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By G. D. Tranter

THE importance of ladle and teeming practice and its relationship to the yield and quality of the product has focused considerable attention on this phase of open-hearth operation. Inherently bad steel cannot be perfected by manipulation during teeming, but through the proper handling of "off heats" serious losses, which in many cases arise, can be greatly minimized. Conversely, good steel can be ruined as a result of poor workmanship in the pit, and rendered unsuitable for application to orders where exacting surface and physical requirements are essential. Sufficient evidence has been secured to warrant careful investigation of pit operations when an abnormal number of basic defects develop in the semifinished product or are found on the inspection table. This paper is written from the standpoint of the problems involved in making satisfactory ingots for sheet rolling. Furthermore, since rimming steel is almost universally used for manufacture of sheet, the data presented herein refer particularly to that type of steel. Going back some 30 years in open-hearth history, the word "pit" properly described the hole into which the ladle was lowered to receive the metal tapped from the furnace. The working space was necessarily limited, and the disposal of slag and metal overflowing the ladle or lost because of breakouts presented a serious problem. The equipment, of course, was rather crude in the light of present-day development. Often no ladle stands were provided, the ladle being hung on the crane beneath the runner. When delayed taps occurred, the ladle was often held in position for many hours, thus tying tip pit operations and causing delays to adjacent furnaces. Because of crowded conditions, slag thimbles were not used and a network of cast-steel triangles and old tapping bars, placed before the heat was tapped, was the means for removing slag from the hole. Furnaces of different capacities were used

Jan 1, 1935

By Ian Wark

SODIUM sulfide is used extensively to increase the recovery of oxidized copper and lead minerals by flotation, particularly when using xanthates as collectors. It is generally assumed that the sodium sulfide converts a film of the oxidized mineral to the sulfide, and that the xanthate, while not a very effective collector for the oxidized minerals, is a good collector for the sulfide. On the other hand, Taggart and his collaborators' claim that unless sulfide minerals are oxidized they cannot adsorb xanthates and do not float. Gaudin2 states that amyl xanthate, used in conjunction with sodium sulfide, gives better results than ethyl xanthate. Rabone3 and Mayer-Schranz4 agree that excess of sulfide functions as a depressant. Owing to the greater solubilities of the oxidized minerals than of the sulfides, the consumption of sodium sulfide is greater than that of most other flotation reagents, up to 10 lb. per ton of ore being used in some plants. Luyken and Bierbrauer5 recommend a water washing to remove soluble heavy metal salts; by this means sulfide consumption may be reduced. It was desirable to determine the limits of the sulfide concentrations between which contact is possible at surfaces of anglesite and cerussite in xanthate solutions. Similar determinations were desirable for the sulfide minerals with which the oxidized minerals are usually associated, since conditions should be chosen, if possible, so that the two types of mineral will float together. Because of the formation, especially in acid solutions, of hydrogen sulfide and of the hydrosulfide ion (HS-), the permissible limits of sulfide addition are obviously dependent upon the pH value. Sphalerite responds to ethyl xanthate only in the presence of an activator; for example, copper sulfate. It was necessary, therefore, to determine whether sodium sulfide interferes with the activation of sphalerite by copper sulfate. The combined effect of sulfide and copper sulfate was determined also for galena, chalcopyrite and pyrite.

Jan 1, 1936

By Newell Hamilton

Some years ago, in the manufacture of seamless tubing from an alloy steel containing 0.07 per cent maximum carbon, 18 per cent chromium and 8 per cent nickel, at the plant of The Babcock & Wilcox Tube Co., a peculiar type of piercing defect was noticed. This defect was definitely associated with certain heats of the alloy and was independent of any of the variables of mill operation and billet-heating condition. A thorough analysis of the defective material yielded but one clue to the reason for its abnormal behavior in piercing and that was its oxygen content as determined by the vacuum fusion method. The oxygen content of the defective 18-8 alloy was found to be from two to three times that of the material that had pierced satisfactorily, and this incited an active interest in the vacuum fusion method for the analysis of alloy steels. After a critical survey of the literature on this subject, and considerable experimentation, an apparatus and technique were evolved that gave a fairly rapid, simple and reliable method of analysis. Samples selected from six years of tube production of 18-8 and other corrosion-resistant alloys were analyzed by this method. This paper describes the procedure and gives a correlation of the oxygen, hydrogen and nitrogen contents of a number of alloy steel samples representative of good and bad tube-piercing quality. The Apparatus Basically the apparatus used in this work was that of Jordan and Eckman,' employing a high-frequency induction furnace and the gravimetric method of analyzing the evolved gases, nitrogen being excluded from the determination. In addition, a magazine-type cap and a large-

