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By Harold B. Goldman, Don Reining

The sand and gravel industry is the largest nonfuel mineral industry in the nation (Drake, 1972), Table 1. In 1970, the production of sand and gravel totaled 944 million tons valued at $1.1 billion. California, which leads the nation with more than 140 million tons, together with Michigan, Ohio, Minnesota, Illinois, Wisconsin, and New York, account for 43 % of the total production in the nation. In commercial usage, "sand" applies to rock or mineral fragments ranging in size from particles retained on a No. 200 sieve (0.074 mm openings) to those passing a No, 4 sieve (4.76 mm openings). "Gravel" consists of rock or mineral fragments larger than 4.76 mm, ranging up to 3%-in. maximum size. The construction industry consumes 96% of the sand and gravel produced; the remainder is sand used for specialized products such as glass (see the chapter on "Silica and Silicon"). Utilization The building industry uses sand and gravel chiefly as aggregate in portland cement concrete, mortar, and plaster; the paving industry uses sand and gravel in both asphaltic mixtures and portland cement concrete. Aggregate is commonly designated as the inert fragmental material which is bound into a conglomerate mass by a cementing material such as portland cement, asphalt, or gypsum plaster.

Jan 1, 1975

By E. Goldin, H. J. Juretschke

THE electrical properties of porous conductors have been studied ever since such materials, usually prepared by pressing and sintering of metallic powders, obtained practical importance. In most cases, however, the results have not been easy to interpret because of the great number of independent variables such as powder size, pressure, pressing rate and temperature, subsequent thermal history, porosity, and so on, which enter into the fabrication of industrially desirable materials. In recent years an interpretation of these properties has become of interest because the electrical properties of many new substances, prepared as fine powders by crystallization from the vapor phase or by reactions in the solid state at high temperatures, have to be determined on porous samples formed from the powder. Since theoretically significant information must refer to the fully dense state of the material, it is important to relate the electrical properties measured on such porous samples to those expected for a sample of 100 per cent density. A simple theory for the porosity dependence of the electrical conductivity and the Hall effect was recently proposed by Juretschke, Landauer, and Swanson.' Their model, assuming a distribution of pores of equal size and shape, sufficiently far apart so that each pore is embedded in a region of uni-

Jan 1, 1959

By H. T. Bowman

For more than 80 years the Bessemer process has depended upon the ability, skill, and judgment of the blower, although as early as the I860's it was recognized that the process would benefit by some type of instrumental contro1.l IIowever, instruments with sufficient recording speeds did not exist, so the end-point determination was always dependent upon the blower's eye. This placed an obstacle in the way of precise experimental work, because of the absence of the necessary records and reference points as reported by Work.2 The use of the photocell provided the instantaneous record of the blow that made this experimental work possible and provided more scientific control for the process as discussed by Graham,3 A brief description of the progress of the blow will illustrate the recording function of the instrument. The silicon in the iron is being oxidized during the first minutes of the blow, as pointed out by Henning4 in a table showing the order of metalloid elimination. The product of this oxidation is a solid that remains in the converter, so there is virtually no flame during this part of the blow. This low flame luminosity is illustrated by the flame recording shown in Fig. I, where the silicon blow is plainly marked. The dull flame of the silicon blow gradually gives way to the brilliant carbon flame as the increasing quantities of carbon monoxide formed inside the converter burn to dioxide upon contact with the atmosphere above the vessel. When the carbon reaches some low value under 0.20 per cent, there is insufficient menoxide formed to maintain the dioxide flame, so its intensity drops. Throughout the flame drop carbon continues to burn, until at some value around 0.05 per cent an arrest occurs in the recorded drop. This point has been designated as the end point. The period of time from this end point until the vessel is turned upon its side and blowing has stopped has been called the afterblow. This afterblow is used as a measure of the degree of metal oxidation, and uniformity demands that it be controlled within narrow limits. Iron and blowing conditions are likely to change several times during a turn, necessitating corresponding changes in end-point control. It is the purpose of this paper to discuss these changes, the factors that make them necessary, and their bearing upon the quality of steel. Carbon-FeO Relationship In the Bessemer process oxidation relationships are precise. Fig. 2 shows a graph of the carbon-FeO relationship. The familiar "bomb-test" method, described by Mccutcheon and Rautio,5 was used for obtaining these and all other dissolved FeO values herein reported, all tests being taken from the converter before deoxidation unless otherwise noted. All tests of 0.10 per. cent carbon and above were obtained from metal blown for duplexing. McGinley and Woodworth6 reported iron oxide values for blown metal, but their tests were obtained by a . different method than were those

Jan 1, 1942

By H. T. Bowman

For more than 80 years the Bessemer process has depended upon the ability, skill, and judgment of the blower, although as early as the I860's it was recognized that the process would benefit by some type of instrumental contro1.l IIowever, instruments with sufficient recording speeds did not exist, so the end-point determination was always dependent upon the blower's eye. This placed an obstacle in the way of precise experimental work, because of the absence of the necessary records and reference points as reported by Work.2 The use of the photocell provided the instantaneous record of the blow that made this experimental work possible and provided more scientific control for the process as discussed by Graham,3 A brief description of the progress of the blow will illustrate the recording function of the instrument. The silicon in the iron is being oxidized during the first minutes of the blow, as pointed out by Henning4 in a table showing the order of metalloid elimination. The product of this oxidation is a solid that remains in the converter, so there is virtually no flame during this part of the blow. This low flame luminosity is illustrated by the flame recording shown in Fig. I, where the silicon blow is plainly marked. The dull flame of the silicon blow gradually gives way to the brilliant carbon flame as the increasing quantities of carbon monoxide formed inside the converter burn to dioxide upon contact with the atmosphere above the vessel. When the carbon reaches some low value under 0.20 per cent, there is insufficient menoxide formed to maintain the dioxide flame, so its intensity drops. Throughout the flame drop carbon continues to burn, until at some value around 0.05 per cent an arrest occurs in the recorded drop. This point has been designated as the end point. The period of time from this end point until the vessel is turned upon its side and blowing has stopped has been called the afterblow. This afterblow is used as a measure of the degree of metal oxidation, and uniformity demands that it be controlled within narrow limits. Iron and blowing conditions are likely to change several times during a turn, necessitating corresponding changes in end-point control. It is the purpose of this paper to discuss these changes, the factors that make them necessary, and their bearing upon the quality of steel. Carbon-FeO Relationship In the Bessemer process oxidation relationships are precise. Fig. 2 shows a graph of the carbon-FeO relationship. The familiar "bomb-test" method, described by Mccutcheon and Rautio,5 was used for obtaining these and all other dissolved FeO values herein reported, all tests being taken from the converter before deoxidation unless otherwise noted. All tests of 0.10 per. cent carbon and above were obtained from metal blown for duplexing. McGinley and Woodworth6 reported iron oxide values for blown metal, but their tests were obtained by a . different method than were those

