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By S. Feuerstein, L. Rice

The effect of low pressures on the flow and fracture behavior of molybdenum is described. For poly crystalline samples, room-temperature tensile tests indicate greater ductility under 10 Torr than under intermediate pressures up to and including atmospheric pressure (760 Torr). In addition, tests conducted at 760 Torr under atmospheres of air, dry nitrogen, and purified argon exhibited no apparent difference in mechanical properties. Critical tests involving baking in situ as well as those involving single-crystal deformation further imply that the ductility effect is a pressure-dependent phenomenon related only to the fracture process. This dependency is discussed in terms of adsorption and diffusion contributions. THE effect of very low pressures on material properties has heretofore been presumed to be important only for substances possessing relatively high vapor pressures at ambient temperatures. Research has therefore been concentrated primarily on organic solids and liquids, and in some instances on metals such as zinc and cadmium. Most vacuum-effect studies' on the mechanical behavior of metals have been performed under conditions of either cyclic loading or creep rupture at elevated temperatures, i.e., over extended time periods. These studies were not restricted to high vapor pressure materials but also encompassed such metals as gold, copper, and nickel. Very little concern, however, was placed upon the importance of a vacuum environment on the mechanical behavior of metals subjected to a simple unidirectional deformation at ambient temperatures. A tension test is generally of short duration as compared to a creep test, and at room temperature vacuum effects if any would be expected to be surface-limited. In early 1963, Kramer and podlaseck2 reported a change in the bulk flow behavior of aluminum single crystals during room-temperature tension tests. The deformations were performed under pressure conditions of 760 to 3.4 X 10-8 Torr and indicated for the first time a vacuum surface effect contributing to the bulk tensile behavior of metal specimens. As a consequence, an experimental program was initiated in this Laboratory to study the effects of ultrahigh-vacuum conditions on the mechanical behavior of metals. The results of a preliminary study on poly-crystalline molybdenum3 revealed, unlike Kramer's observations of changes in the stress-strain behavior, only an increased ductility under ultrahigh vacuum. Flow behaviors were nearly identical for all tests re- gardless of pressure. This paper presents comprehensive results obtained in this area of research. 1) EXPERIMENTAL PROCEDURE Three material categories were used in this study: sintered and are-cast polycrystalline molybdenum of nominal purity 99.93+ pct and single-pass electron-beam zone-refined molybdenum single crystals having a nominal purity level of 99.99+ pct. The interstitial levels (weight percent) as determined by the Materials Testing Laboratories, Division of Magnaflux Corp., were as follows: sintered molybdenum (C— 0.005, H—0.0004, O—0.015, N—0.008); and arc-cast molybdenum (C-0.0038, H-0.0003, O-0.015, N-0.023). Single-crystal molybdenum obtained from Materials Research Corp. had a typical interstitial analysis of C-0.0015, H-0.00007, O—0.00045, and N-0.0001. Tensile specimens having a 5 mm diam by 50.8 mm length were prepared from these materials. An average grain diameter of 0.059 mm was obtained for the sintered specimens following a 4-hr, 1600°C heat treatment. Grain sizes from 0.019 to 0.149 mm were obtained in the arc-cast specimens following heat treatments from 1100° to 1600°C for 1 hr. This series of specimens was used exclusively for the grain-size effect studies. All samples were electrolytically polished in 97 pct sulfuric acid solution prior to testing. Experiments were performed at room temperature in an ion-pumped ultrahigh-vacuum system positioned in an Instron tensile machine, Fig. 1. A constant strain rate of 4.2 x 10-4 sec-1 as derived from crosshead displacement was assumed for the deformations. Starting vacuums ranged from 2 to 0.5 X 10-10 Torr. These pressure measurements were made using corrected values4 of an NRC Redhead gage. Comparative readings were also made against a G.E. triggered dis-