Jan 1, 1934

By A. C. Heath, E. H. Dix

The importance of aluminum-silicon alloys in thc light alloy field is now generally recognized. Where silicon was once considered detrimental to the properties of aluminum, useful alloys now contain as much as 13 per cent. Furthermore, silicon is present as an impurity in aluminum of even the purest grades. Iron is another important impurity in aluminum and likc silicon is found in small quantities in the purest aluminum available today. The manner of occurrence of iron and silicon in commercially pure aluminum and many of its alloys exerts a very pronounced influence upon their properties. The effect of large quantities of iron in aluminum-silicon alloys is so detrimental that it has been found necessary to limit the allowable maximum percentage to as low a figure as is consistent with quantity production and satisfactory physical properties. The intimate relation existing between iron and silicon in aluminurn and alurninum alloys makes necessary a more complete knowledge of this ternary system. This paper is divided into two principal parts, dealing respectively with aluminum-silicon solubility equilibria and the constitution of aluminum-iron-silicon alloys. Part I.—Aluminum-silicon Alloys The early work on this system was largely confined to determining the general form of thc diagram and in this respect the results are in good agreement. Briefly, alulninunl and silicon form a simple eutectifcrous series without compounds. Until recently the solid solubility of silicon in aluminum had not been accurately determined. Ipraenkell (1908) stated that aluminum will retain 0.5 per cent. silicon in solid solu-t'ion. Rosenhain, Archbutt and Hanson2 gave the maximum solubility as about 1.50 per cent. and added that "this solubility docs not appear

By V. L. Minear

This paper presents some of the problems encountered and solved by the construction industry during recent years while pressure grouting the foundation rock of dams. Pressure grouting has become "Standard Operational Procedure" and consequently many hundreds of thousands of bags of cement have been used for that purpose. There is nothing weird, mystical, or even particularly difficult about the basic idea. Holes are drilled in the rock and grout is pumped into them. This procedure is used to shut off the flow of water under the dam and to reduce the uplift on the dam. Like most other engineering and construction problems, the fundamental principle is simplicity itself, but some of the "minor details" are rather complex. When faced with the problem of actually forcing the grout into the rock, or keeping it there once it has been injected, an engineer frequently has need for all of the ingenuity and initiative that he has at his disposal. It is proposed to discuss these minor details at length, even at the risk of boring the reader. The difference between success and failure in a grouting program can well hinge upon some such detail that may not be fully understood. Pressure grouting is a method used to make good foundations from bad ones by plugging actual or potential passages within the rock through which water might escape and thereby diminish or even destroy the usefulness of the dam. In some special cases, pressure grouting has been used for the purpose of consolidating broken rock to increase its bearing power. Lacking this useful method, many of the dams constructed during recent years could not have been built. Most of the really excellent dam sites in this country have been utilized long ago. Consequently it becomes necessary to find methods of utilizing the less desirable sites. Pressure grouting plays a vital role in the methods developed. Engineers have learned the hard way, that the term "solid rock" is a misnomer. Solid rock does not exist to any considerable extent in nature. Practically all rock contains imperfections such as shrinkage cracks, bedding planes, joints, solution channels, folds, shear zones, crush zones, and the like. All these imperfections are weaknesses through which ground water is likely to flow. The function of rock grouting is to rectify these imperfections and make the rock as nearly "solid" as practicable. The location, direction, depth and number of grout holes to be drilled are important. Clearly, a hole must pierce fractures in order to serve a useful purpose, for grout cannot be forced into the rock itself. Were it possible to determine the pattern and extent of the cracks within the rock, it might be feasible to drill two or three strategically placed holes so as to make practicable the grouting of the whole integrated network of cracks from them. Such is not the case. While a study of the geology, surface indications, and drill cores is helpful in gaining an idea of subsurface conditions, in the final analysis, the seams must be located by trial and error methods. There can be no doubt that the closer the

Jan 1, 1949

By H. B. Pulsifer

This paper outlines a method for rapid production of flat,, granular surfaces on many of the medium hard alloys. Grinding wheels and fabrics on wheels are not used; the purpose is accomplished by rubbing on emery papers and on fine abrasives heaped on hand boards. The advantages of chromic acid in the solutions for etching nickel and copper alloys are explained. Steels may require an additional step in the mechanical smoothing owing to the lack of an ideal etchant. Chloric acid is a rapid etchant for steel. Thirty-six photomicrographs illustrate the steps in smoothing and the clearness with which structures can be rapidly exposed. New structures in low-carbon steels are announced. After a little practice, many materials can be finished within two or three minutes. CUPRONICKELS In the previous papers on the metallography of copper and magnesiurn which the author has presented to this Institute there has been an attempt to demonstrate the advantages of minimizing the mechanical work of surfacing and depending more on chemical means; the present paper continues the research into a still wider field. It is obvious that the success of a chemical method for smoothing and etching depends almost entirely on the use of a suitable reagent. The etchant must remove the surface granulations and outline the structures. A very special type of reaction between reagent and metal must be displayed. Promiscuous corrosion or the intensification of the attack about local couples formed by impurities or components must not be in evidence. There are several reagents that etch highly polished nickel and copper alloys very well. Acidified ferric chloride solutions, concentrated and dilute nitric acid solutions, and nitric and acetic acids in acetone have been used to good advantage for the purpose. However, if they are expected to etch rather deeply—that is, smooth as well as characterize— the results may be far from satisfactory. Advantages of Chromic Acid In a protracted series of experiments it has been found that the addit,ion of chromic acid may be of the most surprising benefit. The function