Jan 1, 1942

ALTHOUGH the refining period of the heat is generally defined as A starting after the charge has been completely melted, it may more properly be considered as beginning with the first efforts to facilitate the shaping up of the slag and the making of corrective additions for the control of slag or metal composition. Such actions may be initiated during the latter half of the lime boil. The early part of the refining period may, then, in essence overlap the latter part of the melting period. The primary aims of the refining period are to reduce phosphorus and sulphur from the steel bath to levels safely below the maximum contents specified, to eliminate carbon as rapidly as possible and still allow time for proper conditioning of the slag and attainment of the necessary bath temperature, and to deliver the heat ready for tapping or furnace deoxidation, with slag in the proper physical and chemical condition, and with carbon and oxygen contents and the temperature of the steer bath at the proper levels for the composition and grade of steel being produced. The particular conditions that fulfil these aims are distinctly different, depending upon whether the steel is to be finished according to fully-killed, semikilled, or rimming practice and also depending upon the carbon range specified. Regard- less of the type of charging practice employed, the object of the refining period is to produce repeatedly the desired finishing and tapping conditions for the grade of steel being produced. The variations and proportions of raw materials used in the charge may cause some variations in the degree of control required during refining, but not in the method of control. The refining period can therefore be discussed from a viewpoint largely independent of charging and melting practice. SHAPING UP THE SLAG In the first helper's vocabulary, refining practice consists in "shaping up" his heat. This includes elimination of sulphur, phosphorus, and carbon, putting the slag in proper condition, and adjusting bath temperature. Shaping up the slag is a major consideration because

Jan 1, 1944

By W. F. Chiao

Ultrasonic attenuation, a, measurements in the frequency range of 5 to 55 mc per sec have been studied to determine their quantitative relationship with the following three variables of mixed microstructures in steels: 1) the volume percent, XF, of polygonal fer-rite in mixed structures of martensite and polygonal ferrite in Fe-Mo-B alloys: 2) volume percent, XA, of retained austenite plus martensite aggregates in high-carbon steel; and 3) substructural differences between 100 pct bainitic ferrite structures formed at various temperatures. The quantitative relationship obtained in the first two conditions by plotting a us the known structural parameters can be expressed, respectively, as: where al, a 2 and C1, Cz are constants. In the third condition the nature of the attenuation depends on the state of dislocations generated at the transformation temperatures and also on the alloy composition. From these measured results, the mechanism of ultrasonic attenuation caused by these mixed microstructures can also be studied. MUCH interest has recently been shown in the application of ultrasonic attenuation and wave velocity measurements to the study of the microstructural characteristics of steels. The general aims of most of the investigations in this field can be grouped into two categories: one is to study the mechanisms of ultrasonic losses caused by the characteristic phases in the microstructure of steel,''' and the other is to develop nondestructive test methods and applications for quality control.~' 4 Apparently no work has been done on the evaluation of ultrasonic attenuation meas -urements as a means of quantitative determination of a given phase in the microstructure of a steel. It is well-established that the decomposition of austenite results in four main microstructural constituents—polygonal ferrite, pearlite, bainite, and martensite—and that each phase has different mechanical properties. Thus, when a steel consists of mixed microstructures, the mechanical properties can often be related to a quantitative measure of the volume percent of each phase present. This study relates ultrasonic attenuation measurements to: 1) the volume percent of polygonal ferrite in mixtures of martensite and polygonal ferrite in Fe-Mo-B alloys; 2) the substructural differences between 100 pct bainitic ferrite structures formed at various temperatures; and 3) the vol- ume percent of austenite in austenite plus martensite aggregates in a high-carbon steel. The choice of the specimen materials was based on the laboratory stocks which were suitable to produce the required mixed microstructures for this study. EXPERIMENTAL PROCEDURES Materials and Heat Treatment. Polygonal Ferrite Plus Martensite Structures. This mixture of phases was produced in a vacuum-melted Fe-Mo-B alloy. The alloy was hammer-forged at 1900" ~ to a -f-in.-sq bar. By isothermally heat treating the alloy at 1300° F for various times and then water quenching, variations in the amount of polygonal (or proeutectoid) ferrite can be controlled in a microstructure in which the balance of the material is martensite. In the present work, four different times of isothermal transformation were adopted; after heat treatment, the four specimens were machined for ultrasonic measurements. The compositions, heat treatments, and dimensions of the four specimens are listed in Table I. 100 pct Bainite Structures Formed at Different Temperatures. It has been well-established by Irvine et al.= that the presence of molybdenum and boron in ferrous alloys can retard the formation of polygonal proeutectoid ferrite and expose the bainitic transformation bay, so that a more acicular or bainitic ferrite can be obtained over a wide range of cooling rates. Their investigation6 also showed that the mechanical properties of fully bainitic steels are usually closely dependent on the substructural characteristics of the steels. For studying the substructural characteristics in completely bainitic structures, six Fe-Ni-Mo alloys, of which five were free from carbon addition and one with 0.055 pct C addition, were selected so that a wide range of hardness values for 100 pct bainitic ferrite structures could be produced by normalizing at 1900" F followed by air cooling. The different bainitic transformation temperatures were recorded during air cooling. All of the alloys were vacuum-melted and then forged at 1900" F to square bars. Data on the six specimens of these structure series are summarized in Table 11. Austenite Plus Martensite Structures. The high-carbon steel used to study austenite plus martensite structures was vacuum-melted and then forged into Q-in.-sq bar. The series of mixed structures of austenite plus martensite was produced by quenching the specimens from the austenitizing temperature to room temperature and then refrigerating them at various temperatures within the range of martensite transformation to produce different amounts of retained austenite. Data on the four specimens of this series are listed in Table 111. Quantitative Analysis of the Microstructures. The microstructures containing martensite plus polygonal ferrite were analyzed by the point-counting technique.

