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By A. Hansson, G. E. Tardiff

WHILE it is generally known that cold-worked low-and medium-carbon steels exhibit substantial increases in tensile rupture ductility with increased deformation velocity172 (up to the von Karman limit), the observations for annealed or normalized steel do not permit simple generalization. Various investigators, for example, have reported both small increases1,3 and small decreases4,5' in rupture ductility with increased rates of deformation of normalized low-carbon steel. The purpose of the present note is to report on the dependence observed for strain-aged steel since preliminary work here indicates that strain aging results in the development of a consistent type of behavior that is understandable in the light of current knowledge of the lower yield dynamics for steels which deform inhomogeneously.6 This realization throws additional light on the influences responsible for the behavior of normalized steel. The results presented here were obtained for a 0.21 pct C, 0.012 pct N sheet (0.012 in. thick) steel which was received in a temper-rolled condition (approximately 3 pct reduction in thickness after process annealing); the as-received material had a spherodized structure with a ferritic grain size of ASTM 8. The material was selected for testing after 6 months room temperature aging, at which time the static lower yield and ultimate tensile strength measured 79 and 82 kpsi, respectively. ASTM 2-in. reduced section, 1/2-in.-wide specimens were used in smooth bar tests and 3/4-in.-wide specimens containing two 60-deg opposed edge notches (root radii = 0.002 in.) were used in notched bar tests. To facilitate strain measurement, the smooth bars were blued with ink and marked at 0.1-in. intervals along the gage length; the notched

Jan 1, 1968

Canada's newest low-grade porphyry copper mine, Gibralter Mines Ltd. (N.P.L.), has reached production. The subsidiary of Placer Development Ltd., located at Williams Lake in the Caraboo District of central British Columbia, began open pit mining in mid-June on reserves estimated at 358 million tons assaying 0.373r: Cu and 0.016C; MoS,. Each of four separate zones will be mined in a predetermined sequence, in one or more stages, and with a throughput of more than 36,000 tpd. The sequence and stages of mining the zones have been determined by computer calculation and economic analysis and are designed to maximize recovery and minimize cost. At the very least, the mine is off to a promising start. Development costs leveled off at $67 million. 9'; below the anticipated budget.

Jan 7, 1972

By Daniel R. Stewart, Ralph R. Sacrison

The function of the geological engineer is to assist in mine planning and operations by collecting, interpreting, and applying geologic data to the solution of engineering problems. The geologist supports this effort by collecting additional geologic information specifically useful to the engineer. This use of geologic information reinforces the value of mine geology to the mining process beyond the traditional role of orebody definition. Work discussed includes: evaluation of caving strategies at the Climax and Henderson mines, support definition and slope stability at the Climax mine, and some uses of geology in cavability estimation for the Mount Emmons project.

Jan 1, 1984

By Karl L. Fetters

In the process of making steel in the open-hearth furnace the refining of the metal during the working period of the heat is largely accomplished through the agency of the slag. From the birth of the process until the present day steelmakers have recognized the importance of the slag in determining the composition of the metal and the quality of the product. The general relationships between slag composition and metal analysis have long been known, at least in a qualitative or approximate fashion. For examples, the iron oxide content of the slag is higher on lower carbon heats; the more basic slags are higher in iron oxide for a given carbon content; certain amounts of iron oxide and lime arc required for phosphorus removal and a high lime-silica ratio is needed if the sulphur content of the metal is to be diminished. In recent years a number of quantitative relationships involving these and other variables have been developed through plant and laboratory studies by numerous investigators in this country and abroad. The direct comparison of laboratory and open-hearth data involves the question of the degree to which each approaches the conditions of chemical equilibrium, a question which, from the open-hearth standpoint, we are scarcely yet in position to answer. And, although a considerable body of dependable equilibrium data has been obtained in the laboratory, this work has not yet been extended to cover the ranges of slag composition encountered in basic open-hearth practice. In the present study we shall not attempt to draw comparisons between data from the two sources; nor do we attempt to draw conclusions as to the approach to chemical equilibrium in the open-hearth furnace. Many of the operating variables that are likely to be erratic or unrecorded during the earlier stages of the heat become more consistent and arc more readily subject to observation and control during later stages. For example, undigested lime or ore gradually goes into solution, the rate of carbon drop levels off, and the temperature of the metal is brought under control. For these and other reasons a greater degree of self-consistency is likely to be found among data obtained during the