Jan 1, 1929

By H. B. Pulsifer

This paper outlines a method for rapid production of flat,, granular surfaces on many of the medium hard alloys. Grinding wheels and fabrics on wheels are not used; the purpose is accomplished by rubbing on emery papers and on fine abrasives heaped on hand boards. The advantages of chromic acid in the solutions for etching nickel and copper alloys are explained. Steels may require an additional step in the mechanical smoothing owing to the lack of an ideal etchant. Chloric acid is a rapid etchant for steel. Thirty-six photomicrographs illustrate the steps in smoothing and the clearness with which structures can be rapidly exposed. New structures in low-carbon steels are announced. After a little practice, many materials can be finished within two or three minutes. CUPRONICKELS In the previous papers on the metallography of copper and magnesiurn which the author has presented to this Institute there has been an attempt to demonstrate the advantages of minimizing the mechanical work of surfacing and depending more on chemical means; the present paper continues the research into a still wider field. It is obvious that the success of a chemical method for smoothing and etching depends almost entirely on the use of a suitable reagent. The etchant must remove the surface granulations and outline the structures. A very special type of reaction between reagent and metal must be displayed. Promiscuous corrosion or the intensification of the attack about local couples formed by impurities or components must not be in evidence. There are several reagents that etch highly polished nickel and copper alloys very well. Acidified ferric chloride solutions, concentrated and dilute nitric acid solutions, and nitric and acetic acids in acetone have been used to good advantage for the purpose. However, if they are expected to etch rather deeply—that is, smooth as well as characterize— the results may be far from satisfactory. Advantages of Chromic Acid In a protracted series of experiments it has been found that the addit,ion of chromic acid may be of the most surprising benefit. The function

Jan 1, 1929

By A. E. Worthington, R. F. Meldau

An analog computer study was made of the reduction of the magnitude of the SP by formation geometry and resistivity effects. Practical field .situations were studied. The analog data were converted to the form of departure charts. These charts may he used to determine the reduction in the SP due to the above eflects pith good precision Quantitative interpretation of the SP log in terms of formation water resistivity is presently based on the premise that the observed SP is equal to the electrochemical potential developed across a shale between the mud filtrate and the formation water. This procedure inherently assumes that, first, no electro kinetic (streaming) potential is present, and, second, that the SP is not reduced by resistivity or geometry effects in the formation. When, however, such a reduction of the observed SP does occur, one may write, SP = b,E, b, E, (1) where SP is the observed self-potential opposite the center of the bed under consideration. In this case, E, is the electrochemical potential, E, is the electrokinetic potential, b, is the electrochemical reduction factor, and h, is the electrokinetic reduction factor. The first assumption above is equivalent to assuming E, = O in Eq. 1 and the second assumption is equivalent to h, = b, = 1. Examination of electric logs shows that for many formations of interest the observed SP is reduced below its maximum value. The object of this work is to aid quantitative SP interpretation in at least some of these situations by obtaining values for b, and b, in Eq. 1 as functions of realistic combinations of bed thickness, depth of invasion, and formation resistivity. The only previously published work in this field known to the authors is by H. G. Doll' in 1948. He evaluated b, under conditions permitting exact analytical solution. His work clearly established the importance and qualitative nature of formation geometry and resistivity effects upon the SP, but the necessity of obtaining analytical solutions restricted his study to situations of limited practical interest. In order to extend such studies to practical combinations of formation parameters which do not lend themselves to feasible analytical solutions, the results reported in this paper were obtained by use of a special analog computer. THE ANALOG MODEL The analog model used for this study was the Guyed Analog Computer which originally was designed and built for resistivity log departure curve studies. It consists of a two-dimensional mesh of resistors, with the vertical mesh corresponding linearly to vertical distance along the borehole, and the horizontal mesh corresponding to radial distance from the borehole axis. By proper choice of horizontal resistor values, a three-dimensional, axially symmetric, borehole-formation problem can be modeled with this two-dimensional array. These and other details of the model are contained in a paper by H. Guyod'. The geometry used for the SP studies with the analog is depicted in Fig. 1. This configuration has a horizontal plane of symmetry, and, hence, the model, and the following discussion, need only to be concerned with one quadrant such as shown in Fig. 2. A further simplification arises by considering that both the natural potential sources and those used in the model have fixed internal impedance. Therefore, the current flows produced by these sources can be separated and studied independently ( i.e., the superposition theorem can be applied). SP = SP, i SP, = h,E, + b,E, ,(7)

By R. P. Alger, M. P. Tixier, D. R. Tanguy

In the combination induction-electrical log used at present in the field, the induction logging tool is appropriate for the investigation of moderately invaded formations. A new induction sonde with a radius and investigation about twice as large has been developed recently for the case of deep invasion. It has very nearly the same vertical resolution as the present sonde so that thin beds are defined as accurately as before. The characteristics of the new tool are described, the corresponding interpretation charts are given and field examples are discussed. The design of the sonic logging tool has been modified to improve the calibration and the reliability. The fact that porosity can be accurately recorded by means of the sonic log has prompted new interpretation procedures for saturation estimation, wherein the data concerning the various permeable beds in a given well are correlated. One approach consists of plotting transit time vs true resistivity, with an appropriate scale. With this approach, saturations can be estimated conveniently even in cases where formation water resistivity is not well known. In another approach, a comparison is made of the values of the formation waters computed from the re- sistivity and sonic logs. Using the concept of continuity, this procedure makes possible a quick determination of zones of saturation in shaly sands and/or in case of appreciable variations of formation salinities with depth. It has been found that the comparison of porosity from the sonic log with the apparent porosity computed from a short-investigation resistivity log may reveal, in many cases, the presence of residual oil and thus detect potentially productive formations; this procedure is valuable when the true formation resistivity and the resistivity of the formation water are in doubt. INTRODUCTION During the past year, the efficiency of log interpretation has been vastly improved. The improvements have largely resulted from the introduction of a deep-investigation induction device and from the application of new interpretation techniques that utilize sonic vs resistivity readings. Since the new interpretation techniques depend, in part, upon good values of true formation resistivity, the new induction log will be discussed under Part I. The sonic interpretation techniques will be studied under Part 11. Early in 1959, the 6FF40 induction equipment was introduced in the field. This device was designed for a better approach to true formation resistivities in deeply invaded zones. The greatly improved radial investigation of the 6FF40 equipment has been achieved without sacrificing vertical resolution. The first combination induction-electrical log, the 5FF40, was introduced as a standard tool in 1956 for the logging of wells drilled with fresh muds. The tool has received wide industry acceptance in the United States. 'The 5FF40 induction log has a radial investigation sufficient to overcome average depths of mud filtrate invasion. At 5d invasion, for example, the 5FF40 induction log will read about 1.4 R. in a water sand where R., = 10R,. At 10d invasion, such induction log would read 2.45 R. in the same water sand. In either case, the effects of invasion would not be sufficiently great to cause a water sand to be mistaken for a shale-free oil- or gas-producing zone. Some formations, however, invade deeply — in excess of 10d. Such water zones could be mistaken for oil-or gas-saturated sands unless the porosity balance' can clearly make the distinction. It is for these deeply invaded formations that the 6FF40 was developed. CHARACTERISTICS OF THE 6FF40 Radial Investigation Characteristics To describe the comparative responses of the 5FF40