Jan 1, 1969

By Forrest F. Craig

Both early and more recent1 laboratory measurements of gas-oil relative permeabilities were made by subjecting oil-saturated cores to external gas drives. In these runs it was generally assumed that the flowing gas/oil ratio was constant at every point throughout the core. Using this assumption, the resulting equation for the gas-oil relative permeability ratio becomes A where Q is the flow rate at the producing end of the system. This relative permeability was then specified for the average saturation of the core. The assumption and resulting equation fail to recognize that in an external drive, the oil flow rate varies from zero at the injection end to a maximum at the producing end. The assumption also fails to consider the existence of a saturation gradient during an external drive. This saturation gradient is due solely to non-steady-state flow. Some authors2,3,4 have used this erroneous method of calculating relative permeability ratios from external drives. Other authors5,6,7 have used relative permeability ratios in calculating expected field performance by external drive, using Equation (1) and making the incorrect assumption that the saturation is uniform within the driven portion of the reservoir. To find the correct relation between the relative permeability. ratio at the average saturation and the produced gas/oil ratio, the insertion in Equation (1) of a factor, F, to adjust it for oil velocity gradient has been considered. The equation then takes the form Assuming that the oil velocity is directly proportional to the distance from the injection point leads to the conclusion that, for a linear system, the average oil velocity is one-half that at the producing end. Thus, the average gas/oil ratio is twice the produced gas/oil ratio, and Equation (2) is transformed into However, here again the existence of a saturation gradient is not recognized. The produced gas/oil ratio is related to the relative permeability ratio at the saturation of the outlet end of the system. It can be shown quite readily that, if the true log k,/k, saturation relationship is linear over small ranges of saturation, then d log kjko Where aaxv and u2 are the average and outlet saturations, respectively. Examination of Equation (3) shows that the factor F cannot have a single value over the whole saturation range. Another method of dealing with external drives is that of Buckley and Leverett.' Their method, which assumes no gas expansion and outlet end effects, considers fully the saturation gradient present due solely to the displacement mechanism during an external drive, and applies Equation (1) to each point along this gradient. The calculation of production history using relative permeability ratio is straightforward. However, the calculation of relative permeability ratios from production history by this method is impractical. In a recent paper, Welge,1 using an approach similar to that of Buckley and Leverett, presents a simplified method for determining the saturation at the producing end of the system. At thi; saturation, the relative permeability ratio calculated by Equation (1) applies exactly, after breakthrough of the stabilizej front. By this method, relative permeability ratios or production history may be calculated with equal ease. Use of this method as a laboratory tool in determination of relative permeability ratios by external drive requires the knowledge of the total injected fluid volume; in addition to the average saturation and producing ratio. As a preliminary test of this method of calculation, laborntory external gas drives were run on a 3% in. diameter, 11 in. long sample of Nellie Bly consolidated sandstone. This core sample had a permeability of 824 md and a porosity of 28.1 per cent. The driving fluid was air. Three different oils were used, having viscosities of 1.4, 9.8, and 125 cp, respectively. The runs were made under identical pressure differentials,

Jan 1, 1952

By AIME AIME

OUR new Director from the 15th District is Robert W. Thomas; of Ray, Ariz., general manager of the Ray Mines division, Kennecott Copper Corp. In electing him to this office his fellow engineers pay tribute to his ability as an engineer and express appreciation for his service to the A.I.M.E. and its Arizona Section. ?Bob? Thomas was born April 1, 1886 at St. James Minn. received his early education in the public schools of Topeka Kans. and was graduted from Topeka High School in 1905. Already he had decided upon mining engineering as a profession. so he entered the mining school of the University of Kanas from which he was graduated with the degree of B.S. in hlining enginrering. While in college he became a Student Associate of the A.I.M.E. After graduation, lution and isolated mining camps wel-e not the most desirable places in w

Jan 1, 1944

By J. S. Vanick

An extremely hard, tough, and strong, white or chilled cast iron has been applied for the past several years to industrial and mining services in which its unusual properties have been confirmed by its ability to deliver in many instances much better performance than plain chilled iron, or other wear-resistant materials. It is being produced regularly by alloying a good base composition of chilled or white cast iron with essentially 4 to 6 per cent of nickel and 1 to 2.5 per cent of chromium. Such a material can attain a hardness exceeding 600 to 750 Brinell as against 380 to 530 for corresponding grades of plain chilled iron. The strength is approximately doubled and the toughness significantly increased. These properties make it especially useful for many applications requiring a high hardness for resistance to wear, abrasion, attrition, deformation; to some extent to high compressive loading and to a lesser but important degree to corrosive action. A wide variety of commercial castings is being successfully produced from this iron, ranging in size from the small grain-grinding plates or burrs through medium-sized castings such as sand pumps up to large, heavy castings such as rolls for metal rolling or cement grinding. The composition of this white cast iron may be roughly bracketed within the range shown in Table 1.