Jan 1, 1940

By T. H. Dunn, P. L. Menaul

This paper discusses the results of an investigation made to develop a method of combatting corrosion of subsurface oil-well equipment caused by brines containing hydrogen sulphide. Carbon monoxide, aldehydes, and certain cyanide compounds were found by laboratory tests to effectively inhibit corrosion of steel by sulphide brines. Experiments were made for one year in eight wells in West Texas fields using formaldehyde as an inhibitor. It was found that the inhibitor treatment successfully prevented the severe corrosion previously experienced in these wells, and effected important net savings in operating costs. Introduction Corrosion of oil-field equipment has long been a problem in areas producing sour crudes. These areas include the major fields of Arkansas, Western Kansas, West Texas and New Mexico. Corrosion in these fields is caused primarily by the chemical action of hydrogen sulphide in the presence of water and by electric currents entering the wells through flow lines. Hydrogen sulphide is noncorrosive to iron or steel in the absence of water but under the usual conditions prevailing in oil wells where more or less water is present, hydrogen sulphide is very corrosive. This type of corrosion occurs over the pH range below 9, which includes all natural oil-field brines. If air is present in addition to hydrogen sulphide and water, corrosion proceeds at an extremely rapid rate. It was reported several years ago that a string of oil-well tubing was literally dissolved within 50 days where an air lift was used on a well producing considerable water and hydrogen sulphide. Air is generally absent in wells producing sour crude. After hydrogen sulphide corrosion starts, it proceeds with increasing severity and its correction becomes progressively more difficult. This characteristic of sulphide corrosion has been attributed to the formation of galvanic couples between the iron and steel equipment on one hand and the products of corrosion on the other.' Severe corrosion of subsurface oil-well equipment leads to a multitude of troubles. In addition to destruction of costly equipment, producing sands often are damaged by flooding with water leaking through corroded casing; bad mechanical conditions may develop in a well due to obstructions caused by corroded equipment lost in the hole, or partly collapsed casing; pumping operations are interfered with, and severe emulsification problems may result from the homogenizing action of corroded balls and seats.% A typical case of severe corrosion caused by hydrogen sulphide was reported in Howard County, Texas, where it was necessary to pull tubing once a week to repair leaks after the tubing had been in use for only one year. On one well in this area a string of tubing was pulled 11 times in 8 months; 11 joints of tubing being replaced because of leaks. In Ector

Jan 1, 1946

By Lester L. Hirst, Arno C. Fieldner, Henry H. Storch

EXPERIMENTAL work on liquefaction of coal was taken up by the Bureau of Mines in 1936 when it became evident that a prudent policy from the national point of view should include preparation for the time when gradual exhaustion of petroleum resources would require supplementing the growing demand for motor fuel with gasoline and diesel oil from coal. At that time (1936) certain foreign nations that had no home sources of petroleum, especially Germany, England, and Japan, were conducting active research and at least two of them were producing liquid fuel from coal on a commercial scale. Germany was reported to have an annual producing capacity of 800,000 metric tons of gasoline per year, and England had just put into operation the Billingham plant of Imperial Chemical Industries for the hydrogenation of bituminous coal and tar by the Bergius-.I.G. process. The annual capacity of this plant was about 150,000 long tons of gasoline per annum (3500 bbl. per day). With these developments taking place in foreign countries, it seemed important to undertake a long-range program of fundamental research in this country to establish a sound groundwork for the evaluation of foreign work on synthetic liquid fuels and at the same time to obtain data on the oil yields and operating difficulties using various kinds of American coals and lignite to the hydrogenation process. The results of such research would be useful in determining the yields and quality of liquid products obtainable from various coals so that American industry would be in position to select the most suitable coals and make rapid progress in establishing this new industry when the commercial need should arise. It was hoped, also, that progress in a better understanding of the chemistry of coal hydrogenation would reduce the cost of the process materially. To carry out this program, a small continuous unit capable of hydrogenating 100 lb. of coal in 24 hr. was installed at the Central Experiment Station of the Bureau of Mines at Pittsburgh, Pa. Small steel autoclaves or bombs of 0.3 gal. (1.2 liters) capacity also were used for batch-hydrogenation experiments in the study of the chemical fundamentals of the process. Much valuable assistance was obtained in planning the experimental program and designing the equipment from the Fuel Research Station of Great Britain and the Fuel Laboratories of the Mines Department of Canada, where such investigations had been in progress for several years. EQUIPMENT AND GENERAL PROCEDURE OF RESEARCH The industrial liquefaction of coal by the Bergius-I.G. hydrogenation process as practiced at Billingham, England, from

Jan 1, 1944

By L. A. Delano

During 1916, the St. Joseph Lead Co. milled 2,505,670 tons of ore. This is a daily operating average of 7855 tons. The economic concentration of such a large tonnage necessarily requires a plant equipped with modern machinery and operated efficiently. The milling process used in producing this output has been a gradual development through the long period of years that the company has been in existence. HISTORICAL SUMMARY OF MILLING PRACTICE Ore was first mined at Bonne Terre, Mo., in 1864. The early milling practice was crude. It consisted of breaking the ore into small pieces by hand, pulverizing in a Blake crusher and a pair of Cornish rolls to approximately minus 6 mm., and jigging in the old-fashioned hand jigs. Only the coarse heavy galena was saved, the gangue being shoveled off and discarded. The output for the first year under this method was only 240 tons of pig lead. The first mill of the company was a combination of extensions and additions built from time to time as the mines developed. It was a museum of early milling machinery, such as jigs, percussion tables, buddies, dolly tubs, log washers, etc., following no definite flow sheet. The chats, or tailings, were hauled to waste dumps by mule and ox teams, as much as 500 tons per day being moved in this manner, until a railroad was built in 1880. This mill was burned in 1883, at which time the annual output had reached approximately 7300 tons of pig lead. A new mill of 500 tons capacity was designed and built by C. B. Parsons. This mill has been admirably described by H. S. Munroe.' The ore was crushed in Blake crushers, Cornish rolls, through 6-mm. screens, and treated by jigs of the Parsons type, percussion tables and log washers, or trunking machines, for cleaning the galena. The middlings were recrushed in rolls and treated on Harz jigs. The mill was operated without change, except later installing Gates crushers and en-

