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By A. Moskowitz, L. S. Redmerski

The corrosion resistance of stainless steels can be strongly affected by surface treatments. Changes in corrosion resistance can relate to surface composition, integrity and stability of the passive film, and to surface profile (roughness). Operations producing oxidation at the surface, such as annealing, heat treating, and welding, can result in a chromium-rich scale and a chromium-depleted metal surface. In order to restore full corrosion resistance, chemical or mechanical clean-up techniques must remove not only the oxide, but also a very thin layer of metal. Laboratory and field test studies show that these factors are particularly significant in less highly alloyed steels. Annealing stainless in a reducing atmosphere (bright annealing) avoids chromium depletion, but as-bright-annealed material does not display optimum corrosion resistance in certain environments. Electro passiva-tion can be applied to improve pitting resistance without significantly changing bright surface appearance. Potentiometric studies show that electropassivated material also displays significantly greater resistance to breakdown of passivity in acid solutions. The application of special surface finishes for appearance purposes can affect corrosion resistance. Roughness is a key factor. Samples of related appearance but with different surface profiles can show significant differences in corrosion resistance. Thus nonreflec-tive stainless with a relatively smooth surface produced by a special rolling process is much superior to material chemically etched to a similar low reflectivity. THE corrosion resistance of a stainless steel is affected by other factors in addition to its bulk composition and metallurgical structure. These other factors include those relating to the specific chemical and physical condition of the steel's surface. This paper will consider certain aspects of surface condition in relation to corrosion resistance. In particular, studies will be described on the effects of oxidation encountered in heat treating or welding operations, of passivation after bright annealing, and of different surface finishes. EFFECTS DUE TO OXIDATION When stainless steels are exposed to high temperature in an oxidizing environment, as in annealing or welding, the oxides formed are relatively rich in chromium. As a consequence of oxidation, the metallic layer directly beneath the scale may be low in chromium to some very thin but finite depth.1"8 Such a change in chromium content could lower the corrosion resistance at the surface, whether or not the oxide layer is removed. Studies were performed relating to the effect of oxidation and chromium depletion produced during annealing and welding on the corrosion resistance of stainless steels. The nominal compositions of steels used in this study and others are given in Table I. A) Annealing Studies on 17 pet Cr Steels. 1) Effects of Pickling Treatments. Studies were performed to investigate the corrosion resistance of air annealed type 430 stainless as a function of the amount of electrolytic pickling after annealing. The material used in this study had been air annealed and electrolytically pickled in the mill. All scale had been removed, and yet the material showed unusually poor corrosion resistance. Laboratory electrolytic pickling studies were performed to determine whether additional metal removal from the surface would improve corrosion resistance. Electrolytic pickling was performed in a sulfuric acid bath using various conditions of bath acidity, temperature, time, and current density. The samples were then rated for corrosion resistance in a ferric chloride spot test. For this spot test, a solution was prepared by dissolving 10 g of FeCl3 . 6H2O, 5 g of NaCl, and 2.5 ml of concentrated HC1 in 200 ml of water. An area on a specimen was cleaned and a drop of test solution was placed on the prepared area. After 5 min, the drop was rinsed off and the area wiped dry. The spot was then rated between 1 and 5 by visual comparison with standard spots. The numerical rating of the standard spots can be described as follows: 1—No clouding of surface; 2—very slight clouding of surface; 3—slight clouding of surface; 4—moderate clouding of surface; 5—strong clouding of surface. A rating of 1 or 2 was considered to have passed the test, a rating of 4 or 5 represented failure, and a rating of 3 was considered borderline. The severity of etching in this test has been related to the actual chromium content at the surface.4 Etching (clouding) occurs on type 430 stainless (rating of 4 to 5) when the surface chromium content is 14 pct or less. The effects of current density and retention time when electrolytically repickling this material in 6 pct sulfuric acid are shown in Fig. 1. Increasing the cur-rent density or retention time improved corrosion resistance as measured by the spot test. Similarly, increasing acid concentration of the bath or bath tem-perature was found to improve corrosion resistance. The conditions making for improved spot ratings resulted in increased metal removal, regardless of specific pickling conditions used, Fig. 2.

Jan 1, 1970

Wabush Mines is the largest single supplier of iron ore to the Canadian steel industry, with 42% of its 6 million tpy of iron ore production going to the company's two Canadian owners-The Steel Co. of Canada and Dominion Foundries and Steel Ltd. Six other companies hold interests in Wabush Iron Co. Ltd. These are Lykes-Youngstown, Inland Steel Co., Intrerlake Steel Corp., Wheeling-Pittsburgh Steel Co., Finsider of Italy and Pickands Mather & Co. Field work on Wabush began in mid-1957 when a long-range program of economic, geologic, and metallurgical investigations started. This work was followed in 1959 by the construction of a temporary camp and a 700-tpd pilot plant. At the same time, work was also started on a 38-mi railway connection to Ross Bay, Newfoundland.