By H. L. Teicliman, E. M. Sipprelle

ENACTMENT of Public Law 290 by the 78th Congress authorized the U. S. Department of the Interior, Bureau of Mines, to conduct an experimental program to develop the technology for obtaining oil from oil shale. In adopting and later extending this legislation, the Congress recognized the impending necessity of supplementing ground petroleum reserves with synthetic fuels. Under the provisions of this legislation, the Bureau of Mines, among other things, was charged with the responsibility of developing mining techniques, methods, and equipment for mining the oil shales of the Green River formation of Colorado, Utah, and Wyoming.

Jan 1, 1950

By Paul Tyler

FULLY a decade ago, demand for ground mica began to exceed supplies of scrap mica from manufacturing operations and of waste block from feldspar and sheet mica mining in the United States, with the result that in recent years the market has absorbed larger and larger quantities of mica recovered as a by-product from clay washing,1 as a joint product with kyanite,2 and by grinding schists. So far, only schists that contain a large percentage of mica have been utilized for making ground mica, but already there has been a good deal of wishful thinking with regard to recovering mica as an aid to the prospective working of low-grade gold ores and ores of certain base metals. With wet-ground mica selling at $60 to $100 a ton and even dry-ground mica worth over $20 a ton, many ores that could not be considered as otherwise workable under present conditions will show commercial possibilities if they can be made to yield even a relatively small percentage of salable mica. An interesting paper might be written on the coming role of industrial minerals as joint products of metal mines, It is largely a matter of mar-kets. Many years ago I watched the mess left behind the gold dredges in the mountains of Colorado and thought of the Denver sand and gravel operators who prided themselves upon their canniness in providing devices for catching gold merely as an incident to their regular business of selling what we miners classed as "tailings." Nowadays almost every milling or mining operation near settled communities finds use for at least part of its waste for road material or concrete aggregate and several eastern iron mines have gone into the crushed-stone business. Promoters now mention fertilizer "filler" as potentially salable at all the way from $1 to $10 a ton, or whatever is needed to cover costs of mining and treating the "ore" and leave the metal values as "clear profit." In emulating the pork packers in their efforts to utilize "everything but the squeal,"

Jan 1, 1938

By D. L. McElroy

It is too broad a statement to say that the mine car is the most important unit in a haulage system, but almost every mining man will admit that it is one of the most important. The mine car is to the mine haulage system what the railroad car is to the railroads; the main purpose in each instance is to move the greatest number of ton-miles of material at the least cost. The data presented in this paper are taken from a study of mine haulage conducted by the School of Mines of West Virginia University at 42 mines in 8 coal fields of Wrest Virginia. The study was made possible by a graduate fellowship of the School of Mines and the cooperation of the mining companies of the state. Three important factors in the use of mine cars in West Virginia are: (I) the number of mine cars in use per loader; (2) the capacity of mine cars; (3) the distribution of mine cars. ("Loaders" in this paper refers to all men loading coal, whether manually or mechanically.) During the World War many mine managers were annoyed by the reduction of efficiency and production caused by railroad-car shortages. Today relatively little complaint is heard about a shortage of mine cars, yet possibly 50 to 75 per cent. of the mines in West Virginia are suffering from this cause of reduced production and increased costs. The railroads have solved their car shortage by placing in service more cars of larger capacity and better design. Many coal mines in West Virginia should solve a part of their cost problems by the same simple procedure. Such a procedure requires an initial outlay of capital, but there is little doubt that this will be repaid, with a good return on the investment. Determining Number of Cars Needed There can be no mathematical rule to determine the number of cars which should be in use per loader in a coal mine, because numerous factors such as concentration of mining, system of haulage, car capacity, speed of haulage, distance of working places from tipple, and so forth, affect materially the number of cars in use. These factors in turn are more or less determined by height of bed, character of roof and coal,