Jan 1, 1918

By J. E. Smith, P. B. Crawford, B. L. Laudrum

A method is presented by which the displacement efficiency of a steam-injection process may be determined. The method consists of a determination of the position of the steam front at a particular time and the application of the Buckley-Leverett theory to the hot and cold regions of the reservoir with the appropriate hot or cold fluid properties. A uniform, linear flow system is assumed for this study. The method is applied to a number of reservoir conditions. The primary properties which affect the results of a steam-injection process are the oil viscosities at steam and reservoir temperatures, injection rate, pay thickness and oil saturation. The efficiency of steam injection is compared with that of water injection for a 10-acre, linearly flooded reservoir. In reservoirs where the oil viscosity is about 35 times the water viscosity, the steam process yields recoveries about 20 per cent higher than the water flood. Where the oil viscosity is near 500 cp, the steam process may recover from three to four times as much oil as a water flood. INTRODUCTION In a previous paper,' a method was suggested for evaluating a steam-injection process. Emphasis was placed upon the determination of the steam-front position in the reservoir at various times. In the present paper, the displacement process is studied in more detail. The approach is essentially that employed by Jordan, Rayne and Marshall3 in their study of hot-water injection. The steam-injection process is quite complex, and an exact description of the process has not been found; however, a qualitative description can be made. When a quantity of steam is injected into a relatively cold reservoir, the leading edge of the steam front continaally flows into cool sand, and some steam condenses. As more and more steam condenses, a bank of condensed water will form which is augmented by displaced connate water. The reservoir may be divided in three regions—(1) a region containing displaced fluids at reservoir temperatures, (2) a region contain- ing water at reservoir temperature and (3) a region occupied by steam. The reasons for the lack of a region of hot water or oil of any appreciable size have been discussed.' A method has been presented by which the location of the steam front can be determined even when heat losses to the regions surrounding the reservoir are sizable compared with the amount of heat injected. It remains to show the effectiveness of steam injection in increasing the ultimate oil recovery. To illustrate the technique for determining the increase in displacement efficiency and, hence, the increase in ultimate production, two sets of hypothetical reservoir conditions will be studied in detail.

By R. E. Zimmerman

THE separation of fine sizes of coal from its impurities by means of various flotation methods has become of increasing importance in the coal industry. This, no doubt, will be even more so in the future as the quantity of high grade coal is depleted, particularly that used for metallurgical purposes. The purpose of this paper is to describe and report the results of research work done under the auspices of the Pittsburgh Coal Co. to determine the amenability of their bituminous fine sizes of coal to flotation, to investigate the value of various reagents and factors affecting their use, and compare the results between froth flotation and bulk oil flotation. Compared with the preferential flotation of complex minerals, or ores, the flotation of coal is comparatively easy. However, this statement should not lull one into the feeling that there are no special problems involved. For instance, the separation of coal from pyrite in high sulphur coals is still far from being 100 pct successful. Size consist has considerable effect on reagent consumption and recovery. Other factors will be described and finally it must be remembered that in the flotation of coal a low priced material is being treated and thus economic considerations govern more closely its application than is generally the case in treating other minerals. As a result of the research work done by the Pittsburgh Coal Co. on the flotation of coal, it was concluded that it was practical to clean the -48-mesh coal commercially by froth flotation and after several different types of flotation units and circuits were investigated by means of pilot plants, large scale units were installed at their Champion Nos. 1, 4 and 5 Preparation Plants for the cleaning of -48-mesh slurries. These large scale operations have been recently described by D. H. Davis. 1 C. P. Proctor and C. B. Carlson2 in their chapter on Froth Flotation of Coal in the AIME Seeley W. Mudd series book on Coal Preparation describe some of the practical applications of our Pittsburgh Coal Co. laboratory work in actual plant practice as well as summarizing part of the investigational work. The author presents this paper, however, as a supplement to their reports, and records the basic research accomplished in the laboratory investigational work as well as the results of experi¬ments using bulk oil flotation. In presenting this work the author wishes to state much more work must be done in applying the principles of flotation to cleaning coal, especially in view of recent studies and practices in other mineral beneficiation fields. METHODS OF CONDUCTING LABORATORY TESTS The bulk of the research work was conducted in the laboratory of the Champion No. r Preparation Plant. This plant has elaborate facilities for sampling and analyzing coal and proved to be an admirable location