Jan 1, 1933

By A. F. van Everdingen

The pressure drop in a well per unit rate of flow is conrolled by the resistance of the formation, the viscosity of the fluid. and the additional resistance concentrated around the well bore resulting from the drilling and completion technique employed and, perhaps, from the production practices used. The pressure drop caused by this additional resistance is defined in this paper as the skin effect. denoted by the symbol S. This skin effect considerably detracts from a well's capacity to produce. Methods are given to determine quantitatively (a) the value of S, (b) the final build-up pressure, and (c) the product of average permeability times the thickness of the producing formation. INTRODUCTION Equations which relate the pressure in a well producing from a homogeneous formation with pressures existing at various distances around the well are generally used within the industry. The relation ii quite simple when the fluid flowing is assumed to be incompressible. It becomes somewhat more complicated when the flowing fluid is considered compressible so that the duration of the flow can he considered. In each case the major portion of the pressure drop occurs close to the well bore. However analyses of pressure build-up curves indicate that the pressure drop in the vicinity of the well bore is greater than that computed from these equations using the known, physical characteristics of the formation and the fluids. In order to explain there excessive drops it is necessary to assume that permeability of the formation at and near the well bore is substantially reduced as a result of drilling. completion and, perhaps. production practice. This possibility has been recognized in the literature. A method to compute the pressure drop due to a reduction of the permeability of the formation near the well bore. which is designated as the skin effect. S, is given in the following paragraphs. To start, equations normally used to describe flow in the vicinity of a well are given without considering this effect. These equations then are modified to include the effect of a skin on the pressure behavior. Finally a method is given to estimate the effect of the skin on the pressure and production behavior of a well. PRESSURE EQUATIONS Incompressible Fluid Flow If p is defined as the flowing pressure in a well of radius the pressure at distance r from the well has been shown to be:" The total pressure drop between the drainage boundary, and the well bore is given by These equations are valid only if the flow towards the well occurs in a horizontal homogeneous medium and the fluids are incompressible. The assumptions imply that all fluid taken from the well enters the system at r a condition rarely encountered in practice. Compressible Fluid Flow, Steady State A more realistic equation is obtained if it is assumed that the compressibility, c, of the flowing fluids is small and has a constant value over the pressure range encountered. After the well has been producing for some time so that its rate has become constant and steady state is reached, the pressures throughout the drainage area are falling by the same amount per unit of time, and the pressure differences between a point in the drainage area and the well are constant. When these conditions are met. the rate of production, q, from a well is equal to where dp/dt is the pressure drop per unit time. The fluid flowing at a distance from the center of the well is equal to From the last equation and from Darcy's law it can be shown that The equation holds for a depletion-type reservoir of radius drained by a well located in its center, provided the compressibility of the fluid per unit pressure drop is small and constant, and no fluid moves across the boundary Compressible Fluid Flow — Nonsteady State Table 111 of reference (5) shows the relationship between the pressure at the well bore and the reduced time, The pressure-drop function, p represents the drop below the original reservoir pressure, p caused by unit rate of production for several values of R, the ratio of drainage boundary radius to well radius, r In most reservoirs the values of approach infinity. and under these conditions the values of p shown in Table I of reference (5) can be used where p then signifies the difference between the pressure in the well and the prevailing reservoir pressure per unit rate of flow. The total pressure drop below prevailing reservoir pressure amounts to where the factor converts the cumulative pressure drop per unit rate of production to cumulative pressure drop for actual rate. q. For values of T > 100 the P function may be written (equation VI-15 of reference 5) as Using the time conversion the difference in pressure between reservoir and well becomes If values for the physical constants of the formation and the fluids are inserted, it is found that T exceeds 100 after a few seconds of production (or closed-in time), so that the approximation becomes valid almost at once. A simple relation between the pressure in the well and in the reservoir can also be derived by considering the well as a point source"" '" instead of a unit circle source, that is, by using Lord Kelvin's solution instead of the unit circle source