Jan 1, 1931

By C. E. Jackson, E. C. Nelson, A. L. Christenson

Much information regarding the transfornlatio~lal characteristics of a steel as it cools in a known manner from the austenitic state can be obtained from dilatometric studies. This method has received more arid more attention because of its great flexibility, accuracy, and ease of interpretation. 'The method is entirely applicable to any rate of heating and cooling although the experumental procrdures for high rates of cooling have offered some difficulties. This paper presents a description of equipment employing cooling rates up to 500 °C. per secorld and the results of dilatometric observations on six commercial steels are included. French and Klopsch1 studied the cooling transformations of a serirs OF carbon steel, using the thermal arrest method. This was followed by the systematic investigatiol1 of Esser and co-workers on the effect of carhon2 and other alloying additions. in which the transforlnation temperature\ were determined by magnetic induction measurements indicated by a string galranoineter. Emphasis was placed on determining Ar' trailsformations and the critical cooling rates for these steels. The maglietic measurements wrere used in an effort to obtain more accurate data at higher cooling rates. Measurements of thermal arrest were made also to check the validity of the magnetic indications, and good correlation was found between the two, although Esser's,Ar' temperature measurements on iron-carbon alloys were about 200°F. lower than the measurements made by Fresnch and Klopsch. A notable contril~ution by Esser was the introduction gas quenching. wever and Rose4 used a moving-coil galranometcr in the study of the .Ar and Ar" of iron-carbon alloys by the thermal arrest method and obtained somewhat lover Ar" temperatures than those observed by Esser below I per cent carbon and considerably higher ahove. They concluded that the cooling rate had little influcncc on the Ar" temperatures above 0.4 per cent carbon, although Esser had observed a decrease in the -4r" temperature with increasing cooling rate with similar steels. Digges determined the .Ar" temperature4 for a scries of high-purity iron-carbon alloys, and close agreement with his results was obtained by Greninger. The thermal arrest method. together with metallographic observation used in both these studies, represents the latest investigations of this type. Any investigation by thermal analyses is dependent on the heat of reaction and the specific heat of the

Jan 1, 1945

By R. E. Reed-Hill, W. H. Hartt

The "(3034) " twin lamellae in magnesium have been reexamined using electron microscope replicas. The double twinning sequence (1011)- (1012) for these lamellae has been reconfirmed. Evidence is presented showing that the irrational habit of these twins is probably the direct result of a need to accommodate the second-order twinning shear. This accommodation vesults in both an external shear in the matrix and an internal shear in the lamella. A model is presented which accounts for the experimental obseruations. HCP metals are generally characterized by strong textures in which the basal planes of the grains tend to be aligned parallel to the rolling direction in sheet or plate and to the axis of wires and rods. Since these directions are normally those in which finished products may be subjected to uniaxial tensile stress, these textures effectively place the crystals of magnesium objects in orientations unfavorable to both basal slip and {1012) twinning, the easily activated deformation systems of this metal. However, when magnesium crystals are deformed near room temperature by a tensile stress nearly parallel to the basal plane, another mode of deformation can occur.',2 This is _a double twin which forms first by twinning on {loll), followed by retwinning on (1012). The resulting twin lamellae are of considerable interest. First, they can be responsible for "brittle fracture''; when a tensile stress axis lies in the basal plane, because the reoriented crystal structure of a lamella is well-aligned for slip while the parent crystal is not. Extensive internal deformation may thus occur while the matrix is still almost undeformed. This deformation can produce a ductile rupture running the length of the twin.3 Complete failure of the specimen may then oc-cure by the spreading of cracks from one twin lamella to another, or by the movement of a crack into a grain boundary and then along grain boundaries. Since the the volume fraction of these doubly twinned elements is normally very small, the fracture may be classed as brittle, although the fracture mechanism is, of itself, essentially ductile. It is quite probable that the ductility transition, normally observed4 in magnesium at or slightly Obove room temperature, is closely associated with these second-order twins. The detailed relationship of these twins to fracture in single crystals will be the topic of another paper. The present paper is concerned with a second important aspect: the irrational habit of these double twins that falls close to {3034), or approximately 7 deg away from the primary (10il) twin habit. There is good reason to believe that this habit results directly