Jan 1, 1948

By Karl L. Fetters

In the process of making steel in the open-hearth furnace the refining of the metal during the working period of the heat is largely accomplished through the agency of the slag. From the birth of the process until the present day steelmakers have recognized the importance of the slag in determining the composition of the metal and the quality of the product. The general relationships between slag composition and metal analysis have long been known, at least in a qualitative or approximate fashion. For examples, the iron oxide content of the slag is higher on lower carbon heats; the more basic slags are higher in iron oxide for a given carbon content; certain amounts of iron oxide and lime arc required for phosphorus removal and a high lime-silica ratio is needed if the sulphur content of the metal is to be diminished. In recent years a number of quantitative relationships involving these and other variables have been developed through plant and laboratory studies by numerous investigators in this country and abroad. The direct comparison of laboratory and open-hearth data involves the question of the degree to which each approaches the conditions of chemical equilibrium, a question which, from the open-hearth standpoint, we are scarcely yet in position to answer. And, although a considerable body of dependable equilibrium data has been obtained in the laboratory, this work has not yet been extended to cover the ranges of slag composition encountered in basic open-hearth practice. In the present study we shall not attempt to draw comparisons between data from the two sources; nor do we attempt to draw conclusions as to the approach to chemical equilibrium in the open-hearth furnace. Many of the operating variables that are likely to be erratic or unrecorded during the earlier stages of the heat become more consistent and arc more readily subject to observation and control during later stages. For example, undigested lime or ore gradually goes into solution, the rate of carbon drop levels off, and the temperature of the metal is brought under control. For these and other reasons a greater degree of self-consistency is likely to be found among data obtained during the

Jan 1, 1940

By J. H. Faulk

An examination is made of the various factors influencing drilling rate and drill bit life in various diameter holes. It is concluded that drill bits in the size range 4% to 6 1/4 in. can be used to attain substantially the some daily drilling progress as conventional size bits in soft rock drilling operations. An examination of the most important factors influencing "hazard of losing the hole" in the different hole size results in the conclusion that the smaller hole sizes can probably be drilled at reasonably low risk. However, this risk will be somewhat greater in the smaller diameter holes, requiring that special drilling and mud engineering practices be used to make small diameter holes practicable in soft rock drilling operations. An engineering analysia is made of the power and hydraulic requirements of several drill string-hole combinations to test the feasibility of drilling .small diameter holes in soft rock areas. Large econormies in rig power requirements appear possible by drilling .smaller .size holes in these operations. INTRODUCTION The industry now is re-examining the utility of small diameter holes in the light of substantial technical advances made in recent years. Faced with increasing cost of finding reserves and with proration after developing them, the industry must either develop methods of economizing or receive a lower rate of return on investments. Small diameter holes appear to involve an attractive method of economizing. Our objective is to determine if this is technically possible in soft rock operations. Soft rock, as used in this report, refers to those formations of a "drill-ability" corresponding to that of all Gulf Coast formations shallower than and frequently including much of the Eocene rock system. An important phase of technology which we shall examine is relative drilling rate and bit footage which may be obtained with various size bits. Rig operating efficiency, particularly as influenced by hazard, is also discussed in detail. The technical conclusions resulting from these examinations are used to develop sample drill string design and rig horsepower requirements for drilling holes as smaH as 4 3/4 in. and larger. The principal criterion used for the drill string design is that approximately the same daily drilling progress would be possible in all size holes in soft rock operations. This facilitates a comparison of rig size required for drilling the hole sizes in the range between 4 3/4 and 8 3/4 in. BROAD PROBLEM OF DRILLING RATE AND BIT FOOTAGE The three factors controlling daily drilling progress are: (1) drilling rate of bit while on bottom turning, (2) bit footage, and (3) rig operating efficiency. Let us look now at the first two of these factors. Drilling technology has progressed to the point that a semi-quantitative analysis of the effect of various operating variables upon these factors can be made. Those factors which apparently limit both drilling rate and bit footage for bits now in use are: (1) bit design, (2) weight on bit, (3) hydraulic cleaning capacity for bit cutting surfaces and hole bottom, and (4) rotary speed. (We neglect the effect of mud and formation properties because these factors arc the same for the various size bits.

Jan 1, 1957

By J. H. Carpenter

LMENITE, rutile, zircon, and other heavy minerals are found in small amounts in the sand that covers most of Florida. Small enriched deposits occur on the beaches and coastal dunes. One beach deposit east of Jacksonville was worked during World War I and another near Vero Beach during World War 11. Both ceased operation when the resumption of imports reduced prices. Early in World War II reduction of rutile imports made a domestic source of the mineral necessary to maintain the expansion of armaments. Explorations made near Jacksonville discovered a relatively large body of low-grade ore about 10 miles inland from the beaches. A plant installed by Rutile Mining Co. of Florida using both flotation and tables encountered difficulties because of low plant capacity and organic slimes in the ore. In 1944 Humphreys Gold Corp. solved the problem of concentrating the low-grade ore by using the newly developed Humphreys spiral concentrator and by mining with a hydraulic dredge. This combination of low cost mining and concentration permitted the plant to continue operation in competition with foreign ores when imports were resumed following the war. The success of the Jacksonville operation renewed interest in Florida as a source of titanium. An extensive survey of the state was made by E. I. du Pont de Nemours and Co., Inc., under the direction of J. L. Gillson in 1945 to 1946. Sampling was carried on by drive pipe drilling to depths of 20 to 25 ft. Encouraging values were discovered near the location of the present Trail Ridge mine, 50 miles southwest of Jacksonville, near the town of Starke. The United States Bureau of Mines was interested in exploring for heavy minerals in Florida, and on the recommendation of both the state geologist of Florida and of Du Pont geologists, drilled deeper where marginal indications were found on Trail Ridge. In 1947 it was discovered that sufficiently higher values occurred at depth to make the deposit commercial. The orebody at Trail Ridge is a long sand deposit averaging about 1 mile in width and 35 ft in depth. It is approximately 1 1/2 miles wide at the north end of the portion now being worked, tapering to a blunt point 3 miles to the south. The ore reaches a maximum depth of 65 ft near the center and feathers out into barren sand at the edges. The ground surface is relatively flat and is covered with vegetation including pine, scrub oak, palmetto, and occasionally in swampy areas, cypress. The remain of a dense woody growth underlies and marks the bottom of the Ore 'One. It is difficult to drill through this layer, but in some cases where it is less than 5 ft thick it has been possible to drive through the wood. Sand lying below is coarser than that in the ore zone and contains no values. The wood layer consists of unconsolidated carbonized fragments of branches and other forest trash associated with a considerable amount of ar-