Jan 1, 1970

Jan 1, 1970

By Michael A. Arkoosh, E. A. Peretti

ANALYTICAL results have previously been presented for the diffusion-controlled solution of a second phase in a finite medium for planar, cylindrical, and spherical geometries.' These results were obtained by numerical methods using digital computer techniques and are applicable not only to the stage of the problem where the unstable phase shrinks to zero size, but also the subsequent stage where the concentration gradients in the matrix phase become negligible (essentially complete homogenization). It is anticipated that the results of such an analysis may be of use to those workers who are interested in the processes

Jan 1, 1970

By John D. Rockaway

This report and accompanying engineering geologic map describe the generalized engineering geology of St. Louis County, Missouri for use in determining the most efficient, economical, and environmentally sound program for land development and urban growth. It includes an evaluation of such factors as the physical and engineering properties of soil and bedrock, surface stability, and subsurface geologic structure. The map and text are designed primarily for property owners, engineers, architects, real estate developers, and city planners involved in land-use planning. The geologic information and engineering interpretation must be considered as a general guide and not as a substitute for a complete on site investigation prior to initiation of any land-use project. The map scale, 1:63,360 (1 inch to a mile) is too small to include the detailed information normally provided on the 7 1/2-minute quadrangle series (1:24,000). The smaller scale is most useful at regional planning levels and was chosen to present information on the more significant engineering factors of the geologic environment for county-wide planning and development. A conventional geologic map deals primarily with the distribution and variation of bedrock formations, and a pedologic map presents information on the soil or natural medium for plant growth. Basic geologic maps and pedological maps are valuable tools that can be of assistance in studying the geologic environment, however, these maps do not provide all the information required for land-use planning. The engineering geologic maps are designed to provide this data. The engineering geologic map is related to both of these basic maps but emphasizes the engineering properties of the rock formations and soils rather than their age or origin. Some of the unit boundaries shown on the county map will closely follow some geologic formation and/or pedologic boundaries; others will transgress these conventional boundaries. Earth materials, bedrock and soil, that have similar engineering characteristics have been mapped as one unit without regard to their geologic or pedologic classifications. This is to assure that geological factors are recognized, adequately interpreted, and presented for use in engineering practice.

Jan 1, 1970

By G. A. Colligan, G. L. F. Powell

A new experimental technique has been developed to study nucleation behavior in eutectic alloys. It is somewhat similar to that applied by Sundquist and Mondolfo1 but with the advantages that: 1) bulk samples are undercooled instead of small droplets thus allowing the thermal behavior to be monitored by a thermocouple immersed in the sample, and 2) nucleation behavior is investigated in the same sample on either side of the eutectic composition by adding additional component to the sample under controlled conditions which preclude the addition of nu-cleation contaminants. Sundquist and Mondolfo carried out ]nucleation ex-periments on a large number of eutectic alloy sys-tems and concluded that nonreciprocal nucleation operated. If one phase a was a good nucleant for the other phase 0, then B was a poor nucleant for a. This was determined experinlentally by comparing the nucleation temperatures of 100 to 300 u diameter droplets of hypereutectic and hypoeutectic composition cooled from above the liquidus and from a temperature between the liquidus and the eutectic temperature. Primary phase a was concluded to be an efficient nucleant for the other phase B, if the following experimental result was obtained. Referring to Fig. 1, the temperature TI at which a drop of hypereutectic alloy of composition B froze when cooled from above the B liquidus was noted. This was the nucleation temperature for B in the absence of a. A drop of hypoeutectic alloy of composition A was then frozen from temperature T2 between the a liquidus and the eutectic temperature. The temperature T3 at which the eutectic nucleated in the presence of the primary or proeutec-tic a was noted. If this temperature T3 was higher than the temperature TI at which the B nucleated in a hypereutectic alloy, it was concluded that the primary a had nucleated the 6. This temperature T3, representing a certain undercooling below the equilibrium eutectic temperature Te , was designated ?TB by a> the undercooling below T, for nucleation of 13 by a. If there was no substantial difference in nucleation temperature between the hypereutectic drop cooled from above the /3 liquidus and the hypo-eutectic drop cooled from a temperature between the a liquidus and the eutectic temperature, it was considered that the a nucleated B at an undercooling equal to or greater than that at which P nucleated from a hypereutectic alloy. Sundquist and Mondolfo1 found that faceted primary crystals were good nucle-ants for metals that grow as orthogonal dendrites when present as the primary phase. Jackson2 has questioned Sundquist and Mondolfo's technique and proposed that in Sundquist and Mon-dolfo's samples, such as composition A, primary a retained B in reentrant grooves at their surfaces when heated to a temperature above the eutectic but below the a liquidus. This objection was suggested by experiments with organic eutectics where reten-