Jan 1, 1967

By N. F. Schulz, H. A. Lex, J. D. Zetterstrom

A green ball of iron ore faces many perils from the time it is formed until it finally emerges from the pelletizing furnace as a hardened pellet. For instance, if the rate of heat transfer into a ball is sufficient to produce vapor from either the free or combined water more rapidly than it can escape at a tolerable pressure, the ball may split, spall, or even explode, a failure commonly known as decrepitation. To avoid such failures, one must either limit the rate of heat transfer during the drying and preheating stages, at the expense of production rates, or improve the decrepitation resistance of the green balls. The latter remedy may often be accomplished through changes in ore preparation, balling procedures, or the judicious use of binders or other additives. INTRODUCTION Pelletization has become established as an especially desirable method for the agglomeration of fine taconite concentrates and it promises to be equally satisfactory for improving the physical structures of certain natural ores. A high-quality pelletized iron ore consists of uniformly sized spheres, usually about 1/2-in. diam, which are strong enough to resist abrasion and breakage during handling and which reduce well without disintegration in the blast furnace. The unfired agglomerates, "green balls", are subject to several destructive effects that must be avoided or minimized if a high-quality product is to be obtained by pelletization. Among these are abrasion and impact deformation or breakage during handling of the wet green balls, deformation and breakage by compressive forces in the bed of ore in the pel-letizing furnace, decrepitation during drying and preheating, wind erosion, and radial cracking at firing temperatures. Moisture condensation from the warm saturated gases downstream from the drying zone on wet, cool balls may cause bed collapse if it becomes excessive. Decrepitation is defined as the sudden disintegration of green balls, usually with an audible pop, that occurs when they are heated too rapidly during the drying or preheating stages of the pelletization process. The extent of ball disintegration may vary from merely splitting off a small fragment to almost total disintegration into the original ore particles making up the ball. Such ball destruction results in a decreased yield of pellets, and the fragments, which also tend to interfere by obstructing the gas flow through the bed, must eventually be screened from the fired product and recycled. The closely related type of ball failure that sometimes occurs during the high temperature firing stage, resulting in radial cracks without fragmentation, was not considered to be decrepitation for the purpose of this investigation. Failure by decrepitation is not usually a serious problem in the pelletization of taconite concentrates. The problem is significant, however, in the pelletization of some natural ores, especially those containing hydrous iron oxides. In some instances, economicd production rates cannot be maintained if the drying and preheating rates are slowed down enough to avoid decrepitation. OBJECTIVES This investigation was undertaken to: (1) Develop a practical laboratory means for quantitatively measuring the tendency for green balls to decrepitate in iron ore pelletizing furnaces, and (2) Investigate the causes and cures of ball decrepitation. MATERIALS Two iron ores were used in the work reported here: a taconite concentrate at 90% minus 325 mesh, containing 65.0% Fe, 8.4% SiO2, and no loss-on-ignition; and a crude oxidized ore at 54% minus 325 mesh, containing 59.1% Fe, 3.6% SiO2, 1.1% A12O3, and 9.5% loss-on-ignition. For a special test of effect of particle size distribution on decrepitation, two other

Jan 1, 1967

By Ursula E. Wolff

The precipitation of carbides from an alloy containing 33 pct Ni, 21 pct Cr, balance iron, was investigated electron microscopically by means of extraction replicas and thinned metal foils. Annealing temperatures ranged from 565°to 870°C and up to several thousand hours. M23C6 precipitated in pain boundaries, incoherent and coherent twin boundaries in that sequence. The orientation relationship between carbides and austenite matrix was determined and correlated with the morphology of the carbides and with the type of boundary in which precipitation occurred. In large-angle grain boundaries, as well as in coherent twin boundaries, the carbides had the same orientation as one of the adjacent pains. These carbides formed sheets of individual flakes with shapes related to the orientation of the boundary. In incoherent twin boundaries carbides precipitated in ribbons composed of pavallel rods. An unidentified subcarbide was found to precede precipitation of M23C6 in these boundaries. The M 23 C6 rods had a kind of fiber texture with (110) parallel to the long dimension of the rods and ribbon, and with orientations of both of the adjacent twin-related austenite crystals Predominant in the texture of the carbide. A hard sphere crystal model has been used to discuss orientation and morphology of the carbides in terms of free volume and vacancies available in the boundaries. A number of papers have dealt with the morphology of chromium carbide (M23 C6) precipitated in austenitic stainless steels.1"7 In all these investigations, the carbides were examined in the electron microscope by means of extraction replicas. With this technique, the carbides retain the spatial distribution they had in the bulk sample. However, since the matrix is dissolved in the process, the particles can turn in an unpredictable way; and the orientation relationship between matrix and carbides cannot be established. In this paper the results of studies on extraction replicas and on thinned metal foils are reported. These studies were undertaken to determine the matrix-to-car bide orientation relationship, and to correlate the orientation of the carbides with their morphology. PROCEDURE The material used was an austenitic alloy with 33 pct Ni, 21 pct Cr, balance iron, containing approximately 0.05 pct C. Coupons of 1.25-mm sheet were first solution-annealed at 1050°C for 15 min and air-cooled. Then, to precipitate the carbides, samples were isothermally annealed in the range from 565" to 870°C for times up to several thousand hours. All further specimen-preparation procedures were carried out after the final anneal. Carbon extraction replicas from polished and etched surfaces were made with 10 pct bromine in methyl alcohol.' Thin foils were prepared from punched-out 3-mm-diam disksg which fit into the electron-microscope holder. The disks were prethinned by grinding to approximately 0.5 mm thickness, and then electro-polished in a polytetrafluoroethylene holder1' with a solution containing 5 pct perchloric acid in acetic acid to which 10 g per 1 Cro3 and 5 g per 1 nickel chloride were added (etchant modified from that of Briers et al."). This solution dissolves neither the carbides nor the austenite around the carbides preferentially. By using extraction replicas, electron micrographs and selected-area electron-diffraction patterns were taken from the same carbide arrays. By using thin foils, electron micrographs were made from a grain boundary area containing carbides. Electron-diffraction patterns were then taken from the same area and from each of the adjacent grains separately. In this manner, the orientation of each grain could be determined without interference by the carbide pattern. A peculiarity of extraction replicas should be pointed out. After the matrix is etched away, the carbide arrays float freely in the etching and washing solutions, and are held in place only at the anchoring points in the carbon replica. When the replica is picked up with a screen the carbide arrays tend to flip to one side. Thus, while the surface features are preserved, the original arrangement of the carbides may severely and unpredictably be disturbed whenever the specimen contains large amounts of interconnected carbides. Nevertheless, it is possible to correlate the different morphologies of the carbides with the type of boundary in which they have precipitated. RESULTS 1) Extraction Replicas. Fig. 1 shows that the grain boundaries usually are curved, multicornered surfaces of random orientation. The coherent twin boundaries (which are (111) planes) cut a grain into parallel slices. Incoherent twin boundaries occur at the ends and on the steps of twins and are often narrow, parallel-sided strips which are much longer than they are wide. Different morphologies can clearly be distinguished for the M23Ce carbides precipitated in each of these types of boundaries, and agree well with those observed by kinzel.2 The kinetics of this precipitation has been investigated." The first carbides precipitate in junctions of three grain boundaries and fan out from there into the adjoining boundary surfaces, Fig. 2(a). These carbides are oriented randomly, Fig. 2(b), and become coarser and thicker as annealing time increases. The large-angle grain boundaries are next to fill