Jan 1, 1954

By Eleanor Haslem, Carl A. Zapffe

THE present investigation has three principal purposes: I. To develop a method for measuring hydrogen embrittlement that avoids certain errors complicating previously used methods. 2. To explore in a preliminary way some of the fundamental factors controlling embrittlement. 3. To apply the measurements specifically to stainless grades of steel, whose sensitivity or insensitivity to hydrogen embrittlement has never been clearly defined. SELECTING A TEST METHOD Hydrogen embrittlement is a condition of low ductility resulting from excessive absorption of hydrogen by the steel at some period in its history, and may be revealed by almost any test involving cold deformation. Tensile tests, impact tests, and bend tests are commonly used for detecting hydrogen embrittlement; although numerous other tests, such as cold-upsetting or extrusion, could be used. The simplicity of using a wire specimen for cathodic and acid pickling tests, and the especial adaptability of the bend test to wire specimens, led to selection of the bend test for the present research. Bend tests usually have been of three general types: (I) fatigue, (2) reversed bend, and (3) single bend. The first two types, though widely used, are inaccurate because their measurements are counteracted by an aging effect; and the third type has not been developed to its fullest utility. The effect of cold-working in removing hydrogen is well known. During a bend test hydrogen can be observed escaping from the convex side simply by coating the specimen with oil; and any technique employing flexing or reverse bending may therefore have its measurements masked because the mechanical action reduces the embrittlement during the test. This factor is so important that even elastic flexing of a hydrogen-charged wire specimen should be avoided before testing if accurate measurements are desired. DEVELOPING A MACHINE FOR MEASURING HYDROGEN EMBRITTLEMENT As for the single-bend test, its theory is good, and recovery caused by mechanical work is kept to a minimum. With a given degree of hydrogen embrittlement, a specimen will break at a given angle if the bending is applied unidirectionally and uniformly. The radius of the bend must be kept constant; and the rate of bending should be a constant, slow enough to allow reading of the breaking angle, and yet rapid enough to prevent significant recovery from the escape of hydrogen during bending. A simple apparatus (Fig. I) was constructed using a type H Foxboro drive unit A, which is a synchronous motor with a gear-reduction ratio of 600 to I. A cord, fixed at one end to a wooden pulley B on the drive shaft of the motor, follows the pe-

Jan 1, 1946

(The paper by L. H. De Wald-Tech. Pub. No. 429 was presented at the Boston meeting, September, 1931.) W. A. SCHEUCH, Chicago, Ill.-Since starting up our Hawthorne copper wire plant we have found that wire bars from certain suppliers perform quite differently from those of other suppliers. In attempting to evaluate these bars, we made cross-sections, and in making these cross-sections we found considerable variation in the crystal structure. Indications were that there was some preference in the type of crystal structure. In attempting to find the reason for that we discussed it with the various producers and-also reviewed the literature. Mr. DeWald was assigned to determine the various factors that enter into copper wire bar crystal structure, on the basis that the product was a horizontally cast wire bar of practically identical composition and of recognized good composition for the present quality product sold in the market. Mr. DeWald has asked me to say that he should have made reference to Mr. Dalzell's paper on a theory concerning gases in refined copper. D. K. CRAMPTON, Marion, Conn. (written discussion).-Mr. DeWald has set forth an interesting and thorough exposition of the factors controlling macrostructure of this material. It is particularly interesting to us as it somewhat parallels work we have done on macrostructure of round copper billets for piercing into tubes. Our findings as to the effect of the several variables on macrostructure check Mr. DeWald's. The general principles underlying the two are precisely the same. The fact that we worked with copper deoxidized with phosphorous instead of tough-pitch copper, and round billets cast on end instead of wire bars, does not influence the results. We have found that round billets cast so as to produce large radial grains have greater soundness and density than those with a fine macrostructure. Further, and more important, we have found that the billets with large radial grains show markedly different performance on piercing from those having a fine equiaxed structure. With a given temperature of billet and adjustment of piercing machine, the coarse-grained material requires appreciably lower power for piercing and goes through the operation inn appreciably less time. These two differences are of sufficient commercial importance to warrant exercise of great care in maintaining the coarse structure. It seems probable that much the same phenomenon should hold in the hot rolling of tough-pitch wire bars. We would expect that, other things being equal, the coarse-grained wire bars would roll more readily and require less power than fine-grained ones. Moreover, we believe the differences in initial structure of the wire bars should be largely eliminated in the hot rolling process and during the subsequent drawing and annealing, of wire would be entirely eradicated.