Jan 1, 1970

By R. G. Turner, M. G. Hubbard, A. E. Dukler

Gas phase hydrocarbons produced from underground reservoirs will, in many instances, have liquid phase material associated with them, the presence of which can affect the flowing characteristics of the well. Liquids can come from condensation of hydrocarbon gas (condensate) or from interstitial water in the reservoir matrix. In either case, the higher density liquid phase, being essentially discontinuous, must be transported to the surface by the gas. In the event the gas phase does not provide sufficient transport energy to lift the liquids out of the well, the liquids will accumulate in the wellbore. The accumulation of the liquid will impose an additional back pressure on the formation that can significantly affect the production capacity of the well. In low pressure wells the liquid may completely kill the well; and in the higher pressure wells there can occur a variable degree of slugging or churning of the liquids, which can affect calculations used in routine well tests. Specifically, the calculated bottom-hole pressures used in multirate backpressure tests will be erroneous if the well is not removing liquids on a continuous basis, and gas:liquid ratios observed during such a test may not be correct. Several authors1,3,8,14 have suggested methods to determine if the flow rate of a well is sufficient to remove liquid phase material. Vitter14 and Duggan' proposed that wellhead velocities observed in the field would be adequate for keeping wells unloaded. Jones8 and Dukler3 presented analytical treatments resulting in equations for calculating, from physical properties, the minimum necessary flow rate. An analysis of these studies indicates the existence of two proposed physical models for the removal of gas well liquids: (1) liquid film movement along the walls of the pipe and (2) liquid droplets entrained in the high velocity gas core. Although there probably is a continuous exchange of liquid between the gas core and the film, they will be treated separately for the purposes of this study. The development and comparison of these separate models with experimental data will permit the determination of which, if either, is the controlling mechanism for the removal of liquids from gas wells. The Continuous Film Model Liquid phase accumulation on the walls of a conduit during two-phase gas/liquid flow is inevitable due to the impingement of entrained liquid drops and the condensation of vapors. The movement of the liquid on the wall is therefore of interest in the analysis of liquid removal from gas wells. If the annular liquid film must be moved upward along the walls in order to keep a gas well from loading up, then the minimum gas flow rate necessary to accomplish this is of primary interest. The analysis technique used follows Dukler2 and Hewitt5 and involves describing the profile of the velocity of a liquid film moving upward on the inside of a tube. The minimum rate of gas flow required to move the film upward is then calculated.

Jan 1, 1970

By H. C. H. Darley

The principal causes of unstable boreholes* have been known for many years. For example, in a paper published in 1938, Halbouty and Kaldenbachl listed nearly all the classes of troublesome shales that we know today. Much progress has been made since then, but we still have difficulty in identifying the cause of hole problems and consequently in selecting the right technique for combatting them. This subject was discussed at length by Kelly2 in a recent paper and much valuable information was provided. In the Shell Laboratory it was felt that there was a need for a better understanding of the basic mechanisms underlying the various forms of hole instability, and accordingly, a study was undertaken. This entailed reviewing the physics and chemistry of shales, developing tests for characterizing shales, and constructing a model to study borehole stability. Full simulation of underground conditions was not attempted; for example, we used reconstituted shale specimens, and often simple solutions or suspensions rather than practical drilling muds. Such procedures are necessary in order to establish mechanisms, but caution must be exercised in applying the results to the more complex conditions in the field. Part I — Compaction Swelling and Dispersion of Shales Compaction of Sediments Shales are formed by the compaction of sediments. Water is expressed as sediments are buried by subsequent layers, and the degree of compaction is proportional to the depth of burial, provided the water is able to escape easily to permeable formations. The younger sediments, when recovered at the surface, soften and disperse when mixed with water; the older shales have undergone diagenesis (alteration of the clay minerals, secondary cementation, etc.), and remain hard and unaffected by water. In this paper we shall apply the term "shale", as the drilling engineer does, to everything from clays, which are highly reactive to water, to completely lithified materials such as claystones and slates, which are completely inert. However, because these materials behave quite differently when encountered in the drilling well, it is desirable to develop a simple means of characterizing them. The feature that distinguishes the various shales is their dispersibility in water —soft clays disperse readily, harder shales disperse slowly when agitated, the lithified materials will not disperse at all unless milled. In the dispersibility test used in our study, a weighed amount of dry shale particles in the 12-to-100-mesh-size range was placed in a tube filled with distilled water and allowed to soak for 16 hours. The

Jan 1, 1970

By F. R. Lee

This publication lists permissible equipment approved by the Bureau of Mines during 1967 and 1968 (calendar years), except breathing apparatus and explosives. The purpose of this publication is to inform the public about approved equipment for use in underground mines.