Jan 1, 1953

By R. H. Frazier, C. H. Lorig, F. W. Boulger

THERE are both advantages and disadvantages in using semikilled steels in place of killed steels. One advantage of semikilled steels is they provide a higher ingot-to-product yield. This is especially important to shipbuilders in the time of national emergency. By using semikilled steel for hull plates, a greater number of ships can be built from the same ingot tonnage. Consequently, if semikilled steel plates are adequate for the service, the advantage of the higher product yield is of considerable importance. The performance of hull plates is closely associated with the ductile-to-brittle transition temperature, and this, in turn, is strongly dependent on the composition of the steel. A low transition temperature is desirable because it indicates that the steel is less likely to fail at low ambient temperatures. Killed steels are known to have lower transition temperatures than semikilled steels. It is believed that the better qualities of killed steels in this respect are due mainly to the low oxygen contents of the steel. The principal deoxidizers, aluminum, silicon, and manganese, lower the oxygen content. Fundamental studies1-0 have shown that the oxygen content remaining after the addition of one of these three elements is influenced by the residual amounts of the other two present. In the current study, therefore, various amounts of silicon and aluminum were added to steels containing different manganese contents for the purpose of studying the influence of silicon and aluminum on the notched-bar properties of hot-rolled steels. Eleven types of steels were studied. The temperature at which the plates were finish-rolled was care- fully controlled at 1850°F. All plates were rolled to ¾-in. thickness, and tested in the as-rolled condition. The total number of steels prepared in the laboratory for this study was 95. The charge consisting of ingot iron and ferrosilicon equivalent to 0.10 pct Si was melted in a 200-lb induction furnace under an atmosphere of argon to insure low, uniform nitrogen contents. After the charge was melted and the desired temperature was obtained, the melt was partly deoxidized with either silicomanganese or aluminum. Aluminum was used for this purpose in only those steels with very low silicon contents, where the finished steel was to contain some aluminum. This initial deoxidizing addition was made to obtain consistent recoveries of subsequent additions of ferro-manganese, ferrosilicon, and aluminum. Carbon, in the form of graphite, was added, either just prior to tap or to the final aluminum addition. The entire heat of 200 lb was poured directly into a 6x6-in. big-end-up mold. The ingots of semikilled steel were capped with a steel plate. The killed steels, on the other hand, were poured with a hot-top containing 14 pct of the total volume of the ingot. The ingots were processed by heating to 2250°F, followed by forging to slabs 1¾ in. thick and 6 in. wide. After reheating to 2250°F, the slabs were rolled to 0.9-in. gage, using reductions of approximately 1/6 in. per pass. The 0.9-in. thick plates were immediately recharged in a furnace held at 1850°F. After 30 min in the furnace at 1850°F, the plates were rolled to ¾ in. in one pass. Following the final pass, the plates were stacked on edge on a brick floor, with a brick separating one from another, where they were allowed to cool in air. Drillings for chemical analysis were taken from the plates at locations corresponding to the top and bottom of each ingot. Carbon, manganese, silicon, phosphorus, sulfur, and nitrogen contents of each sample were determined. The analysis of each steel was carefully controlled so that the contents of

Jan 1, 1957

By C. F. Floe, N. J. Grant, A. Joukainen

A CCORDING to Guertler,¹ Smith and Hamilton were the first to study the Cu-Ti alloy system, but because of the presence of large amounts of impurities their data are inconclusive. Hensel and Larsen² in 1930 and Kroll³ in 1931 determined the high copper end of the diagram. In 1939 Laves and Wallbaum,4 in a short summary of compound determinations in titanium binary alloys, mentioned the existence of a face-centered cubic compound, Ti2Cu, with 96 atoms per unit cell, and also a compound, TiCu3, which was said to have a deformed hexagonal close-packed structure in which ordering had been observed. The existence of a compound, TiCu, was also found but the crystal structure was not determined. Craighead, Simmons, and Eastwood determined the effect of copper on the allotropic transformation in titanium. The investigation was limited to alloys containing from 0 to 5 pct Cu, using titanium of fairly high impurity content. Experimental Procedure The methods used for determination of the diagram included metallographic examination and X-ray and thermal analyses. The system was first worked out using the higher purity "Process A" sponge titanium and oxygen-free copper. The high titanium region was next determined more accurately using iodide titanium and vacuum-melted, oxygen-free copper. Preparation of Alloys: The alloys were prepared by arc melting under prepurified helium atmos- pheres in water-cooled copper crucibles. The high purity iodide titanium alloys were prepared by melting three compositions along with a specimen of unalloyed titanium in a single charge. A multiple crucible was used which consisted of a copper plate with four cup-like depressions. The unalloyed titanium was melted first and acted as a getter for any oxygen and nitrogen in the melting chamber. Since these elements harden titanium, the hardness of the standard specimen was an index of the highest probable contamination of the alloy melts. The sponge titanium alloy melts weighed from 100 to 200 g each and the iodide titanium melts from 20 to 25 g. In order to insure greater homogeneity most of the alloys were melted, turned, and remelted twice. The larger buttons made from sponge titanium were sectioned or crushed before remelting. These alloys up to 30 pct Cu were further homogenized by forging at 925°C. They forged readily up to 20 pct Cu but numerous cracks were formed in the alloys containing from 20 to 30 pct. Above 30 pct Cu the sponge titanium alloys were homogenized by heating for 200 hr at 850°C under prepurified helium. Similarly, the iodide-grade titanium alloys containing up to 3 pct Cu were homogenized at 1000°C for 24 hr and all others at 880°C for 200 hr.

Jan 1, 1953

By AIME AIME

IT IS not necessary to travel hundreds of miles from New York City to see examples of modern mining methods applied in tunnel work. In the various subway jobs, for instance, underground work is done on so large a scale as to justify the oft-quoted remark that here is the world's greatest mining camp. In such cases, however, the size of the excavation makes wholly disproportionate comparison with the haulage drift or adit level of the West. But in West Orange, N. J., Antonio -DiMarco is driving a tunnel from two headings on opposite sides of First Mountain, under contract with the town of West Orange, which is similar in nearly every respect to the type of work that must be done at the mines, and merits description as an example of fast and economical tunnel driving under conditions commonly met with by the mining engineer in more inaccessible parts.

