Tr) where To is the specimen temperature and T, is the approach gas temperature (oK). Natural convection occurs when inhomogeneities exist in gas density. These may be caused by concentration gradients, temperature gradients, or both. In the present work the temperature gradient between the sphere and the bulk gas was very large and in some cases, for example the runs with pure oxygen, the concentration gradient was also appreciable. The Grashof number defined by Mathers, Madden, and piret5 was used since it took account of both temperature and concentration gradients: where Gr&apos; is the Grashof number for mass transfer (p2fgd3|-yA-yA|/µ2f), Gr is the Grashof number for heat transfer (p2f gd3p|To - T,]/µ2fTf), Pr is the Prandtl number (cpµ/k)f, g is the acceleration due to gravity (cm sec-&apos;f, a is the concentration densification coefficient (1/p)(ap/ayA)T, yA is the mole fraction of component A at the gas-metal interface, yA is the mole fraction of component A in the bulk gas stream, cp is the heat capacity of the gas per unit mass at constant pressure (cal g-I OK-&apos;), and k is the thermal conductivity of the gas (cal cm-&apos; sec-1 OK-1). Mathers et al. tested this combined Grashof number

Jan 1, 1968

By Hiroshi Oikawa, R. G. Blake, A. G. Guy

An equatzon has been derivedfor conveniently calculatzng the couvse of homogenzzation in a three-corviDonent solid solutiorz. The necessary assumptions are that the initial distributions of concentration are sinusoidal and that the four interdiffusion coefficients are constant. Employed in the deriuation were the Laplace transform and the fouter Fourier sine transfovwz. The final equation is shown to be in good agveetnent with the experimental results of Kirkaldyet al. on Cu-Sn-Zn alloys. COMMON boundary conditions for representing physical problems are those of the finite solid and of the infinite solid. Many metallurgical phenomena, however, have the geometrical form of a finite pattern reproduced throughout an infinite solid. Precipitation within a uniform matrix and segregation during solidification are examples. The purpose of this treatment is to show that a convenient and useful mathematical analysis is possible in those cases in which the finite pattern can be approximated by a sine function. The particular topic to be considered here is the elimination of segregation by diffusion, but the mathematical model has applicability in many other areas. It should be recalled that the mathematical solution of a typical problem involving a finite solid, such as diffusion into a thin layer, is quite involved.&apos; Various types of solutions are used depending on the degree of advancement of the diffusion process and on the initial conditions. A step function is the simplest initial condition, but even in this case the general solution has the form of an infinite series. Kirkaldy et a1.2 have