Jan 1, 1970

By Clarence O. Babcock

Model pillars of limestone, marble, sandstone, and granite, with length-to-diameter (LID) ratios of 3, 2, 1, 0.5, and 0.25 (0.286 for granite), were broken in axial compression to determine to what extent an increase in end constraint increased compressive strength. Radial end constraints of 13 to 23% of the average axial stress in the pillar, produced by solid steel rings bonded with epoxy to the ends of dogbone-shaped specimens, increased compressive strength somewhat above that of cylindrical pillars without ring constraint. However, when the results were compared with those obtained by other investigators for straight specimens of several rock types taken collectively, with LID ratios greater than 0.5, the resulting strengths were not significantly different. Thus, the amount of end constraint produced by the solid steel rings was about the same as that produced by the friction from the steel end plates. In other tests, a radial prestress of 3000 or 5000 psi was applied prior to axial loading by adjustable hardened steel rings to increase the constraint above that obtained for the solid rings. The average radial constraint stress, expressed as a percentage of the average axial pillar stress at failure for the 3000 psi prestress, was 54.3% for limestone, 40.3% for marble, 44.7% for sandstone, and 23.4% for granite. The average radial constraint stress, expressed as a percentage of the average axial pillar stress at failure for the 5000 psi prestress, was 74.2% for limestone, 51.2% for marble, 61.6% for sandstone, and 29.7% for granite. These constraints increased the compressive strength significantly above the strength of straight specimens and solid-ring constrained specimens. These results suggest that large horizontal stresses in orebodies mined by the room-and-pillar method should increase the strength of the pillars and allow an increase in ore recovery by a reduction of pillar size when major structural defects are absent. One important objective of the U.S. Bureau of Mines (USBM) mining research program is the rational design of mining systems. In the design of room-and-pillar mining operations, pillar strength is a fundamental variable. It is customary to estimate this strength from uniaxial compression tests of rock samples and to correct this value for the length-to-diameter (LID) ratio of the in-situ pillar. This method of estimating pillar strength corrects for pillar shape but does not consider the effect of a large horizontal in-situ stress field that sometimes exists in underground formations. The purpose of the work covered in this report was to determine to what extent the compressive strengths of model pillars of relatively brittle rock loaded in axial compression were affected by lateral end constraint. In previous work, Obert l used solid steel rings bonded to the ends of dogbone-shaped specimens to study the creep behavior of three quasi-plastic rocks -salt, trona, and potash ore - during a test period of 1000 hr. These rings provided radial constraint during the loading cycle of 20 to 50% of the axial stress for specimens with LID ratios of 2, 0.5, and 0.25. He concluded that (1) "for a quasi-plastic material the end constraint strongly affects the specimen strength, and (2) as D/L increases (length-to-diameter decreases), the specimens lose their brittle characteristics and tend to flow rather than fracture." He also concluded that model pillars constrained by rings were better for use in predicting the strength of mine pillars than either cylindrical or prismatic specimens. This conclusion appears to be valid where mine pillars, roof, and floor are a single structural element. In the present study, 460 specimens of four relatively brittle rocks — limestone, marble, sandstone, and granite - were tested to failure. The study consisted of two parts: (1) the effect on the compressive strength of end constraint produced during the axial loading cycle by solid steel rings bonded with epoxy to the ends of the specimens, and (2) the effect on the compressive strength of increased end constraint produced in part by a prestress applied prior to axial loading and in part by lateral expansion of the specimen during the loading cycle. The first part of this study was reported in some detail earlier.2 EXPERIMENTAL PROCEDURE AND EQUIPMENT Model rock pillars of the sizes and shapes shown in Fig. 1 were broken in axial compression when the ends were constrained as shown in Fig. 2. he straight specimens were broken without ring constraint. The specimens of dogbone shape were broken with (1) solid