Jan 1, 1967

By R. W. Kraft, L. D. Graham

The process of' spheroidization, or more properly coarsening, of Al-CuAl,eutectic alloy specimens with various initial microstructures was studied by quantitative metallographic and X-ray diffraction techniques. By measuring the rale at which specimens with a very fine dispersion of phases (produced by quenching molten droplets of the alloy in water) coarsened it uias determined that the rate-controlling mechanism for coarsening was diffusion, probably of aluminum in the aluminum-rich phase. The lamellae in specimens with a high degree of microstructural and cr-ystallog/uphic anisotropy (produced hy unidirectional solidification of ingots) thickened during heat treatment by recession of the CuAl, platelets from jaulted regzons, yet the specinlens retained a very high degree of. anisotropy after prolonged heat treatments at a temperature within 8°C of the eutectic temperature. In such specimens the crystallographic orientation relationship between the phases remained constant and no change in the crystallographic substructure occurred. Based on these observations a model was developed for the coarsening—or rate of' thicken-ing—oj- the lamellar structures which predicts that the rate of decrease of interface area is proportional to the square of lamellar interface area. Experiments with degenerate and very coarse lamellar microstruc -tures preduced by extremely slow unidirectional solidification) indicate that initial microstructure is a most important factor governing the final micro-structure after heat treatment. The particle size and shape of dispersed phases are important parameters affecting the properties of a wide variety of two-phase materials. As is well-known, varietythe dispersed-phase particles tend to coarsen at appropriately high temperatures because the interface energy of the system is reduced by the concomitant reduction in interface area. The phenomenon of