Jan 1, 1968

By A. E. Wraith, N. J. Petch, J. D. Embury, E. S. Wright

The two most important parameters controlling the fracture behavior of a solid are its intrinsic properties, e.g.,grain size, and the operative stress system. The latter may be modified in laminates by the presence of weak interfaces. This is studied in notch-impact tests on a mode1 system of mild steel laminates containing a variety of interfaces. The effect of these is evaluated in terms of the ductile/cleavage transition. Two laminate geometries are distinguished, here called "crack-arrester " and "crack-divider". In both, cleavage is inhibited. This arises because of relaxation of a state of triaxial tension. In the crack-avrester laminates, cleavage initiated at a notch is confined to the layer containing the notch. In crack-cliuider laminates, a thick specimen behaves as the Sum of a number of thinner ones. Additional benefit may derive from improved intritnsic propevties of- the lanlinate layers arising from greater deformation in their manufacture. It has long been recognized that the two most important parameters controlling the fracture behavior of solids are their intrinsic properties (e.g., grain size friction stress,3 distribution of second phase particles4) and the operative stress system under which fracture occurs. In solids that show a ductile/cleavage transition, cleavage is favored by the presence of a notch. This is because triaxial tensions, generated by the localized plastic constraint at the notch, are operative when fracture occurs.= Anything that suppresses these triaxial tensions will be unfavorable to cleavage. Such suppression may possibly occur in laminates containing weak interfaces and the purpose of the present paper is to explore this possibility. Two basic laminate geometries, here termed "crack-avrester" and "cvack-divider", are examined. They are illustrated in Fig. 1. With the crack-arrester laminates, there is the possibility that, when the fracture crack approaches the interface, this, if weak, may delaminate due to the tensile stress acting parallel to the plane of the crack.= If this happens, energy will be used in delamination, the crack will be completely blunted, and the triaxial tension associated with the crack will be relaxed. To fracture the second portion of the laminate, crack reinitiation will be necessary and, because of the relaxation of the triaxial tension, this reinitiation will occur under conditions of nearly uniaxial tension, which are unfavorable to cleavage. Thus there is the possibility of cleavage suppression in the second and subsequent subunits of a crack-arrester laminate. With the crack-divider geometry, there is again the possibility of delamination at the interfaces. This will divide the crack into a series of cracks propagating through the individual laminate subunits. If these are sufficiently thin, the triaxial tension will be relaxed towards a state of biaxial tension in each of them. Thus, with the crack-divider laminates, there is again the possibility of cleavage inhibition. In the present work, these possibilities are explored using a notched impact test on mild steel laminates bonded with soft solder, silver solder or copper. Even if delamination does not occur, it is still possible that cleavage may be inhibited in laminates. With the crack-arrester geometry, the cleavage crack in the first layer may be blunted and arrested by plastic deformation in the laminate bond, if this is ductile. Partial relaxation of the stress transmitted ahead of the crack into the second layer will then result and this will reduce the significance of this stress in the fracture of the second layer. With the crack-divider geometry, there cannot be much effect in the absence of delamination unless a large amount of energy is absorbed in rupturing the ductile material. EXPERIMENTAL DETAILS The composition of the mild steel (wt pet) was: 0.04 C, 0.29 Mn, 0.01 Si, 0.006 P, 0.008 S. "As-received" plate was annealed for 2 hr at 900°C and slowly cooled to give a grain size of 0.04 mm. The laminates were made by brazing or soldering together mild steel plates 8 by 3 in. by various thicknesses. These were obtained from the annealed plate by machining, so that the intrinsic material properties were .kept constant. Laminates containing two to six steel layers were studied using standard Charpy V-notch specimens cut from the bonded plates. Standard homogeneous specimens from the annealed plate and subsize ones from the laminate components

Jan 1, 1968

By J. H. Swisher

The solubility of sulfur and rate of solution of sulfur in pure Lron were measured in H2S + H2 and H2S + H2 H2O gas mixtures. The solubility and diffusivity of sulfur at 1410°Care 0.13 pet S and 1.0 x 10-5 sq cm per sec, respectively. The solubility iS the same, but the rate of sulfurization is slower in the presence of H2O in the reacting gas. Under these conditions, the over-all rate is controlled jointly by a slow surface reaction and by solid-state diffusion; the mechanism for the surface reaction has not been identified. KNOWLEDGE of the behavior of sulfur in solid iron is desirable for the metallurgy of such products as free machining steel, where a high sulfur level is required, and inclusion-free high-strength steels, where the sulfur specifications are very low. The present investigation was undertaken to check previously reported values for sulfur solubility and diffusivity in 6 iron, and to study the poisoning effect of chemisorbed oxygen on sulfurization kinetics in H2-H2S-H2O gas mixtures. All of the experiments were performed at 1410°C. The thermodynamic behavior of sulfur in 6 iron was the subject of a paper by Rosenqvist and Dunicz.&apos; The sulfur solubility at 1400" and 1500°C was determined by equilibrating pure iron specimens with H2-H2S gas mixtures. The maximum solubility of sulfur in 6 iron was alsc determined by Barloga, Bock, and parlee2 by reacting iron wires with sulfur in sealed capsules. In another investigation, the diffusion coefficient of sulfur in 6 iron at temperatures up to 1450°C was measured by Seibel.3 The method used was to measure sulfur concentration profiles in diffusion couples containing radioactive sulfur EXPERIMENTAL Apparatus. A vertical resistance furnace wound with molybdenum wire and containing a recrystallized alumina reaction rube was used for the experiments. The hot zone in the furnace was approximately 2 in. long with a temperature variation of ±3oC. The hot zone temperature was automatically controlled to within ±2°C, and the test temperature was measured with a pt/Pt-10 pet Rh thermocouple before and after each experiment. Flow rates of the reacting gases were obtained using capillary flow meters. Materials. The source of H2S in the gas train was a premixed cylinder containing 5 pet H2S in H2. This mixture then was diluted with additional hydrogen and argon. In some experiments, water vapor was introduced by passing hydrogen and argon through a column containing 10 pet anhydrous oxalic acid and 90 pet oxalic acid dihydrate. The vapor pressure of water above this mixture is well-known.4 Argon was used as a diluent to minimize thermal segregation of H2S in the furnace5 and to reach higher H2O:H2 ratios than could be obtained in mixtures of H2 and H2S alone. Argon was purified by passage over copper chips at 350°C and subsequently over anhydrone. Hydrogen was purified by passage over platinized asbestos at 450°C and then over anhydrone. The H2-H2S mixture was purified by passage over platinized asbestos and then over P2O5. The specimen stock was made by melting and vacuum-carbon deoxidizing electrolytic "Plastiron" in a zirconia crucible. The principal impurities are listed in Table I. In some of the equilibrium experiments, six-pass zone-refined iron was used to minimize impurity side effects. This zone-refined iron had a total impurity level of about 25 ppm. Procedure. Specimens were annealed in hydrogen for a period of at least 2 hr at the beginning of each experiment. The specimens were held in the reacting gas for times varying between 10 min and 17 hr, and cooled to room temperature in a water-cooled stainless-steel block at the bottom of the furnace. The pH2S/pH2 ratios reported are those for gas equilibrium at 1410°C. Calculations based on available thermodynamic data8 showed that the only other gaseous8 species that formed in significant amounts in the furnace were S2 and S. Even when water vapor was introduced into the gas mixture, the concentrations of SO2, SO, and so forth, were negligible. The initial partial pressure of H2S was therefore corrected for its partial dissociation to S2 and S in determining the equi-