Jan 1, 1932

By T. H. Dunn, P. L. Menaul

This paper discusses the results of an investigation made to develop a method of combatting corrosion of subsurface oil-well equipment caused by brines containing hydrogen sulphide. Carbon monoxide, aldehydes, and certain cyanide compounds were found by laboratory tests to effectively inhibit corrosion of steel by sulphide brines. Experiments were made for one year in eight wells in West Texas fields using formaldehyde as an inhibitor. It was found that the inhibitor treatment successfully prevented the severe corrosion previously experienced in these wells, and effected important net savings in operating costs. Introduction Corrosion of oil-field equipment has long been a problem in areas producing sour crudes. These areas include the major fields of Arkansas, Western Kansas, West Texas and New Mexico. Corrosion in these fields is caused primarily by the chemical action of hydrogen sulphide in the presence of water and by electric currents entering the wells through flow lines. Hydrogen sulphide is noncorrosive to iron or steel in the absence of water but under the usual conditions prevailing in oil wells where more or less water is present, hydrogen sulphide is very corrosive. This type of corrosion occurs over the pH range below 9, which includes all natural oil-field brines. If air is present in addition to hydrogen sulphide and water, corrosion proceeds at an extremely rapid rate. It was reported several years ago that a string of oil-well tubing was literally dissolved within 50 days where an air lift was used on a well producing considerable water and hydrogen sulphide. Air is generally absent in wells producing sour crude. After hydrogen sulphide corrosion starts, it proceeds with increasing severity and its correction becomes progressively more difficult. This characteristic of sulphide corrosion has been attributed to the formation of galvanic couples between the iron and steel equipment on one hand and the products of corrosion on the other.' Severe corrosion of subsurface oil-well equipment leads to a multitude of troubles. In addition to destruction of costly equipment, producing sands often are damaged by flooding with water leaking through corroded casing; bad mechanical conditions may develop in a well due to obstructions caused by corroded equipment lost in the hole, or partly collapsed casing; pumping operations are interfered with, and severe emulsification problems may result from the homogenizing action of corroded balls and seats.% A typical case of severe corrosion caused by hydrogen sulphide was reported in Howard County, Texas, where it was necessary to pull tubing once a week to repair leaks after the tubing had been in use for only one year. On one well in this area a string of tubing was pulled 11 times in 8 months; 11 joints of tubing being replaced because of leaks. In Ector

Jan 1, 1946

By C. Kolm, E. P. Warekois, S. A. Kulin

MUCH insight has been gained into the nature of the cold-worked state of metals in recent years through the use of modern X-ray techniques. These methods have revealed the existence of stacking faults together with regions of high internal strain and have provided means of measuring the atomic perturbations in plastically deformed metals. In view of the recent increased interest in the solid state, it is desirable to extend these techniques to the study of lattice imperfections introduced into semiconductors during plastic deformation. It is of particular interest to compare the state of imperfection sustained by metallic bonding with that sustained by the covalent bonding found in semiconductors. A knowledge of the imperfections which can exist in semiconductors is important from both a theoretical and a practical point of view since they can greatly influence many of the physical properties. In order to determine the possible existence of stacking faults in covalently bonded structures, precise measurements were made of the diffracted peak positions of plastically deformed germanium, gallium antimonide, and indium antimonide. These measurements were based on the theoretical treatment of Paterson1 and are similar to those employed by Warren and warekois2 in their studies of deformed a brass. In addition, diffraction peak profiles were measured on the annealed and plastically deformed materials in order to obtain information concerning the distribution of internal strains through the use of the Fourier methods developed by Warren and Averbach.3 EXPERIMENTAL PROCEDURES AND TECHNIQUES Because of the room-temperature brittleness of the semiconductors studied, it was necessary to plastically deform the materials at elevated temperatures. The brittle-ductile transition temperature ranges of GaSb and InSb are sufficiently low to permit hot-filing operations. Therefore, high-purity, polycrystalline GaSb and InSb were filed in an argon atmosphere at 400' and 300°C, respec-