Jan 1, 1931

By H. I. Najarian

This paper is a companion piece to the description of the electrothermic process that begins on page 141. It will be confined to a brief story of the development. of the Weaton-Najarian vacuum condenserf at this plant, together with up-to-date design and operating data. The Josephtown smelter was designed primarily for production of zinc oxide. However, the development of a method for production of zinc metal had always been under consideration, and accordingly one of the original eight units of the elcctro-thermic furnaces built in 1930 was set up to produce metal. The design of this furnace was identical with that of the oxide furnaces except that in place of oxide tewels opening into oxide manifolds, conventional conical clay condensers—similar to condensers used in horizontal retort smelting—were installed around the periphery of the furnace and in several tiers vertically for condensing the zinc vapors. The early experimental work in trying to condense zinc out of the mixtures of zinc vapor and carbon monoxide gas from the electrothermic furnaces indicated that, while the gases from electrothermic smelting would condense in surface-type condensers, the formation of blue powder was excessive and condenser efficiency low. Furthermore, operating a large unit of electric furnace with several hundred small condensers, with attendant high labor cost and unfavorable operating conditions, did not appeal to us. We also realized that a single unit of surface condenser capable of condensing 12 torg tons of metal per day would be of huge dimensions and possibly difficult of control. So we took as our aim the development of a method whereby a single condenser unit of reasonable dimensions would condense zinc, in one step, from the large volume of gases that the electric furnaces produced. We set about searching for knowledge on zinc metallurgy and design of zinc condensers in particular. Our study of the prior art focused our attention on the oft-repeated statement by earlier experimenters, that the most efficient way to condense metallic vapors, such as zinc vapors, was to bring the vapors into "intimate contact" with molten metal; but the methods offered for securing this "intimate contact" in any practical manner left much to the imagination. We were handicapped by not having some-one on the Josephtown smelter staff who could lay claim to being an expert zinc metallurgist and could give guidance from actual experience on the practicability of various schemes that haunted our imagination. Laboratory Experiments However, we had an expert ex-steam engineer in the person of George I?. Weaton, manager of the Josephtown smelter, who had had long experience with steam-jet condensers and would reiterate his belief at every opportunity that the logical and the most efficient way to condense zinc would be with a jet-type condenser. We became intrigued by the possibilities of a zinc con-

Jan 1, 1944

By Lyall Zickrick

Experiments of previous investigations have indicated that calcium-copper alloy, when used as a deoxidizer for molten copper, results in a sound copper casting of good physical and electrical properties. Braden-berg and Wiensl have obtained successful results in casting sound copper using calcium for deoxidizing. Masing2 has obtained deoxidized copper of high density and high conductivity by use of calcium. Pratt,3 in 1907, patented the use of calcium for the deoxidation and degasification of copper. Schumacher, Ellis and Eckel,l in 1929, conducted a series of experiments on deoxidizing copper with calcium. They concluded that so long as there is only a small percentage of residual calcium the mechanical and electrical properties of the copper deoxidized are not impaired, and the deoxidation is thorough. For this investigation, a copper-calcium alloy high in calcium and 10 variously deoxidized copper ingots were prepared. The investigation concerns itself with the casting properties and structure of these variously deoxidized ingots, their working and annealing characteristics, and the resulting physical and electrical properties of the worked materials. Preparation of Special Copper-calcium Alloy and Experimental Ingots For use as a deoxidizing agent, an alloy of copper and calcium with fairly high calcium content was prepared, by melting pure electrolytic copper in a graphite crucible in an ordinary gas-fired pot furnace. The molten copper was kept well covered with calcium chloride slag. Small chunks of calcium were wrapped in thin copper sheet, placed on the end of a graphite rod and plunged down into the molten copper and thoroughly stirred. Upon completion of the calcium additions the crucible content was poured out into a cake about one inch thick. Analysis of this alloy gave 4.4 per cent calcium. The alloy was brittle and easily broken into small chunks. Some calcium was lost during the addition, owing to

Jan 1, 1933

By P. L. Rittenhouse, M. L. Picklesimer

A rapid and seniquantitative method of determining prefered orientation on large numbers of. Zircaloy-2 specimens was desired. knoop microhardness measurerrzetzls were irvestigated as a solldtion to this pro6lem. The variation of Knoop microhardness measurerlerzts on selected planes as a function of 'irzdenle axis relutilje lo cryslallograplzic or fabrication divectals were used to corzstrrcl a polar coordinate hardness contour map. With use of an empirical relationslip between the single-crystal hardnesses and those of the polycrystalline material conentional pole figures could be constructed which compare favorably also obtained. To determine preferred oriention qualitatively from hardness data requires a minimum of twelve measurements per plane on three, preferattention to grain size, specimen prepartion, and in-rreinetzt, and analjlsis is of the order of- 45 to 60 rrin. THE design of structures from Zr alloys requires consideration of preferred orientation and the resulting anisotropy of mechanical properties. Rapid and semi-quantitative methods of evaluating anisotropy and of determining preferred orientation are needed for quality control and for examining the large number of test specimens required in development programs. The variation of Knoop microhardness with indenter orientation has been studied in single crystals of several hcp metals including titanium.' beryllium,' magneium, and zinc.4 The maximum hardness observed on any crystallographic plane other than the basal plane invariably occurred when the long axis of the Knoop indenter was either parallel or perpendicular to the projection of the [ OOOI.] direction on the plane of examination. When the major slip mode was (0001)(i2i0j the maximum hardness occurred at the parallel positio! but when the operating slip system was {10i0) (i210) the hardness was a maximum perpendicular to the [0001] projection. A minimum hardness was always observed at a rotation of 90 deg from the maximum. It follows that the orientation of the projection of the [0001] can be determined on any non-basal plane by making hardness measurements at a number of indenter orientations. The determination of the orientation of the [0001] projection on two non-parallel, preferably orthogonal, surfaces of the specimen will allow location of the [0001] direction in the specimen. It seems possible that such measurements could be used to examine, at least qualitatively, the preferred orientation existing in polycrystalline hcp materials. An investigation of the microhardness anisotropy in Zircaloy-2 was undertaken to ascertain whether these measurements could be used for this task. EXPERIMENTAL PROCEDURE Single crystals of Zircaloy-2 were grown by an a-8-a annealing sequence using electron-beam heating.= The orientation of the crystals was determined by a conventional back-reflection Laue technique. The crystals were then mounted on a goniometer head and the desired crystallographic faces were milled and chemically polished. Polycrystalline Zircaloy-2 specimens were prepared from fabricated sheets or plates. Inverse pole figures for these materials were obtained using the X-ray diffraction techniaue described by Jetter, McHargue, and illiams.' A Wolpert-Greis Micro-Reflex hardness-testing machine was used to make the Knoop microhardness measurements. The single-crystal and polycrystalline specimens were loaded to 0.5 and 2.0 kg, respectively. Determination of the scatter of hardness numbers as a function of applied load for several indenter orientations on several specimen surfaces showed that the loads selected were the lightest consistent with minimum scatter. Heavier loads did not appreciably decrease the scatter and produced hardness impressions too large to be conveniently measured with the equipment used. Seven crystallographic planes of the single crystals were examined, while six planes of examination were used in studying Zircaloy-2 polycrystals. The specimens were rotated 10 to 15 deg after each measurement and from four to eight impressions were made at each angle of rotation. RESULTS The two angles which were used to relate crystallographic directions and planes in the hcp cell to the planes of examination of the single crystals are shown in Fig. 1. 8 is the angle between the c axis. [0001]. and the normal, N, to the plane of examination. a is the angle between the long diagonal of the Knoop indenter and the projection of the c axis on the plane of examination. For exampIe, if P = 90 deg and a = 0 deg, the plane of examination is of the family