Jan 1, 1967

By H. R. Ogden, E. S. Bartlett, A. G. Imgram

Unmodified disilicide coatirigs were applied to sheet-tensile specimens ofCb-Dg3 and Mo-TZM veJractovy- metal alloys. Coating thickness, degree of coating-substrate interdiffusion, and specimen geonzetry (notched and plain were included in the variables studied. Tensile tests were made to determine the ductile-lo-brittle transition temperature. The disilicide coating modestly increased the transition temperatlre of TZM, but had no effect on 043. Neither material condition (recrystallized or stress-velieved) nor specimen geometry (notched or unnotched) significantly altered the effects of coatings on the transilion temperatures of. the alloys. Cracks in the brittle coatings did not propagate into the substrate, and fracture modes appeared to be the same for both un-coated and coated specimens. MOST potential structural applications for refractory metals and alloys involve exposures to oxidizing environments at elevated temperatures. The general lack of oxidation resistance of these metals will require protective coatings to allow fulfillment of their potential. Currently preferred coatings for the oxidation protection of refractory metals are brittle intermetallic aluminides or silicides. These are typically formed on the surface of the refractory-metal substrate by a diffusion reaction between the substrate and a gaseous or liquid medium that is rich in aluminum or silicon. Because of the brittleness of these coatings, they will sustain no plastic deformation at low temperatures. They are frequently cracked by cooling from the coating temperature because of the thermal-expansion mismatch with the substrate alloy. Even if they survive cooling intact, they crack rather than sustain deformation under load at low temperatures. Thus, when a coated refractory metal is strained beyond the elastic limit of the coating at low temperatures, the mechanical environment of the substrate would include both static and dynamic cracks. These might be expected to influence the flow and fracture behavior of the substrate. This could be manifested in an altered fracture mode and/or an increase in the normal ductile-to-brittle transition temperature of the refractory-metal substrate. This paper presents the results of a research program that was conducted to determine the influence of the presence of a brittle surface coating on the low-strain-rate tensile behavior of typical refractory metals at low temperatures. EXPERIMENTAL PROCEDURES Material Preparation. Thirty-mil-thick sheets of molybdenum TZM alloy (Mo-0.5Ti-O.1Zr) and colum-bium D43 alloy (Cb-IOW-1Zr-O.1C) were obtained commercially. These alloys were selected as substrate materials representing two classes of materials important in current refractory-metal technology. The TZM was in the stress-relieved condition, and exhibited a heavily fibered grain structure. The D43 had been processed by the duPont "optimum" fabrication schedule,' and exhibited slightly elongated grains typical of this process. Tensile specimens of two geometries were prepared from these materials: 1) plain specimens with 0.2-in.-wide 1.0-in.-long gage sections; 2) specimens similar to above, but with a 0.06-in.-diam hole drilled in the center of the gage section, providing a stress concentration factor, Kt, of 2.5. The "notch" geometry was selected to represent a typical condition of a rivet hole or other geometric discontinuities as might be encountered in various applications. Machined specimens were degreased, with a final rinse in acetone, prior to the application of coatings. Specimens of each substrate and configuration were pack-siliconizedin a particulate mixture of 80 pct A1203, 17 pct Si, and 3 pct NaF. Specimens were embedded in this mix (contained in graphite retorts) and coated in an electrically heated argon-atmosphere furnace under time-temperature conditions to effect nominal 1- and 3-mil-thick silicide coatings: Coating Thickness, mils Thermal Treatment 0.6 to 1.4 24 hr at 982°C 2.4 to 3.2 48 hr at 1093°C Coating kinetics were similar for both the TZM and D43 substrates. These treatments had little or no visible effect on the substrate microstructure as determined by optical metallography. The coatings on TZM were essentially single-phase unmodified disilicides, while those on D43 showed substantial evidence of modification by proportionate reaction with the respective substrate elements or phases, as shown in Fig. 1. It was recognized that these coatings might not be particularly desirable regarding protective capability. However, it was desired to circumvent possible inter -ferring chemical interaction with the substrate by pack additives such as chromium, titanium, boron, aluminum, and other elements that typify the better protective coatings for these materials.' Thus, the results presented apply specifically to the simple silicide coatings investigated. They may not be rep-

Jan 1, 1967

By E. P. Williams

"Prince Edward Island, Canada's smallest Maritime Province, is located in the southwestern part of the Gulf of St. Lawrence. The Province is more or less centrally located in the Maritimes Basin, a large intermontane basin within the Appalachian orogenic belt. The Maritimes Basin is subdivided into sub-basins and uplifts which exhibit two dominant structural trends: east and northeast. The Basin is known to be petroliferous because of the seeps, shows, oil shales and albertite found in southern New Brunswick and northern Nova Scotia and the gas and oil produced from the Stony Creek field near Moncton, New Brunswick.Permian beds are exposed on the Island, mostly along sea-cliffs. A maximum thickness of about 5,000 feet of red beds -shales, sandstones and conglomerates -make up the sequence. Over most of the Island, the Permian section is much thinner. Four key wells (Mississippian tests) and several shallower tests have been drilled. The Pennsylvanian-Mississippian section thickens rapidly off the Port Hill Uplift at the northwest, where it is less than 4,600 feet thick, and continues to thicken to about 20,000 feet in the Cumberland Basin at the southeast. Geological and geophysical data combine to give us the structural picture of the deeper beds.Prospective reservoir rocks are primarily in the Missis-sippian Horton and Windsor groups. Prospects are:-1. on or over structural highs in the basement; 2. on anticlines or fault highs; 3. over or peripheral to salt domes or salt-core anticlines; 4. at truncation pinchouts of Mississippian prospective beds; 5. in basal sandstone or granite wash on the pre-Carboni-ferous basement; and 6. in facies traps at changes from sandstone to shale or porous to tight carbonate rocks."

Jan 1, 1967

By Donald M. Keagy

How many times have you said or heard someone say, 'What are you doing right now?" And how many times have you heard the reply, "Breathing air!" Probably never, or at most only a few times in a facetious vein. Breathing air is absolutely necessary to sustain human life, and yet most of us take it completely for granted. Beginning ten to fifteen years ago there was growing concern on the part of the general public that pollution of the air is a threat to man's health and welfare. Concurrently much thought and effort was devoted to the task of defining and resolving the problem of air pollution. In the course of this effort it has become quite clear that our National policy in this regard should be founded upon three basic axioms: (1) Action should not be postponed until emergency conditions make it compulsory; (2) The air cannot be purified after it is polluted, and (3) Air pollution control cannot be accomplished without close cooperation among all levels of government, industry, and the public.