Jan 1, 1959

By G. R. Belton, R. J. Fruehan

The Knudsen cell-mass spectrometer combimtion has been used to study the Fe-Al and Ag-Al liquid alloys. By application of the recently developed integration technique to the measured ion-current ratios, activities have been derived for the Fe-A1 system at 1600° C and for the Ag-Al system at 1340"C. The results are partially represented by the following equations: Internal consistency between the data on silver-rich and iron-rich alloys is demonstrated by application of the literature measurements on the distribution of aluminum between the nearly immiscible liquids iron and silver. The usual restrictions on the ratio of the mean free path of the escaping atoms to the orifice diameter of the Knudsen cell are shown not to be limiting in this technique. DESPITE the importance of a knowledge of the activity of aluminum in understanding deoxidation equilibria in molten steel, no direct studies have been made of activities in liquid Fe-A1 alloys at steel-making temperatures. Lower-temperature direct studies have, however, been carried out on aluminum-rich liquid alloys by Gross, Levi, Dewing, and Eilson' at 1300°C and by Coskun and Elliott' at 1315°C. Apart from phase diagram calculations by Pehlke, other determinations have been indirect and were made by measurement of the distribution of aluminum between iron and silver475 and combination of these data with extrapolated activities in the Ag-A1 system.~-% ecently, however, Woolley and Elliott have made a significant contribution by directly measuring heats of solution in the Fe-A1 system at 1600°C. The present authorslo have recently employed a Knudsen cell-mass spectrometer technique in a study of activities in iron-based liquid alloys. In this technique activities and heats of solution are determined from a series of measurements of the ratio of ion currents of the components; and since ion-current ratios are used, problems caused by changes in instrument sensitivity or cell geometry are overcome. Results obtained for the Fe-Ni system were found to be in excellent agreement with previous work, thus demonstrating the reliability of the method. The present paper describes a similar study of activities in the liquid Fe-A1 and Ag-A1 systems, this latter system being included in order that a meaningful comparison can be made with the above-mentioned indirect studies. INTEGRATION EQUATIONS A detailed derivation of the equations used to determine the thermodynamic properties from the measured ion current ratios has been given elsewhere;'' however it is useful to summarize them here. By the combination of the Gibbs-Duhem equation with the direct proportionality between ion-current ratios and partial pressure ratios, it was shown that for a binary system at constant temperature and pressure: where al is the activity of component 1 with pure substance as the standard state, N, is the atom fraction of component 2 in the solution, and I; and t'2 are ion currents of given isotopes of the components. The activity coefficient is given by: this latter equation being more suitable for graphical integration. Combination of Eq. [l] with the Gibbs-Helmholtz equation gives an expression for the partial molar heat of mixing: EXPERIMENTAL A Bendix Time-of-Flight mass spectrometer model 12! fitted with a 107 ion source and a M-105-G-6 electron multiplier, was used to analyze the vapor effusing from the Knudsen cell. The arrangement of the Knudsen cell assembly was essentially that of the commercial instrument (Bendix model 1030) but with several modifications. Instead of heating with a single tungsten filament, a cylindrical tantalum-mesh heater was employed. Up to 1400°C simple resistance heating was used but above this temperature electron bombardment between the tantalum mesh and the tantalum cell susceptor was necessary. The temperature was measured by means of a Leeds and Northrup disappear ing-filament type optical pyrometer sighted on an essentially black-body hole in the side of the cell. Details of the temperature control, temperature measurement, and in situ calibration of the optical pyrometer can be found elsewhere.I0 In the investigation of the Fe-A1 system the Knudsen cells were constructed of thoria crucibles with fitted thoria lids (Zircoa). The cells employed in investigating the Ag-A1 alloys were made up of high-purity alumina crucibles (Morganite) with lids of recrystal-lized alumina (Lucalox). The cells were 0.370 in.

Jan 1, 1970

By G. P. Conard, E. H. Rennhack

The creep behavior of hot-rolled, hypoeutectic Zn-Ti alloys was investigated in the temperature range from 0.43 to 0.53 TM. Secondary flow was found to originate primarily from strain-induced gvain growth where grain boundary )nigvation served to relieve the strain energy of distortion introduced by slip, grain boundary sliding, and subgvain formation. The extent to which this recovery mechanism operated was determined by the ratio of grain width to the spacing between planar fibers of TiZn,, compound particles generated in these alloys during rolling. When this ratio was unity, creep resistance demonstrated a marked improvement. In this condition, which was fulfilled by annealing following rolling, structural stability was enhanced with decreasing grain size below the equicohesive temperature (-0.5Tm), while the reverse was true above this temperature. TITANIUM concentrations approaching the eutectic composition of 0.23 wt pctl have been shown to promote a significant increase in the creep resistance of rolled zinc,2 The alloying effect created with titanium is somewhat unique; a structure closely resembling that of a fiber-reinforced metal composite can be developed which selectively modifies creep strength in preference to other mechanical properties. In an earlier investigation,~ the present authors found that, while the fiber network, composed of individual TiZn,, compound particles, had a distinct influence on rolled texture, the crystallographic variations produced were of minor importance with respect to creep. Rather, creep resistance seemingly increased when the grain size appeared to coincide with the in-terfiber spacing. The work described here was undertaken to explore this effect in greater detail. EXPERIMENTAL PROCEDURE Three zinc-base alloys containing 0.05, 0.12, and 0.16 wt pct Ti were prepared from CP zinc and iodide titanium in the form of 4 by 2 by f in. chill-cast ingots. The melting and casting procedures for these alloys have been detailed el~ewhere.~ Individual ingots of each alloy were hot-rolled at 200°C (392°F) to total reductions of 10, 25, 50, 75, and 90 pct in from one to five passes, respectively, employing a 10-min reheat prior to each rolling pass. With grain, tensile-type creep specimens with a 1-in.-long, -in.-wide gage section were machined from the rolled strips for test purposes. Annealing studies to explore the influence of grain size on secondary creep flow were carried out at 400°C (752°F) in argon for times extending up to 60 min. The grain-size effect was evaluated in terms of average grain width and length values statistically derived from lineal intersection measurements.4 A similar method was applied in establishing the average interfiber spacing, i.e., average perpendicular distance between adjacent planar fibers. The creep characteristics of the alloys were investigated by means of constant-load and constant-stress creep tests. The former tests were conducted at 25°C (77°F) under an initial stress of 10,000 psi, while the latter were performed in the range from 25°C (77°F) to 90°C (194°F) at stress levels varying from 8000 to 22,000 psi. Total specimen strain, as determined with Budd HE-1161-B strain gages, was in excess of 0.10. Maintenance of constant stress was achieved through periodic load reductions made at 0.01 strain intervals to compensate for the attendant incremental reduction in specimen cross-sectional area. The maximum indicated error in the applied stress at these strain intervals was less than 3.0 pct. RESULTS AND DISCUSSION Constant-Load Creep. In an effort to clarify the in-terrelation between interfiber spacing and grain size with respect to the creep resistance of the Zn-Ti alloys, their separate effects on secondary creep rate were determined as a function of titanium content and rolling reduction. These results are set forth in Figs. 1 and 2, respectively. The average grain diameter plotted in Fig. 2 was resolved from average grain width and length values. No data are presented for reductions of less than 50 pct because of the inability to obtain consistent measurements on these strips. The curves of Fig. 1 indicated that, for a given titanium content, a decrease in interfiber spacing, as produced with increasing reduction, promoted a decrease in creep rate. Depending on titanium content, however, wide variations in creep rate occurred at the same interfiber spacing suggesting that interfiber spacing, by itself, has little or no influence on creep resistance. Grain size, on the other hand, decreased progressively with both increasing rolling reduction and titanium content, the effect of which led to a pronounced decrease in creep rate, particularly when the average grain diameter became smaller than 3.0 x 10"4 in., Fig. 2. The continuity of this relationship tended to support the view that grain size rather than interfiber spacing was predominant in controlling secondary creep. Annealing Effect. The observed dependence of creep flow on grain size suggested that a further contribution to creep resistance would result when the alloys were annealed to effect a coincidence between grain width and interfiber spacing, see Fig. 3(b). ~eiides creating an immediate barrier to grain boundary movement, annealing offered the possibility of providing increased structural stability by eliminating many high-energy, mobile grain boundaries.= To test this hypothesis, specimens from the Zn-0.16 Ti strips reduced 75 and