Jan 1, 1970

"Geological investigation in the Appalachian region of Canada began more than 150 years ago. The distribution of rock formations, and their ages and regional structure are today reasonably well known in most parts of the region to 1-or 2-mile scale. Most Newfoundland geology is known only to 4-mile scale. About 200 earth scientists carry out research in the region, of whom about 25 per cent are government employees, 50 per cent university staff and graduate students, and 25 per cent industry employees.Increased activity is needed toward both regional analyses and problem studies through the efforts of multi-disciplinary teams. The ultimate objectives of earth science must be the discovery and development of mineral re•-sources and the use and conservation of natural material in the environment, all for the benefit of the local in-habitants. To accomplish this, the scientific community must carry out an array of research projects ranging from the technical products of geological, geophysical and geochemical surveys through to the research products de-signed to renew theories and hypotheses bearing on natural processes. Some scientific sub-objectives are listed.Recommended is the increase and broadening of communication among Appalachian scientists, specifically those resident in the Atlantic Provinces. It is proposed that an Appalachian Division of the Geological Association of Canada be formed to provide a forum for discussion of Appalachian topics. In addition, a committee or council of university, industry and government earth scientists should be formed to examine the state of the science in the region, to identify programs of investigation and individual projects of research, and to recommend methods of approach. If the committee succeeds and the scientific community acts upon the recommendations, the quantity, quality and pertinence of research will increase, and earth science will better serve Appalachian society."

Jan 1, 1970

By Niels Hansen

The substructure formed by drawing at room temperature in aluminum (99.5 and 99.998 pct purity) and in recrystallized aluminum aluminum-oxide products containing from 0.2 to 4.7 wt pct of aluminum -oxide was examined by transmission electron microscopy, and the flow stress of the drawn materials was measured by tensile testing at room temperature. A sub-grain structure was present after a reduction in area by drawing of 10 to 20 pct, and the subgrain size was observed to decrease with increasing deformation. The tensile data show that the increase in flow stress (0.2 pct offset) by drawing from 10 to 95 pct depends on the reduction in area, not on the composition of the materials. Dispersion strengthening and subgrain bowzdary strengtlzening contribute to the flow stress, and these strengthening processes have been found to be linearly additive. The flow stress (0) can be related to the subgrain size &) by the Petclz relation = uo + k . t, where go is dependent on the composition of the products and k is approximately the same far all materials. THE microstructure of dispersion-strengthened aluminum aluminum-oxide products consists of small oxide plates distributed in an aluminum matrix. The matrix structure depends on the manufacturing history, and in hot-worked as well as cold-worked products the matrix is divided by subgrain (or dislocation) boundaries. For hot-extruded products it has been shown1 that dispersion strengthening and subgrain boundary strengthening are linearly additive, and the flow stress (0.2 pct offset.) at room temperature has been related to the subgrain size (ts) by a Petch equation,2,3 s = so + k . ts-1/2, where s0, increases with increasing oxide content. For cold-worked products containing subgrains no systematic work has been reported, and it was the aim of the present study to examine the microstructure and the relationship between the flow stress and the subgrain size for such products. The behavior of' aluminum aluminum-oxide products depends on the purity of the aluminum matrix, and aluminum of the matrix purity (99.5 pct) was included in the investigation. The literature contains few data about the behavior of this impure aluminum, and aluminum of a higher purity (99.998 pct) was therefore also examined. As regards the relationship between the flow stress and the subgrain size in cold-worked dispersion-strengthened products, no systematic work has been reported. For aged cold-worked structures containing fine precipitates (Fe-Mo carbide) a Petch relation has been found,4 and it has been shown that the k value NlELS HANSEN is Head, Metallurgy Department, Danish Atomic Energy Commission, Research Establishment Riso, Denmark. Manuscriot submitted January 9, 1969. IMD is approximately the same as in iron, whereas the s0 value is higher owing to the presence of the precipi-tates. Investigations of metals such as tungsten,' ferrous metals,4,6 and molybdenum7 cold drawn or swaged at room temperature have shown that the flow stress can be related to the subgrain size by a Petch relation when ts is taken as the subgrain size perpendicular to the direction of deformation. For aluminum no work has been reported on the relationship between the flow stress and the subgrain size after deformation at room temperature, whereas for aluminum tensile strained at different temperatures in the range -183" to 375°C a Petch relation has been found by taking ts equal to the subgrain size.' In the present study two aluminum materials (99.998 and 99.5 pct) and three aluminum aluminum-oxide products (containing 0.2, 1.0, and 4.7 wt pct oxide) were drawn at room temperature to reductions in area from about 10 to about 95 pct. The structures were studied by transmission electron microscopy, and the flow stress (0.2 pct offset) was measured at room temperature. EXPERIMENTAL Materials. The materials are given in Table I together with the chemical analysis. The three aluminum aluminum-oxide products were manufactured from aluminum powder that had been compacted and Table I. Chemical Analysis of Materials Al203 Fe SI Material wt pct wt pct wt pct 99.998 pct* - 0.0004 0.0012 Aluminum 99.5 pctt - 0.36 0.16 Aluminum AlMD13† 0.2 0.16 0.12 Aluminum- -Oxide AlMD105† 1.0 0.26 0.18 Products SAPISML960s† 4.7 0.22 0.19 *Other impurities: O.0004 pct max each of Cu and Zn (supplier's analysis). †Other impurities: 0.03 pct max Cu. 0.02 pct max each of Mn, Mg, Zn, Ti. Table 11. Mean Diameter of Aluminum-Oxide Particles in Extruded and in Cold--Drawn Aluminum Aluminum-Oxide Products Mean Diam. of A1203-Plates* Material State A AlMD105 Extruded 540 Cold Drawn 97 pct 510 SAP ISML 960 Extruded 770 Cold Drawn 95 pct 820 *The standard deviation of the mean is approx. 5 ±pct.