Jan 1, 1967

By F. Habashi

Conclusive evidence is given showing that the dissolution of gold in cyanide solution follows mainly the over-all equation A similar equation can also be written for the dissolution of silver. Theoretical derivation of the velocity equation for this reaction has been obtained, which describes quantitatively the experimental facts. The equation is as follows: where [CN-] and [O2] = the concentrations (in moles/ml) of cyanide and dissolved oxygen, respectively. DcN- and Do2 = the diffusion coefficients of cyanide and dissolved oxygen; 1.83 x 10-5 and 2.76 x 10-5 cm2 sec-1, respectively. A = the surface area of the metal in contact with the aqueous phase, in cm S = the thickness of the boundary layer; varies between 2 and 9 x 10-3 cm, depending on the speed and method of agitation. Rate being expressed in g. equiv. sec-1. INTRODUCTION During recent years a number of papers have been published on the kinetics of dissolution of gold and silver in cyanide solution.1,6 The authors agree that the rate of dissolution is diffusion-controlled, but disagree regarding the mechanism of the reaction. Some authors'-3 support the Bodlander equations: The apparently conflicting results, when critically reviewed, are concordant and lead to the conclusion that the proper equation for the dissolution reaction should be only Eq. 1. This conclusion is based on the following facts: 1) For every 2.2 equivalents of metal dissolved one mole O2 was consumed. 2) For every 1 equivalent of metal dissolved, 2 moles of cyanide were consumed.' 3) Hydrogen peroxide is formed during the dissolution of gold or silver, and for every 2.2 equivalents of metal dissolved, one mole H2O2 was produced.1,2 The fact that Kudryk and Kellogg4 did not detect H2O2 during the dissolution of gold should not throw doubt on the many affirmative reports of other investigators. Lund2 has shown that depending on the crystalline nature of the silver surface, (e.g. method of etching the sample) H2O2 may undergo catalytic decomposition heterogeneously according to: Further Kudryk and Kellogg4 carried out their experiments in the presence of 0.5% KC1 to achieve a greater electrolytic conductivity, and Matsudaira7 has shown that H2O2 is catalytically decomposed (homogeneously) in the presence of C1- ion in alkaline solution. 4) Experiments carried out by Boonstra8 and Lund2 showed that the dissolution of gold and silver respectively in KCN + H2O2 in the absence of oxygen was a slow process. Thus the reaction takes place to a minor extent only. Further kinetic studies showed that: 1) The rate of dissolution depends on the surface area of the metal in contact with the liquid phase, thus indicating that the process of dissolution is a heterogeneous process. 2) The rate of dissolution depends on the speed of stirring,5,6 thus indicating that the process is controlled by a physical phenomenon.

Jan 1, 1967

By d&apos, Kathleen J. Amico

This summary appears in Minerals Yearbook volumes I-II, and III, which cover mineral production in the United States, its island possessions, the Canal Zone, and the Commonweath of Puerto Rico, as well as the principal minerals imported into and exported from the United States. The sections of this chapter and the area chapters in volume III contain further details on production. A summary table comparing world and U.S. mineral production also is included. Mineral production may be measured at any of several stages of extraction and processing. The stage of measurement used in the chapter is normally what is termed "mine output." It usually refers to minerals in the form in which they are first extracted from the ground, but customarily includes for some minerals the product of auxiliary processing operations at or near mines.

Jan 1, 1967

By E. G. King

The Bureau of Mines made experimental determinations of the heats of formation of forsterite and chrysotile at 298.15° K. The heat capacities of two polymorphs of serpentine, chrysotile and antigorite, were measured over the temperature range from 50° to 298° K and the entropies at 298.15° K were evaluated. The heat content of antigorite above 298.15° K was measured to 850° K. These thermochemical data were combined with other pertinent data to give heat and free energy of formation values at high temperatures. Free energy values are given for the reaction, forsterite + water = brucite + serpentine at different temperatures and pressures.

Jan 1, 1967

By D. E. Stephenson. Discussion by R. G. K. Morrison, L. Obert

R. G. K. Morrison (Chairman, Dept. of Mining Engineering and Applied Geophysics, McGill University, Montreal, Que., Canada) - The discing of drill core has been a recognized pressure phenomenon for many years but only recently has an interest been taken in the mechanism involved. The work of Jaeger and Cook is referred to in the text. The authors have now advanced the study to establish, within certain loading limitations, a direct relationship between axial and radial stress at failure. This is an important contribution. In mines generally, where pressure conditions result in the spalling of openings, the faces of drifts and crosscuts, on scaling, usually show a concavity with respect to the opening very similar to the face of the drill hole after the separation of the stub. The same holds for shaft sinks. This suggests a similarity between the mechanism of the discing of core and that of the spalling of an opening, under pressure, to develop a more stable outline. The latter, commonly regarded as shear, is the most conspicuous type of failure observed in