Jan 1, 1967

By H. Conrad, V. V. Damiano, G. J. London

The slip mode activated during the c axis compression of single crystals of commercial-purity ingot SR beryllium, high-purity (twelve-zone-pass) beryllium, and Be-4.4 wt pct Cu and Be-5.2 wt pct Ni alloys in the temperature range of 25° to 364°C was determined using two-surface slip trace analysis, slip-step height analysis, and electron transmission microscopy. All three techniques indicated the occurrence of copious pyramidal {1 122) (1123) slip in the alloys over the entire temperature range, the amount increasing with temperature. Pyramidal slip was also indicated in the high-purity beryllium by slip trace analysis and electron transmission microscopy, but the amount was somewhat less than in the alloys. For the commercial-purity ingot crystals, only a very small number of pyramidal slip lines were observed, and these were in the immediate vicinity of the fracture surface. No pyramidal dislocations could be detected by electron transmission microscopy in this material. Dislocatransmissiontions with Burgers vectors [0001] and +(ll20) were identified by electron transmission microscopy inthe (1122) slip bands, as well as those with the j (1123) vector. This was interpreted to indicate that the edge components of the 3(1123) vector dislocations activated during c axis compression dissociate upon unloading according to the reaction i (1123) — [0001] + 3(1120) THE microstrain c axis compression of single crystals of commercial-purity ingot SR beryllium (99.6 pct), high-purity twelve-zone-pass beryllium (99.98 pct), Be-5.24 pct Ni and Be-4.37 pct Cu alloys was described in a previous paper.1 This paper covers in detail the analysis of slip traces observed on two mutually perpendicular lateral surfaces of these specimens, and a detailed description of transmission electron microscopy studies performed on foils cut from the bulk crystals after they had been deformed to fracture in the c axis compression. Observation of slip traces on single surfaces of deformed single crystals are generally insufficient to positively identify slip or twinning modes. The use of two carefully cut and oriented perpendicular surfaces can greatly aid in the positive identification and index- ing of slip traces, although even this technique may be quite inadequate if more than one type of slip system operates and if an insufficient number of traces are observed on the surfaces. The problem is greatly simplified for symmetric cases like that for c axis compression of an hep crystal such as beryllium, in which the operating slip systems are all equally inclined to the direction of the applied stress, and each slip system of a given slip mode has an equal chance of operating. For such cases, the traces of any given slip mode observed on the surfaces cut parallel to the c axis are symmetrically tilted about the c axis. It is therefore possible to quickly determine whether one or more slip modes are operating. Confirmatory evidence in support of the observations made on the external surfaces can be obtained from foils cut from the deformed crystals and examined by transmission electron microscopy. This latter technique serves to identify not only the operating slip plane but also the Burgers vector of the dislocations which participate in the slip. For this purpose, a simplified technique based upon a double tetrahedron notation is used in the present paper. The planes and directions in the hep lattice are all designated by letters rather than indices and extinction conditions are easily determined if the Burgers vector lies in the plane contributing to the diffraction. RESULTS 1) Slip Trace Analysis. The standard (0001) stereo-graphic projection of beryllium is shown in Fig. 1. The two mutually perpendicular, lateral surfaces of the compression specimen are represented by the diametrical planes AA' and BB', also referred to as surface A and surface B. For the specific case represented (a Be-5.24 pct Ni specimen deformed by c axis compression at room temperature), the A surface is tilted 5 deg to the (10i0') plane and the B surface is tilted 5 deg to the (1120) plane. Two surface trace analyses may be facilitated by examining in turn the intersection of various great circle traces of specific pyramidal planes with two surfaces and comparing the angles made with the (0001) plane with those actually observed on the two surfaces. One then identifies the slip traces by trial and error on a best-fit basis. The (1122) type planes (it was found that slip occurred on these planes) are shown plotted on the stereographic projection in Fig. 1. One obtains directly the angles between the (0001) plane and the {1122) traces by measuring the angle from the periphery to the point of intersection along the lines