Jan 1, 1970

By P. T. Gallagher, W. A. Oates, J. A. Lambert

FAIRLY extensive equilibrium data exists for carbon dissolved in r iron.1-8 However the temperature coefficients of the carbon activity, ac , are insufficierltly preciseto reveal whether the heat of solution of carbon, ?HC , varies with composition. It is doubtful

Jan 1, 1970

At Appin colliery, geological structural analyses and investigations of roof conditions suggest roof failure may be attributed to vectorial stresses acting on underground openings, and inducing movement along inherent discontinuities in the surrounding rocks. Certain complex joint and fracture patterns tend to exhibit the effect of this movement resulting often in local deterioration in natural support.The following conclusions are drawn.1. Roof failure is related to the inherent nature of the roof rocks, the presence of mechanical discontinuities, and the vectorial stresses imposed upon it.2. Roof failure is not necessarily related to the statistically most prominent jointing.3. Colliery development approximately parallel to the direction of the statistically most prominent jointing sometimes results in favourable roof conditions.4. The maximum principal stress is the resultant of those vectorial stresses acting upon a mine opening and may be inferred from roof adjustments to those stresses after mining.5. Statistical analyses of jointing in the mine workings can provide clues to the tectonic force or forces which have been regionally or locally influential.6. There is a probable relationship between mining induced fracturing, jointing, and micro-fractures in quartz grains, within the sediments of the mine roof.

Jan 1, 1970

By Henry M. Harris

The roll forming of oxide powders was studied in a Bureau of Mines investigation to find the conditions and parameters required to make satisfactory ceramic strip. High-quality porous or dense alumina, zirconia, and porcelain shapes were made by sintering strip roll-formed at room temperature from powders containing minor amounts of binder and water. Strips with thicknesses of 0.04 to 0.08 inch and bulk densities from 40 to 90 percent of theoretical densities were made. The parameters most important to formability were particle size, condition of the powders, and roll gap. Other factors affecting quality were speed and surface condition of the rolls, amount and type of binder, water content, and sintering conditions. Ceramic strip was formed at rates up to 78 feet/minute, which is 13 to 23 times faster than reported by previous investigators, and forming was done in a simple and inexpensive roll unit. Reshaping the strip was possible by cutting, grinding, shearing, and stamping. The following innovations were developed that allow roll processing not normally possible with ceramic powders: (1) Fine-sized powders were made into strip by preparing these as partially sintered granules; (2) thick strip was formed by pressure feeding powders into the rolls; (3) flexible strip was made using a rubber-base bonding agent; (4) corrugated strip was formed on shaped rolls; and (5) porcelain strip was densified and reduced in thickness by rerolling while hot.

Jan 1, 1970

Pressure drops were measured in a column packed with glass spheres and wax particles, both in random and preferential distributions. Variables investigated included wax content, gas flow rates, and temperatures.It is shown that for random distribution of wax, pressure drop is exponentially related to wax content above the melting point of wax and that below this it increases with increasing gas rate and temperature.For preferred distribution of wax the highest increase in pressure drop is obtained with horizontal distribution of wax and the least with vertical distribution.Comparison with operating blast furnace data and application of results to practice are also included.