Jan 1, 1967

By D. Bienstock

The use of alkalized alumina in removing sulfur dioxide from a coal-combustion flue gas at 625° F was investigated on a pilot plant scale. The absorber was 26 feet long and 1.6 inches ED. Counter-current gas-solids flow at gas velocities of 8 to 15 ft/sec in the presence and absence of baffles, as well as solids entrainment at gas velocities of 20 to 23 ft/sec with solids recycle, were employed. The spent absorbent as regenerated as fixed bed with the reducing gases--reformed natural .7.7d hydrogen. Of absorption-regeneration were successful completed using the alkalized alumina rolled into spherical granules 10 to 16 mesh. There was no loss in activity of absorbent toward SO2 with a modest attrition equivalent to 0.l percent of the solids feed. Supporting studies were conducted on the effect of the sodium content in the absorbent, the composition of the reducing gas, thermal treatment to increase absorbent hardness, and removal of absorbed chlorine from the absorbent. A mathematical model was formulated to describe the removal of SO2 by alkalized aluminum from fixed and falling beds.

Jan 1, 1967

By D. T. Peters, C. R. Cupp

Aging of commercial 18 pct Ni maraging steel and of related binary, ternary, and quaternary alloys has been studied by electrical resistivity, X-ray diffrac-tion, and hardness measurements. The aging process is in three stages: 1) recovery of martensite; 2) two precipitation reactions; 3) formation of nickel- rich austenite. The main objective of this work was to discover the nature of the Co-Mu interaction. Addition of cobalt to the Fe-18 pct Ni-5pct Mo alloy results in acceleration of the pvecipitation reaction by increasing the super-sat~lration 0f molybdenum. The cobalt-containing al- loys show no incubation period for the precipitation reaction, but the alloy without cobalt shows an initial slow reaction. These results are interpreted in terms of precipitation on dislocations. At low aging temperatures, the presence of cobalt leads to the appearance of a second type of precipitate which is a particularly effective hardener. Cobalt was found to retard the formation of austenite. Overaging is a combination of classical overaging and the formation of austenite in the structure. he- activation energy for the precipitation reaction determined from resistivity ,measurements is 42.8 kcal per mole and the growth of the precipitate is found to obey at law at high tenzperatures and a tU3 law at low temperatures. HE mechanism of strengthening of the 18 pct Ni maraging steels has been studied extensively since 1962.'-? The strengthening is due to precipitation hardening of the martensitic matrix. The main precipitate is an inter metallic compound involving molybdenum, but there is disagreement about its identity.

Jan 1, 1967

By George H. K. Schenck

Diminishing returns in management's fight to lower manufacturing expenses have added luster to savings that can be achieved in delivered costs through creative management of the distribution function. This is especially true for companies engaged in the production of bulk commodities, for which transport costs may represent 25 to 50% or more of total delivered price, A. E. Cascino, vice president of International Minerals and Chemical Corporation, recently gave an example of why top management in his firm is concerned with distribution: "The price of a ton of phosphate rock, f.o.b. mine, is about $7. The cost of warehousing, freight, and handling frequently totals an additional $11 . . . . If one of our competitors . . . discovers a way in which he can cut his distribution costs by $3, we're dead! Even if we wanted to offset our competitor's more efficient means of shipping with reduced f.o.b. price for our product-we don't have that much profit margin . . . ." In a special report on the revolution now occurring in transportation of goods, Business Week stated in its September 24 issue: "Moving and storing goods on their way from mine and mill through various sub-assemblies to their final markets costs anywhere from $50 billion to $75 billion a year- $100 billion if paperwork costs are included.

Jan 1, 1967

The variation of austenitic grain size with temperature for the steels XKSlSO and XK9261 was determined using the vacuum ctching technique.It is shown that the effect of temperature on the mean grain intercept is relatively small, up to approximately 950°C. Above this temperature the rate of increase of grain size rises sharply.Within the limits of the 1-4 hr vacuum etching times used the effect of time at temperature is relatively small on the ASTM grain size of the steels.

Jan 1, 1967

By Harry Perry

U. S. consumption of sulfur and sulfur products is expected to increase at a rate of 8 percent per year between now and 1980, largely as a result of their use in fertilizer markets. World consumption is also increasing rapidly, but at a-lower rate, about 6-percent per year. In 1965, sulfur recovered in the United States from purification of natural gas; nearly doubled from the 1956-1960 average; production from pyrites declined; and production of elemental sulfur increased 15 percent. Concern about air pollution resulting from sulfur oxides produced from the combustion of fossil fuel has lead to intensive research on methods of removal before combustion, during combustion (in-process methods), and from the resulting flue gases. If all the sulfur in fossill fuels were recovered, more sulfur products would be produced than were consumed in the United States in 1965. Removal of sulfur from coal before combustion could result in a product sufficiently-high in sulfur to be a suitable raw material for sulfuric acid manufacture. In-process methods produce solid sulfates, some of which may have commercial value. Flue gas removal' methods for sulfur oxidest generally result in the production of a byproduct either of sulfuric acid or sulfur. The projected sale of these materials significantly lowers the anticipated cost of sulfur dioxides pollution abatement. Alternate methods for sulfur dioxide reduction are discussed. The various proposed processes are described and costs are given for the various methods for which estimates have been made.