Jan 1, 1969

By R. G. Ward, D. R. Gaskell

Using the maximum bubble pressure technique, the densities of iron silicates at 1410°C have been measured blowing helium, nitrogen, and argon. By ensuring equilibrium between the melt and the blowing gas with respect to oxygen potential and by minimizing tempcrature cycling of the furnace, iron precipitation in the melt has been prevented. Thus the previously reported effect of blowing-gas composition on the densities of the melts has been eliminated. Consideration of the oxygen densities of the melts gives an indication of the structural changes accompanying composition change. The density-composition relationship of iron oxide-silica melts in contact with solid iron has been the subject of several investigations1-7 and considerable disparities exist among the various results obtained. Of these investigations, all except one5 have employed the maximum bubble pressure method. In the most recently reported of these investigations1 the density-composition relationship obtained blowing nitrogen differed from that obtained blowing argon. The measured densities obtained under nitrogen were greater than those obtained under argon, the difference being a maximum at the pure liquid iron oxide composition and decreasing with increasing silica content. This observation rationalized the disparities existing among the results of the earlier investigations, showing that two lines, one for nitrogen and the other for argon, could be drawn to fit all the earlier results. No explanation for this phenomenon could be offered. Chemical analysis of rapidly quenched samples of melt for dissolved nitrogen, and direct weighing measurements, excluded solution of nitrogen in the melt from being the cause of the increase in density. The range of blowing gases was extended by Ward and Hendersons who measured the density of liquid iron oxide bubbling helium, nitrogen, neon, argon, and krypton. The measured density was found to decrease smoothly with increasing atomic number of the bubbling gas. The work reported here is a continuation of the program initiated by Ward and Sachdev7 to study the densities in multicomponent melts in which the iron oxide-silica system is the solvent. As such it is necessary to explain or eliminate the anomalous densities of iron silicates under different atmospheres, and the present rede termination was carried out towards this end. EXPERIMENTAL The maximum bubble pressure method of density determination was again employed and the experimen- tal apparatus used was essentially the same as that used by Ward and Sachdev.7 A molybdenum-wound resistance furnace heated an ingot iron crucible of internal diameter 1 in. containing a 2-in. depth of melt. The bubbling gas was blown through a 1/4 -in.-diam mild steel tube onto the end of which was welded a 2-in. extension of 1/4 -in.-diam ingot iron rod, drilled out to 5/32 in., and chamfered to an angle of 45 deg. The blowing tube was introduced to the furnace through a sliding seal and its position was controlled by a vertically mounted micrometer screw which allowed the depth of immersion to be determined with an accuracy of ± 0.01 cm. A Pt/Pt-10 pct Rh thermocouple was located below the crucible and temperature control was effected initially by means of an on-off controller and later by a saturable core reactor. The bubble pressure was determined by measurement of a dibutyl phthalate manometer using a cathetometer. PREPARATION OF MATERIALS Iron oxide was produced by melting ferric oxide in an inductively heated iron crucible in air. The liquid was quenched by pouring onto an iron plate. Silica was prepared by dehydrating silicic acid at 650°C for 12 hr. RESULTS Before any measurements of the density of a melt were made, the density of distilled water at room temperature was measured bubbling helium and argon. Both gases gave the density as 1.00 ± 0.01 g per cu cm which showed that the density of the manometric fluid (dibutyl phthalate) was not affected by contact with the blowing gas. With the furnace controlled by an on-off temperature controller an attempt was made to measure the density of pure liquid iron oxide by bubbling argon. The furnace atmosphere gas and bubbling gas were dried over magnesium perchlorate and deoxidized over copper turnings at 600°C. It was found that the pressure required to blow a bubble at a given depth increased slowly with time, and thus it was impossible to obtain a unique value for the density of the melt. Inspection of the blowing tube after removal from the furnace showed that rings of dendritic iron had precipitated from the melt onto the immersed part of the tube. This is shown in Fig. l(a) where the various "steps" correspond to different depths of immersion. The precipitation of iron was considered to be due to one or both of two possible causes: i) The composition of the liquid iron oxide is that of the liquidus at the temperature under consideration and can be expressed by the equilibrium

Jan 1, 1968

By Keith Leonard Sutherland, Ian William Wark

Mercaptobenzthiazole and its sodium salt are marketed under the trade names Flotagen and Flotagen S respectively, for use as collectors for cerussite and other minerals. The structural formulas for sodium rnercaptobenzthiazole and for sodium ethyl xanthate are: Chemically there is a resemblance between the two compounds, though the free acid (mercaptobenzthiazole itself) is much more stable than xanthic acid. Both are readily oxidized, e.g., by iodine to disulphides, and can be estimated by iodometric titration. Qualitatively they are similar as collectors in flotation, although there are quantitative differences between them that may be important in practice. It is deduced that the influence of the nitrogen atom is subordinated to that of the sulphur atoms, and that the dominant group of these compounds is the mercapto group —SH or —5Na. The general method of investigation has been based on contact tests. Two temperatures, 10" and 35" C., have been chosen, and with a standard concentration of 20 mg. per liter of mercaptobenzthiazole (i.e., of the free acid) the influence of alkali, cyanide and copper sulphate on contact at sulphide mineral surfaces has been studied. This standard concentration corresponds to about 19 mg. per liter potassium ethyl xanthate; it brings out the differences between the minerals better than a higher concentra-

Jan 1, 1939

By Ian William Wark, Keith Leonard Sutherland

Mercaptobenzthiazole and its sodium salt are marketed under the trade names Flotagen and Flotagen S respectively, for use as collectors for cerussite and other minerals. The structural formulas for sodium rnercaptobenzthiazole and for sodium ethyl xanthate are: Chemically there is a resemblance between the two compounds, though the free acid (mercaptobenzthiazole itself) is much more stable than xanthic acid. Both are readily oxidized, e.g., by iodine to disulphides, and can be estimated by iodometric titration. Qualitatively they are similar as collectors in flotation, although there are quantitative differences between them that may be important in practice. It is deduced that the influence of the nitrogen atom is subordinated to that of the sulphur atoms, and that the dominant group of these compounds is the mercapto group —SH or —5Na. The general method of investigation has been based on contact tests. Two temperatures, 10" and 35" C., have been chosen, and with a standard concentration of 20 mg. per liter of mercaptobenzthiazole (i.e., of the free acid) the influence of alkali, cyanide and copper sulphate on contact at sulphide mineral surfaces has been studied. This standard concentration corresponds to about 19 mg. per liter potassium ethyl xanthate; it brings out the differences between the minerals better than a higher concentra-

Jan 1, 1939