Jan 1, 1968

By K. H. Hiller

A rotational viscometer has been designed which perrnits the measurement of the rheological properties of drilling muds and other non-Newtonian fluids under conditions equivalent to those in a deep borehole (350F, 10,000 psi). The important mechanical features of this instrument are described, and its design criteria are discussed. The flow equations for the novel configuration of the viscometer are derived and the calibration procedures are described. The data and their interpretation, resulting from measurement of the flow properties and static gel strengths of homoionic montmorillonite suspensiom at high temperatures and pressures, are presented. Data are also presented for the flow behavier of typical drilling fluids at high temperatures and pressures. The pressure losses in the drill pipe and the annulus depend critically upon the flow parameters of the drilling fluid. This work demonstrates the need to measure these parameters under bottom-hole conditions in order to obtain a reliable estimate of the pressure losses in the mud system. INTRODUCTION The rheological properties of drilling fluids are affected by temperature and pressure, but the extent of these effects on the dynamic flow properties is not well known. Measurements of changes of the flow properties of clay-water drilling muds with temperature have been reported by Srini-Vasan and Gatlin.1 The temperatures reported did not exceed 200F, a limitation imposed by the apparatus used by these authors. The rheological properties of clay suspensions were measured at temperatures up to 100C by Gurdzhinian.' Neither the nature of the exchange ions in the clay suspensions nor the degree of purity were defined in his work, nor were the measurements extended to currently used drilling fluids. The lack of systematic measurements of dynamic flow properties at high temperatures and pressures seems the more surprising since during the last decade the importance of the control of the hydraulic properties of drilling fluids has come to be widely recognized. Very good mathematical treatments of the friction losses in drill pipe and annulus have been developed.3 4 These treatments are based on the assumption that drilling fluids behave as Bingham plastic fluids. Quite often this assumption is justified, while in other cases a power law equation pro- duces better fit than the Bingham model does. For convenience in applying viscometer data to pressure-drop calculations, the Bingham plastic flow equation is preferable and, therefore, has been applied to the data reported in this paper, although other equations may fit these data more accurately. In a Bingham plastic fluid the relationship between the shearing stress 7 and the rate of shear D is given by the following equation: where is the plastic viscosity and 4 the yield point. If 4 = 0, the equation for simple Newtonian flow, 7 = pD, is obtained. Two empirical constants are required for the description of laminar flow of a Bingham plastic fluid, and calculations of the flow behavior at high temperatures and pressures cannot be better than is permitted by the accuracy with which these constants are known. For this reason a high-pressure, high-temperature rhe-ometer has been designed to measure the plastic viscosity the yield point +, and the static gel strength S, at pressures up to 10,000 psi and temperatures up to 350F. The important features of its design will be described. The results of measurements on homoionic clay slurries will be discussed insofar as they are relevant to an understanding of the general flow behavior of clay-water drilling fluids. The results of measurements on some typical drilling fluids will be presented also, and their practical implications will be briefly discussed. DESCRIPTION OF EQUIPMENT MECHANICAL FEATURES A viscometer designed to measure the plastic viscosity, yield point and gel strength of non-Newtonian fluids must permit the measurement of the shearing stress t at any given rate of shear D. This is possible only if t and D are approximately uniform throughout the entire sheared sample. A Couette apparatus is the most convenient method of realizing this condition, as has been pointed out by Grodde." The "high-pressure, high-temperature rheometer" described in this paper is basically a rotational Couette viscometer that is immersed in a cell in which pressure and temperature can be controlled over the range of interest. Fig. 1 shows schematically the important features of the pressure cell and associated equipment. The heart of the instrument is the rotating cup. It is shown more clearly in Fie. 2. which revresents the lower one-third of the pressure cell (below the input drive shaft shown in Fig. 1), and it is shown in detail in Fig. 3. For measurements of dynamic flow properties, the rotating cup is driven by a 1/2-hp electric motor, which operates through a Vickers

By John D. Verhoeven, Edward E. Hucke

An experimental technique has been developed for the measurement of the rate of electrotransport to a precision of 1 pct in the molten Bi-Sn system. Results are presented across the phase diagram from 30°C above the liquidus to 520°C. A phenomenological description is presented and the data on Bi-Sn are thereby converted to the effective charge, Analysis of the data indicates the true charge of the migrating tin species in bismuth to be +1.8 at 500°C. The data agree well with the recent work of Belashchmko. fieldintensity. The resistivity of the molten Bi-Sn system is also presented. WHEN an electric field is applied to a metal, a relatively large current is produced due to the ease with which electrons move within the metal. The electric field also produces a force on the ions which might cause them to migrate. Such a migration of metallic ions has been detected under certain conditions. This electromigration of the metallic ions will be referred to herein as electrotransport. The study of electrotransport in metallic systems has a rather long history dating back to the initial work of Gerardin1 in 1861. General reviews of electrotransport in liquid and solid metals have been published by Schwarz,2 Jost,3 Seith,4 and Heumann.5 In reviewing the literature it is apparent that the theoretical developments are not yet complete. The difficulty arises in describing the momentum transfer between the migrating ions and the electrons. In addition, there is a lack of good quantitative electrotransport data at high temperatures, especially in liquid metal systems. This work was undertaken to establish quantitative electrotransport data in a liquid metal system which might serve as a critical test of the theoretical developments. The Bi-Sn system was chosen for analysis, and the rate of electrotransport was determined as a function of temperature and composition. THEORETICAL CONSIDERATIONS If all of the atoms of a metal are considered to be positively charged due to the loss of electrons to the