Jan 1, 1970

By R. E. Miner, J. K. Jackson, T. L. Wilson

A study has been made of the transformation kintetics and morphology in gas-quenched Fe-5 pct Ni alloys. Massive ferrite or nlurtensite was found to form at temperatures in agreement with earlier results. Surface Preparation appeared to have the greatest effect in determining the type of transformation Product formed. Grain size change, subgrain morphology, and dislocation densities of massive ferrite were essen-tinlly invariant functions of cooling rate. The mar-tens~tic structures were typical of transformation in austenite grains of the order of the sample thickness. BY introducing the idea of a massive transformation in dilute iron-base alloys, Gilbert and Owen in 1962 served to stimulate a closer inspection of phase transformations in ferrous systems.' A wealth of literature has followed concerned with the morphology,2-5 transformation mode,2'3'6-8 and thermodynamics of transformations.2,5,9 interesting controversies have resulted from the experimental observations; closer attention has been paid to the definition of massive transformations and still to be resolved is the Ms temperature of pure iron. The purpose of this note is to report some observations made in a detailed kinetic and metallographic examination of the transformations that occur in gas quenched Fe-5 pct Ni. The results are pertinent to the Ms extrapolations that have been made for pure iron and the observed substructure of massively transformed alloys. PROCEDURE The material used in this investigation was cast as a 5 lb vacuum induction melted, carbon deoxidized heat. The ingot was hot worked to a strip 0.10 in. thick, decarburized, and cold rolled to final thickness. Specimens were punched to sample shape and decarburized in wet hydrogen at 600°C. The chemistry of test specimens is indicated in Table I. Samples 1 by $ in., by thickness were resistance heated and rapidly cooled in an apparatus as illustrated in Fig. 1. Similar helium quenching apparatuses have been described previously;2,6'10 the distinguishing feature of this apparatus is the nozzle geometry. Twin nozzles with three convergent-divergent, sonic ports were mounted perpendicular to the specimen for quenching purposes. The specimen temperature was monitored with an intrinsic 3 mil chromel-alumel thermocouple spot welded to the specimen and con- nected to an oscilloscope. A single switch stopped the current flow through the specimen, opened a gas flow solenoid valve, and initiated an oscilloscope sweep. Cooling rates were read directly from a photograph of the oscilloscope trace and the quenching rates quoted later were made at a point immediately prior to transformation on the trace. All quenching studies were conducted either under a vacuum of 10"-5 torr or a helium atmosphere. The sample geometry was chosen large enough to permit optical and electron microscopy to be performed on samples. The samples were electropolished for both types of examination in a perchloric-acetic solution. Electron microscopy was conducted on a HU 11A microscope operated at 100 kv. Dislocation densities were determined at the same general operating reflection (110) on foils thick enough to produce Kikuchi patterns. RESULTS AND DISCUSSION Transformation Temperature Observations and OD-tical Microscopy. The quenching results of this study are illustrated in Fig. -2(a). Samples which were treated in the as-decarburized condition transformed in a manner similar to that reported previously—a decrease in transformation temperature occurred as the quenching rate increased until a plateau region was reached. Within the scatter of the results obtained here, there was no break in the transformation temperature-quenching rate plot. This suggests no change in transformation mode. Further metallographic examination confirmed this observation. A martensitic transformation was obtained for similarly treated samples except that the surface was first electropolished. The Ms temperature was approximately 85°C below the plateau determined for the unpolished samples and cooling rates as slow as 2000°C per sec were adequate for producing marten-site. The transformation temperatures are in gen- / STRIP SAMPLE / COPPER I SAX/-/}' / CONNECTOR-----A f, SON|C poRTS AC LEADS 3j ]j"I rofe[ \ Mf/yinK/iKj''^ THERMOCOUPLE X-(^—iie"s*c? ' LEADS 1 INCH Fig. 1-—Schematic scction of gas quenching apparatus

Jan 1, 1970

By Irving Fatt, R. M. Weinbrandt

Efforts have been made for many years to observe pore structure of sedimentary rocks on a microscopic scale. A better description of the pore structure in reservoir rock would aid in the development of relations between flow through tube network models and flow in consolidated reservoir rock. The unique qualities of the scanning electron miscroscope (SEM) make it the ideal tool to use in a study of pore structure. Previous methods of studying pore structure included plastic casts of pore space and optical microscopy.l-7 There is now available a new method to observe three-dimensional flow channels in reservoir rock: a scanning electron microscope having variable magnification from X20 to X20,000 and approximately 1000 times the depth of focus of the conventional light microscopes. This microscope also can obtain stereoscopic images and can measure and diagram flow channels so that it is possible to construct a network of tubes that will model consolidated reservoir rock. THEORY OF THE SCANNING ELECTRON MICROSCOPE The scanning electron microscope (SEM) functions by projecting a beam of electrons through magnetic focusing lenses at a specimen and recording secondary electrons excited by the primary beam. The amount of secondary electron emission portrays the topography of the specimen because more secondary electrons are emitted from high points than from low points. A schematic of the SEM is shown in Fig. 1. The property of the SEM that is of most importance in this study is its great depth of focus. The depth of focus results from using electrons