Jan 1, 1967

By Laurence Delisle

The aim of this paper is the description of a technique to be applied to the study of sections of metal powder particles, less than 20 microns in diam. with the electron microscope, by the replica method, using for replica a material such as formvar or parlodion. This work originated with the study of particles of tungsten powders. Such particles were too small to be examined in sufficient detail with the light microscope. On the other hand, examination with the electron microscope of the powders dispersed in the supporting film was not found satisfactory because: 1. It did not permit differentiating between single particles and aggregates. 2. It did not show the true outlines of the particles but only the projection of a whole surface. 3. No details appeared. For that reason it was attempted to make replicas of sections of the particles imbedded in a mounting material suitable for polishing and etching. The method proved satisfactory for the examination of tungsten powder and was then extended to car-bonyl nickel and carbonyl iron powders. Procedure Several mounting materials commonly used in ordinary metallography were investigated. The problem consisted in finding a mounting material

Jan 1, 1950

By F. Keller, R. H. Brown

BECAUSE of the extensive use of Alclad 24s alloy sheet in aircraft construction, there is much interest in the metallurgical changes caused by heat-treatment of this product.1,2 One of these changes is the result of the diffusion of soluble elements from the core into the coating during treatment. This paper deals with the thermal treatments that may influence diffusion and with the practical effects of diffusion on the serviceability of the product. As is well known, Alclad 24s-T sheet has a core of high-strength alloy combined with surface layers of relatively pure aluminum. The microstructure of a cross section of this product is shown by Fig. I. hot only does the relatively high-purity coating have a high resistance to corrosion, and hence serves as a mechanical barrier between the core metal and the corroding environment, but in addition this coating I exerts electrochemical protection over areas where the core may be exposed, such as cut edges. In addition, the coating affords electrochemical protection to projecting heads of *417S-T, 17S-T and 24S-T rivets, or attached members made from these alloys. Under some conditions of heat-treatment, however, diffusion of copper into the coating will alter the electrochemical relationship between the coating and the core to the extent that only partial protection will be obtained under some corrosive conditions. The reason for the electrochemical protection lies in the fact that the coating layers of pure aluminum are anodic to the alloy core. The addition of copper to aluminum produces alloys in which the potential is lower than that of the pure metal. Moreover, as the amount of copper in solid solution in z4S alloy is increased, the potential of the alloy becomes more cathodic. When heat-treated at 920°F. and quenched in cold water, 24s-T is about 0.16 volt cathodic to pure aluminum. However, copper will diffuse from the core into the coating, and if it reaches the surface the potential will be altered in a cathodic direction. Thus the potential dif-erence between the core and coating may be less than 0.16 volt, depending upon the thickness of the coating, and the time and temperature of heat-treatment. Of the methods available for determining the extent of diffusion of copper from the core into the coating of Alclad 24S-T, two are generally used; namely, the metallographic and the solution potential method.3 METALLOGRAPHIC METHODS Metallographic methods will reveal the progress of diffusion of copper into the coating. For instance, the diffusion zone in the coating intermediate between the coating surface and the core is shown in Fig. I. This photomicrograph is of a polished and etched cross section of 0.040-in. Alclad 24S-T sheet. Diffusion proceeds into the coating more rapidly along the grain boundaries than through the body of the grains. consequently, the diffusion zone is not of uniform width

Jan 1, 1944