Jan 1, 1963

By P. Chiotti, J. T. Mason

Ther?nal, X-ray, metallographic, and vapor pressure data were obtained to establish the phase diagram and standard free energy, enthalpy, and entropy of formation for the compounds in the Sw-Zn system. Four compounds, SmZn, SmZn2 , SmZn4.s, and SmZn8.5, melt congruently at 960°, 94Z°, 908°, and 940°C, respectively. The cornpounds SlnZns, Sm3Znll, and SnzZn7.3 undergo peritectic decomposition at 855", 870°, and 890C, respectively. Another compound of uncertain stoichiometry, SmZn11, undergoes peritectic decomposition at 760°C. Four entectics were observed with the following compositions in weight percent zinc and eutectic tenzperatures in degrees Centigrade: 12 pct, 680°C; 36 pct, 890°C; 58 pct, 850°C; and 72 pct, 900°C. An allotropic transformation and a composition range were observed for the SmZnz compound. The transfor)nation varies from 905" to 865°C as the zinc content increases from 16.0 to 48.5 wt pct, respectively. The free energy of formation of the compounds at 50PC varies between -15.9 kcal per mole for SmZn to -51.1 kcal per mole for SmZn,.,. Corresponding enthalpies vary between -19.2 to -78.3 kcal per mole. The ther-modynamic properties for the liquid alloys are described by the relations: A search of the literature revealed very little information on the Sm-Zn system. Chao et al.&apos; as well as Iandelli and palenzonai have reported the structure of SmZn to be cubic B2 type and Kuz&apos;ma et al3. have reported the structure of -sm2zn17 to be of the Th2Ni17 type. The purpose of this work was to establish the phase diagram of this system, to determine the zinc vapor pressure over the solid two-phase regions of the SYstem, and to calculate the thermodynamic properties of the compounds. MATERIALS AND EXPERIMENTAL PROCEDURES The metals used in this investigation were Bunker Hill slab zinc 99.99 wt pct pure and Ames Laboratory samarium. Analysis of the samarium by chemical, spectrographic, and vacuum-fusion methods gave the following average impurities in ppm: Nd, <200; Eu, <100; Gd, <100; Y, <50;Ca, 225; Ta, 400; Mg, 10; Cu, ~50; 0, 175; H, 20; and N, 15. The elements Fe, Si, Cr, Ni, Al, and W were not detected. The samarium was received as sponge metal and was kept under argon except when being cut with shears and when being weighed. Tantalum was found to be a suitable container for alloys with zinc contents up to the Sm2Znl, stoichio-metry. At higher zinc contents the grain boundaries of the tantalum containers were penetrated by the alloy and the containers failed during prolonged annealing. About 25 g of massive zinc and samarium sponge were sealed in tantalum crucibles equipped with thermocouple wells. These crucibles were in turn sealed in stainless-steel jackets. All closures were made by arc welding under an argon atmosphere. The samples were equilibrated in an oscillating furnace and in some cases were given various heat treatments in a soaking furnace. After appropriate heat treatment the steel jackets were removed and the alloy subjected to differential thermal analysis. The apparatus was calibrated against pure zinc and pure copper and found to reproduce the accepted melting points within 1°C. Alloys were subsequently subjected to metallographic examination and those of appropriate compositions were used for X-ray diffraction analysis and for zinc vapor pressure determinations. The vapor pressures were determined by the dewpoint method. Both the differential analysis and dewpoint measuring apparatuses have been described in earlier papers.4, 5 All alloy samples were etched with Nital (0.5 to 3 pct nitric acid in alcohol) except the samarium-rich alloys. These more reactive alloys were electro-polished in a 1 to 6 pct HClO4 in methanol solution at -700c at a potential of 50 v. EXPERIMENTAL RESULTS Phase Diagram. The results of thermal analysis are indicated by the points on the phase diagram, Fig. 1. Eight compounds and four eutectics were observed. The composition of the compounds and their melting or peritectic temperatures are given on the phase diagram. The four eutectic compositions in wt pct zinc and eutectic temperatures in % are: 12 pct,- 680°C; 36 pct, 890°C; 58 pct, 850°C; and 72 pct, 900°C. The stoichiometry of the most zinc-rich compound is still uncertain, but is very likely either SmZnll or SmZnlz. However, to simplify the presentation which follows it will be referred to as SmZnll. As shown on the phase diagram the phase regions for some of the samarium-rich alloys have not been unambiguously established. A sample of pure samarium was observed to transform at 924°C and to melt at 1074"C, in good agreement with corresponding val-

Jan 1, 1968

By Michael Hoch, Seong Kwan Rhee

The ternary system Zr-Cr-0 was investigated at 1200°, 1500°, and 1700°C. The isotherms at these temperatures were determined by metallographic and X-ray diffraction analysis of carefully selected alloys. AS a part of a series of investigations1-4 of the ternary and quaternary phase diagrams on refractory metals and their compounds, the ternary system Zr-Cr-O was investigated at 1200°, 1500°, and 1&apos;700°C. The binary diagrams Zr-Cr, Zr-O, and Cr-0 as reported by Hansen5 and Levin et a1.&apos; and the existence of a ternary coompound ZrsCrsO (q-carbide structure a. = 11.96A) provided a good base for this investigation of the Zr-Cr-O phase diagram. MATERIALS The materials used and their suppliers were: Zirconium powder, 99.4 pct pure, Charles Hardy, New York; Zirconium dioxide, Fairmount Chemical Co., Newark, N.J.; Chromium powder, 99.85 pct pure, Fairmount Chemical Co., Newark, N.J.; Chromium sesquioxide, 99.86 pct pure, J. T. Baker Chemical Co., Pillipsburg, N.J. Though the materials used were not "hyperpure", the impurities present do not affect the results (lattice parameters, phase boundaries) within the experimental accuracy. EQUIPMENT AND PROCEDURE The detailed procedures and equipment used for this investigation were similar to those described elsewherel&apos; "ith the exception that in this study an induction-heated argon-atmosphere furnace was used. The latter furnace was used to prevent the vaporization of chromium metal in samples in the higher temperature range (above 1200°C). The tungsten crucible was induct ion-heated in a vertical quartz tube filled with argon gas. The quartz tube was 1-1/2 in. in diameter and 10 in. long; it was connected at the top and bottom to water-cooled copper plates. The argon gas of a purity 99.995 pct was further purified by being passed through zirconium metal chips which were maintained at 800°C in a silica tube 1 in. in diameter and 30 in. in length. The furnace was flushed with argon gas for an hour before starting heating; during heating, a slight (3 cm oil) overpressure of argon was maintained in the system. Power was supplied by a 20-kw Ther-Monic Induction Generator. The samples rested on a tungsten-wire basket; the wire basket was connected to a tungsten wire which passed through the tungsten crucible lid, and entered the system on top through a Wilson-type seal. By pulling on the wire, the sample was removed from the crucible and dropped to the water-cooled copper base of the furnace. Because of the presence of argon gas, the cooling of the sample was even more rapid than in the vacuum furnace.&apos; EXPERIMENTAL RESULTS AND DISCUSSION 1) Isothermal Section at 1200°C. The compositions investigated have been numbered within the phase diagram, Fig. 1, and all the pertinent information about the samples can be found in Table I. This table lists the composition of the samples, the phases present in the room-temperature diffraction patterns, the phases detectable in the microstruc-ture, and calculated lattice parameters of the a-zirconium phase. The shapes of the various phase