Jan 1, 1970

By W. A. Oates, J. A. Lambert, P. T. GaIIagher

Monte Carlo methods have been used to compute the arrangements of interstitial atoms dissolved in tetrahedral sites in bcc lattices. It is assumed that the presence of an interstitial atom "blocks " a certain number of neighboring sites and prevents their occupancy. Sites "blocked" by more than one filled site are allowed for. The computed values of. the mean occupation number (defined as the ratio of the total number of sites blocked to the number of solute atoms are used to calculate the configurational entropies of the solutions. These entropies are compared with those resulting from previous theoretical studies of this problem and also with available experin~ental data for the p Zr-H, Nb-H, V-H, and Ta-H systems. Evidence is also given that the "blocking" explanation of low limiting compositions in these systems, rather than this being due to initial limitations on the number of sites available, is probably correct. THE ideal partial configurational entropy of mixing of an interstitial solute in a metal is given by: where p is the number of interstitial sites per metal atom and Xi is the atomic fraction of the interstitial. For the bcc lattice. which we shall be concerned with in this paper, the interstitial positions are shown in Fig. 1. It can be seen that for the tetrahedral sites, p=6. whereas for the octahedral sites, p = 3. Different emphasis has been placed on the relative importance of energy and entropy effects in determining deviations from ideality in interstitial solid solutions. In some cases the same system, e.g., Fe-C, has been described by the contradictory regular and athermal solution models indicating that the enthalpy and entropy functions, derived from equilibrium data, are frequently not accu.rate enough to differentiate between these treatments. However, for certain metal-hydrogen solutions the equilibrium data is available over sufficiently wide ranges of temperature and composition to permit a reasonably accurate determination of the compositional variation of the heats and entropies. Hoch&apos; has attempted to interpret the results of interstitial solid solutions in terms of a regular solution model. In the case of the Ta-H system where 13 = 6, this model entails fitting the experimental relative partial entropies of solution, asH, to the equation: where ASgs is the relative partial excess entropy of solution of hydrogen. Hoch found that the results of Mallett and Koeh1 could be fitted to this equation with an approximately constant value of AF up to XH = 0.25. However, it is apparent from the solubility isotherms in this system which become asymptotic to the composition TaH that, since (Xh /6 - ~Xh ) becomes infinite only at TaH6, it is necessary that AS<&apos; tends to infinity at TaH. In other words, the low saturation composition of TaH, instead of the anticipated TaH,, eliminates the possibility of applying regular solution theory to such systems. Rather large negative excess configurational entropies must exist at higher hydrogen concentrations in order to explain the lower saturation values. To account for these low limiting compositions and excess entropies two distinctly different approaches have been followed. Rees and many others1-l2 have assumed that not all interstitial sites are crystallographically equivalent with respect to the interstitial addition; that is, in Eq. [I] p is less than the value anticipated from geometrical considerations. To describe, say, a bcc metal-hydrogen system with a limiting composition of MH by this approach one would consider that p = 1 in the first instance instead of p = 6.&apos;j3 In some cases, nonintegral values of B have been taken in order to improve the fit with the experimental data over limited ranges of composition. The other approach which has been used to explain the low saturation compositions is to assume that, although all sites are available for occupancy, strong repulsive interactions exist between the neighboring interstitial atoms, and hence occupancy of any site excludes or blocks a certain number of neighboring sites from being occupied. Earliest treatments of this concept considered the exclusion of an integral number, of nearest-neighbor sites from being occupied at all concentrations. In this case, the partial configurational entropy is given by: These early treatments failed to allow for the overlap of the blocked sites which will arise at all but the very lowest concentrations. More recently attempts have been made to calculate the effect of this decrease in the number of blocked sites on the configurational entropy. Using the quasichemical treatment of interstitial solid solutions as given by Lacher and assuming that an infinite repulsive interaction energy existed between the solute atoms. atom obtained an approximate configurational entropy applicable to the blocking with overlap case:

Jan 1, 1970

By F. S. Karn

Measurements were made of the flow of helium, methane, ethane, butane, and toluene through thin disks of coal. All measurements were made on a dense layer in the Pittsburgh seam identified as attritus. Flow increased with pressure differential and temperature. At room temperature and a pressure differential of 1 atmosphere flow rates along the bedding plane of Pittsburgh seam coal were helium 881 X 10-10 cm2 sec-1, methane 1.2 X 10 -10 cm2 sec-1, ethane 0.54 X 10-10 cm 2 sec-1, n-butane 0.35 X 10-10 cm2sec-1, and toluene 3.8 X 10-10 cm2sec-1. Flow rates were 50 percent lower across the bedding plane of the coal than along the bedding plane. Activation energies were 3.9 kcal mole-1 for helium and 13.6 kcal mole-1 for methane, with diffusion measured either along or across the bedding plane.

Jan 1, 1970