Jan 1, 1967

By W. A. Nagel, R. P. Alger, H. Sherman, J. Tittmann

A sidewall epithermal neutron tool has been developed to substantially reduce environmental effects that have previously complicated neutron log interpretation. Designed for operation in uncased wells, the device provides increased accuracy in both liquid-filled and empty holes. A brief discussion of neutron moderation, diffusion and capture shows that logs using epithermal neutron detection depend on a smaller number of formation-characterizing parameters than those using thermal neutron or capture gamma ray detection. Thus, they come closer to providing an unambiguorls determination of hydrogen content. In this new device a directionally sensitive epithertnal neutron detection system has been incorporated in a side-wall source-detector skid to minimize borehole effects. The effects of variations in borehole size and shape, mud type, temperature and salinity are greatly reduced. Small residual borehole effects are then computationally accounted for in the surface control panel to provide a borehole-corrected neutron log. The log presents a direct recording of neutron-derived porosity on a linear scale. With corrections for borehole effects already applied, this direct recording of porosity simplifies log interpretation. Furthermore, comparison with a linear porosity presentation of a formation density log permits sandstones, limestones and dolomites to be readily identified. Thus, in complex or variable lithology, porosity is determined with greater accuracy and reliability than heretofore. Laboratory data and field results demonstrate the improvements in neutron logging afforded by this new side-wall epithermal neutron logging device. INTRODUCTION The new Sidewall Neutron Porosity (SNP) logging system, designed for use in uncased wells, provides reliability and accuracy never before achieved with neutron logs. The effects of variations in borehole diameter and shape, fluid salinity, mud weight and temperature—parameters that have long complicated neutron log interpretation— are suppressed or corrected for by this sidewall epithermal neutron detection system. Furthermore, to simplify interpretation the SNP log presents a direct recording of computed porosity on a linear scale. The performance improvements achieved by this new system arise primarily from the combination of two im- portant design features. First. though not unique to this new tool, an epithermal neutron detection system is used,',' Epithermal neutron detection substantially reduces the perturbing influences of the thermal neutron absorption properties of rock matrices and water salinity. Second, the neutron detection system is mounted in a directionally sensitive sidewall skid to greatly minimize borehole effects. The purpose of this paper is to explain briefy the advantages offered by the detection of epithermal neutrons, to describe the SNP equipment and the log, to present calibration and correction data and to give examples of interpretation methods made especially convenient by this new system. ADVANTAGES OF EPITHERMAL NEUTRON DETECTION Epithermal neutron detection, of all the neutron methods in current commercial use, provides the simplest determination of formation hydrogen content. Advantages of epithermal neutron detectors, as compared with thermal neutron and gamma ray detectors, are probably best explained by a brief review of the life of a source-emitted neutron. A fast neutron from the source will eventually be cap-tured by the nucleus of an atom. However. before capture is likely to occur, the fast neutron (energy of 100,000 electron volts (ev) or more) will be slowed down until it is in thermal equilibrium with its surroundings. The neutron is then considered to be a "thermal" neutron (average energy of 0.025 ev at 25C). The overwhelming majority of the slowing down thus occurs in reaching epithermal energies (energies just above thermal—0.5 to several ev). After reaching thermal energy. the neutron will "diffuse" through the formation with, on the average, no further energy change until capture. Upon the capture of the thermal neutron, relatively high energy gamma rays arc usually emitted. Hydrogen plays a very important role in the process of slowing down fast neutrons. On the other hand, the absorption effects of water salinity and low concentrations of other strong thermal neutron absorbers—relatively unimportant in the moderation process-—are very important in thermal diffusion, capture and the production of gamma rays. Thus, by detecting only epithermal neutrons with the SNP, spurious effects due to these thermal neutron absorbers are greatly minimized as compared to the effects on tools using thermal neutron or gamma ray detectors. The epithermal neutron detection system affords another important advantage. Log response in various litho-

Jan 1, 1967

By N. R. Adsit

THE B-Ni system was chosen for this study because of the great interest being shown in boron-fiber-strengthened composite materials. Boron fibers were obtained from Texaco Experiment, Inc. They average 4.2 mils in diam with a 0.5-mil tungsten wire in the center. In order to make the diffusion couple, the fibers were included in the nickel matrix by electroforming. The samples were placed in a preheated furnace for the desired temperature and length of time. Sectioning and polishing the samples revealed concentric rings as shown in Fig. 1. The average penetration distance, X, was calculated by measuring the radius of the second phase (the white shell in Fig. 1) and subtracting the original radius. The second phase was identified as NiB by X-ray diffraction. This allows the kinetics of the formation of the phase NiB to be calculated by Eq. [I], which is taken from offman:"