Jan 1, 1964

By E. I. Larsen, E. F. Swazy, F. R. Hensel

Experience has indicated that hard bronzes are not suitable for bearing applications where high bearing loads and speeds are involved. It is the general practice to utilize softer materials for these purposes, such as copper, lead, silver, babbitt, lead-base alloys, and more recently aluminum-base alloys, preferably supported by a steel backing. It was the objective of the present investigation to study a new material produced by powder metallurgical methods susceptible to precipitation-hardening. Test MAteriaIs Preliminary tests were made with compacts containing copper, nickel and silicon in quantities sufficient to form 3 to 5 per cent nickel silicide. It mas found that this type of alloy was susceptible to the formation of a soft surface shell when sintered in tank hydrogen. The depth of the shell depended On the length of sintering time and sintering temperature, and varied in thickness from a few thousandths to as much as One eighth inch. This soft shell resulted from the preferential oxidation of silicon, thereby reducing the efficiency of age-hardening by the nickel silicide compound. The body of the sintered compacts below the soft shell could be precipitation-hardened to a hardness of 70 to 85 Rockwell B, by quenching from goo°C. and age-hardening at 450°C. A series of tests was made with various addition agents, in order to decrease the rate of preferential oxidation, and it was found that phosphorus was most beneficial in this respect. After considerable experimentation, the following nominal com-position was accepted as standard: 2.4 per cent nickel; 0.8 silicon; 0.3 phosphorus; balance copper. The physical propertties and certain bearing properties of this alloy are described in the present paper Preparation of Compacts Several methods of incorporating the hardening ingredient (nickel silicide) were studied. Compacts formed from copper, nickel and silicon powders were found to be inferior to those fabricated from prealloyed nickel silicide master alloys, because of the rapid oxidation of pure silicon during sintering. The use of a prealloyed nickel silicide hardener containing 25 per cent silicon and 75 per cent nickel could be further improved by preparing a master alloy, incorporating nickel, silicon, phosphorus and copper, having the following nominal composition~ 25 per cent nickel; 7 silicon; 3 phosphorus 64 copper. This alloy is brittle in the cast condition and can be readily powdered. Sintering Procedure The blended powders were pressed at &apos;5 to 40 tons per sq&apos; in., the pressure depending on the size and shape of the compacts. Sintering was carried out in hydrogen or cracked ammonia atmospheres at

Jan 1, 1946

By E. I. Larsen, E. F. Swazy, F. R. Hensel

Experience has indicated that hard bronzes are not suitable for bearing applications where high bearing loads and speeds are involved. It is the general practice to utilize softer materials for these purposes, such as copper, lead, silver, babbitt, lead-base alloys, and more recently aluminum-base alloys, preferably supported by a steel backing. It was the objective of the present investigation to study a new material produced by powder metallurgical methods susceptible to precipitation-hardening. Test MAteriaIs Preliminary tests were made with compacts containing copper, nickel and silicon in quantities sufficient to form 3 to 5 per cent nickel silicide. It mas found that this type of alloy was susceptible to the formation of a soft surface shell when sintered in tank hydrogen. The depth of the shell depended On the length of sintering time and sintering temperature, and varied in thickness from a few thousandths to as much as One eighth inch. This soft shell resulted from the preferential oxidation of silicon, thereby reducing the efficiency of age-hardening by the nickel silicide compound. The body of the sintered compacts below the soft shell could be precipitation-hardened to a hardness of 70 to 85 Rockwell B, by quenching from goo°C. and age-hardening at 450°C. A series of tests was made with various addition agents, in order to decrease the rate of preferential oxidation, and it was found that phosphorus was most beneficial in this respect. After considerable experimentation, the following nominal com-position was accepted as standard: 2.4 per cent nickel; 0.8 silicon; 0.3 phosphorus; balance copper. The physical propertties and certain bearing properties of this alloy are described in the present paper Preparation of Compacts Several methods of incorporating the hardening ingredient (nickel silicide) were studied. Compacts formed from copper, nickel and silicon powders were found to be inferior to those fabricated from prealloyed nickel silicide master alloys, because of the rapid oxidation of pure silicon during sintering. The use of a prealloyed nickel silicide hardener containing 25 per cent silicon and 75 per cent nickel could be further improved by preparing a master alloy, incorporating nickel, silicon, phosphorus and copper, having the following nominal composition~ 25 per cent nickel; 7 silicon; 3 phosphorus 64 copper. This alloy is brittle in the cast condition and can be readily powdered. Sintering Procedure The blended powders were pressed at &apos;5 to 40 tons per sq&apos; in., the pressure depending on the size and shape of the compacts. Sintering was carried out in hydrogen or cracked ammonia atmospheres at

Jan 1, 1946