Jan 1, 1968

By S. Mukai, Y. Shah, T. Zshikawa, T. Wakamtsu

In order to recover coal concentrate of low ash and low iron content, the electrostatic separation of coal was studied. It is more successful in the corona discharge field to recover the coal concentrate of low ash and low iron content than in the field without corona discharge. The effect of humidity on the electrostatic separation of coal was then studied. From the experimental results, it was clear that the electrostatic separation was excellent in about 60% relative humidity of atmosphere. Thus, the separation of vitrite from coal is practicable by electrostatic separation. In recent years the demand for high quality coal containing low ash, low iron, and low sulfur has increased. To fulfill this requirement, a higher grade coal concentrate must be produced. Study on the electrostatic separation of coal has been performed for several years in the author&apos;s laboratory. From the results of this research, it was considered that the behavior of coal particles in the electrostatic field relates closely to the ash and iron content in coal. In the present paper, the electrostatic separation of coal in corona discharge field was studied in order to recover the high quality coal concentrate and then the effect of humidity on the electrostatic separation was investigated. PREPARATION OF COAL SAMPLES The coals from the Akabira mine, the Kushiro mine, the Miike mine, and the Oshima mine which are famous coal mines in Japan were used in this study. The ash contents of these coals are shown in Table I. From the results of the analysis of the coal samples by the Norelco X-ray diffractometer, it is recognized that the Miike coal includes mainly pyrite, quartz, kaoline, calcite, and epidote; the Kushiro coal: kaoline, quartz, and montmorillonite, and the Oshima coal: siderite, dolomite, and other substances. For the preparation of samples, the coarse pieces of coal were crushed to about 2 mm in diam and then ground in an agator mortar. The ground products were sieved and fractions of 10 — 14 mesh, 14 — 20 mesh, 20-28 mesh, and 28-35 mesh were prepared, respectively. APPARATUS OF ELECTROSTATIC SEPARATION The principal part of the apparatus of the electrostatic separation used in the experiments is shown in Fig. 1. In order to generate the corona discharge field, a needle-shaped electrode combined with a pole electrode is installed as the high tension electrode. In the case of investigating the effects of the humidity on the electrostatic separation of coal, the needle-shaped electrode was combined with a plate electrode instead of the pole electrode as shown in Fig. 2. The pole or the plate electrode was installed to promote the repelling of the charged particles by producing the electrostatic field between this electrode and the grounded roller. It seems to be very useful on the coal separation to install these combined high tension electrodes. SEPARATION OF COAL PARTICLES IN CORONA DISCHARGE FIELD The separation testings on the coal samples in the corona discharge field were performed by the apparatus as shown in Fig. 1. These experiments were carried out under the following conditions: feed size 20 — 28 mesh, room temperature, normal humidity and applied voltage 15-20 KV, and the combined electrodes including the needle-shaped electrode were negatively charged. The results of these testings are

Jan 1, 1968

The amount of liquid retained in a porous bed is determined by weighing a column containing the bed.The column is attached to the free end of a cantilevered beam, and changes in weight are determined by calibrated strain gauges (which form a resistance bridge) attached near the fixed cnd of the beam. By coupling the output from the strain gauges to an amplifier and a recorder, a continuous record of changes in the drainage characteristics of the bed may be obtained.