Jan 1, 1967

By R. D. Pehlke, J. V. Gluck

AS a portion of a general study of liquid-metal thermodynamics, high-temperature galvanic cells were used to study the effect of added dilute solutes on the activity of zinc in dilute solution with molten bismuth in the range 450° to 650°C. 1,2 The cells were of the type The experimental procedures have been described previously.1 In the course of studies conducted in the bismuth-rich corner of the systems Bi-Zn-Au and Bi-Zn-Cu, marked discontinuities were observed in the electromotive force-temperature relations for a number of the experimental compositions. Above the discontinuity temperatures, the relations, which were linear, exhibited slopes similar to the binary alloy of the same mole fraction zinc, as shown in Figs. I and 2. Below the discontinuity temperatures, the slopes were markedly different, but the relations remained linear. In general, as the amount of the third eletnent was increased, the slope of the lower portion of the relations tended to become less positive. The slopes of electromotive force-temperature relations reflect the entropy of mixing of zinc and, therefore, the occurrence of a discontinuity marks the transition between two different equilibrium situations involving the solution of zinc. A number of other investigators3-5 have used such observations to determine liquidus boundaries in binary alloys. Since the upper portions of the ternary electromotive force-temperature relations of this study had the same slopes as the binary alloys, the discontinuities are interpreted as marking the transition between the single-phase liquid region and the underlying two- and three-phase regions. Reference to the Zn-Bi equilibrium diagram6 confirms that the binary alloys were single-phase liquids at the experimental temperatures. Fig. I shows the electromotive force-temperature relations for the alloys containing Bi-Zn-Au and Fig. 2 shows similar relations for the Bi-Zn-Cu alloys. In the lower portion of each figure, the temperature of the discontinuity is plotted vs the mole fraction of the added solute at the various levels of zinc concentra- tion. Cross-plots from these curves at constant temperature permitted the construction of the partial liquidus surface isotherms shown in Figs. 3 and 4.

Jan 1, 1967

By Bengt Helmerson

A new tankhouse was started in January 1959 at the Copper Refinery of the Boliden Co., Skelleftehamn, Sweden. In early 1961 a semiautomatic machine for looping and straightening of starting sheets was introduced to substitute previous manual operations. The machine as well as consequent, racking and handling is described. Finally, economic benefits achieved and new constructions for the future are discussed. HISTORY Tankhouse operations at the Boliden Co. 's Smelter in Skelleftehamn started in 1932 on a scale that since then has been gradually increasing. In order to rationalize the operations, a new tankhouse was erected. It went into production in January 1959 and was designed for a yearly production of 35,000 metric tons at a current density of 16 amps per sq ft. Already from the beginning, however, the tankhouse has been run with a current density of 21.5 amps per sq ft, corresponding to a maximum capacity of 50,000 tons a year. During the time of planning of the new tankhouse, due consideration was given to the possibilities of mechanizing the operations. New ideas could be and were actually tested on full or pilot plant scale in the old tankhouse. In that way we developed a system for the cathode handling including washing, weighing, and transportation. A system using forklift trucks in combination with trailers and overhead cranes has been developed for transportation and racking of anodes and also for handling of anode scrap. With respect to the electrolyte, circulation and temperature control are partly automatic. Special attention was paid to the production of starting sheets, which operation normally requires a great number of man hours, and it was made the object of a particular survey as to the best ways of straightening starting sheets, attaching loops to the sheets, and so forth. As a result, a machine was designed during 1957-58 and built in our own shops. After a period of tests, the new equipment was put in operation commercially on the 10th of April, 1961. Since this date the machine has produced about 2 million starting sheets without interruption and has been the only source of looped starting sheets for the tankhouse. GENERAL DESCRIPTION Fig. 1 shows all the major parts of the system. These parts are: slitting machine with feeding table (I), standard roller leveler, type Ungerer (2), tilting roller table (3), conveyors for sheets and suspension bars (4, 7), storage of suspension bars (51, punching and stitching machine (6), two lift-turn-tilt tables (8) for discharging the starting sheets, two rack conveyors (9) for sheet assemblies. Included are a hy-daulic pump station and panels for pneumatic and electric controls. SLITTING AND STRAIGHTENING The machine is fed by hand by a man sitting in front of the slitting-machine table, Fig. 2. This operator inserts one sheet at a time into the slitter. After being trimmed, the sheet is automatically conveyed to the following step of handling, straightening. The slitting machine cuts away about 8 mm of the upper and lower parts of the sheet (in relation to its original position in the stripper section) for two reasons. The first one is to give the machine sheets of uniform dimensions; the second one is a matter of quality. Normally the starting sheets as stripped have a thick edge at the bottom end. This part would collect anode slimes and might also cause short circuits when inserted in the cells without trimming. The straightener used is of German construction

Jan 1, 1967