Jan 1, 1968

By W. J. Moore, E. M. Swiggard, H. Shenker

Beryllium is the most soluble of the double-acceptor impurities in germanium; the solubility is at least 1 x 10 19 atoms cm3. Photoconductive, optical, and electrical measurements were made on a set of Ge:Be samples grown without other intentionally added imp~ivities. The excited-states spectrum of beryllium in germanium was determined both in zero field and in magnetic fields up to 30 kc. It was found that the absorption 0-f lines in the vicinity of the G line increased markedly with increasing magnetic field. The ioniza-tion energy of neutral beryllium in germanium was determined to be 24.3 * 0.1 mez: using the excited-states spectrum. An infrared detector using a Ge:Be element was found to have a normalized detectivity D* (50 p, 1000 cps, 1 cps) of 9 X ldO cm-~ps"~-w-&apos;. The Ge:Be sambles exhibited low-field breakdown and inibzirity band conduction effects at low temperatures. WHILE the properties of most dopants in germanium have been thoroughly investigated, the properties of beryllium in germanium have had relatively little attention. Much of the work that has been done&apos; has been concerned with the properties of singly ionized beryllium in germanium. The purpose of the present work was to determine the photoconductive and electrical properties of beryllium-doped germanium (Ge:~e) with a small concentration of other electrically active impurities. Ge:Be is of special interest since beryllium is the most soluble of the known double-acceptor impurities in germanium. MATERIALS PREPARATION A set of &:Be crystals with beryllium concentrations between 5 x 1013 and 1x 10&apos;&apos; cmm3 and without other intentionally added impurities was grown in a hydrogen atmosphere by the horizontal zone-refining techniques described by Swiggard and Shenker.2 The segregation coefficient of beryllium in germanium was found to be about 0.07 and its maximum solubility was found to be greater than 1 x 10&apos;&apos; atoms cm-3 which is in agreement with previous results.&apos; Most of the crystals were found to have a small net concentration of shallow acceptors; for example, a crystal having a beryllium concentration of 1.1 X 1016 cm-3 was found to have a net concentration of shallow acceptors of less than 1.5 X 1013 cm-3. Ingots designed to have a beryllium concentration of 1 x 1017 cm-3 or less exhibited a loss of electrically active beryllium. That is, the beryllium concentration was lower than expected and the decrease of the beryllium concentration along the length of the ingot was much larger than expected. It is hypothesized that this effect is due to the oxidation of the beryllium by the residual oxygen in the system. This effect is similar to but not as severe as the effect observed with boron in germani~m.3, 4 OPTICAL ABSORPTION SPECTRUM The excited-states spectrum of neutral beryllium atoms in germanium was studied by measuring the infrared optical absorption spectrum. A typical spectrum is shown in Fig. 1; the labeling of the absorption lines follows that of Fisher and Fan.* The spacings between the observed lines and the D line are nearly equal to the corresponding spacings for the other ac -ceptors in germanium.5-7 By the use of the theoretical result67&apos; that the neutral impurity ionization energy is 2.53 mev larger than the energy of the D line, the ionization energy of neutral beryllium in germanium was determined to be 24.3 * 0.1 mev at 4.2"K. This method yields a more precise value of the impurity ionization energy than the usual Hall effect method.&apos; The absorption spectrum of Ge:Be was also measured as a function of magnetic field using a magnetic field parallel to the incident radiation and using unpolarized radiation. A typical spectrum taken at 30 kG is shown in Fig. 2. An unexpected observation is that the absorption of the lines in the vicinity of the G line (there is a strong possibility that some of these lines may be associated with lines other than the G line) increases with magnetic field. RESISTIVITY AND HALL DATA Measurements of Hall voltage vs temperature were made on several of the samples. The thermal activa-

Jan 1, 1968