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By E. H. Dix

All commercial aluminum contains small percentages of copper, iron, and silicon as unavoidable impurities. The purest metal obtainable commercially, special grade high purity ingot, contains a maximum of 0.50 per cent. impurities of which the usual minimum amount of copper is 0.01 per cent.; silicon, 0.12 per cent.; and iron, 0.20 per cent. This grade is too costly for most purposes. The two standard grades, Nos. 1 and 2, containing a minimum of 99.0 and 98.0 per cent. aluminum, respectively, are more generally used. Other grades of secondary aluminum often contain as high as 3 or 4 per cent. of impurities, which include 1 per cent., or more, of zinc. Specifications for high-grade aluminum-casting alloys generally allow a maximum of 1.7 per cent. for total impurities. The S. A. E. Specification No. 33, which is intended to cover alloys made from secondary aluminum ingot, gives the iron maximum as 1.5 per cent. and the maximum for silicon (including manganese and tin) as 0.75 per cent. The effect of even relatively small amounts of impurities on the physical properties of ingot aluminum is shown by the following cornparison of two lots of aluminum, which may be taken as representative of special grade and grade No. 2 ingot, respectively. AnalysEs Special Grade, Gbade No. 2, Per Cent. PeR CBnt. Copper................................. 0.01 0.32 Silicon................................. 0.12 0.32 Iron................................... 0.42 0.82 Aluminum.............................. 99.45 98.54

Jan 1, 1923

By S. C. Oliphant, R. Floyd Farris

Presented in this paper is a summary of the results of experiments conducted in both the laboratory and the field during the past three years in connection with casing-perfora. tion problems. Included are studies of gun features that influence bullet performance and penetration, and studies of the effect of perforator bullets on casing and the neat cement in the annulus. Discussion and data are also presented relative to the accuracy of depth measurements in deep wells. Introduction It is a common practice in the oil industry to effect the completion of oil wells by setting and cementing casing through the producing horizons and perforating the section of casing opposite the desired interval by means of a gun lowered into the well on a cable or on the tubing. This practice has been followed for some time, and this method of completion has been given considerable study by the companies that render perforating service as well as by the oil companies that utilize their services. Through continued research on this subject, it has been possible to develop guns, bullets, and powder that will permit controlled firing at great depths, and penetration of as many as two strings of casing. It is the object of this paper to present the results of studies made of gun perforating in both the field and the laboratory. These studies were made to determine the factors that affect penetration of the bullet, burring of the casing, accuracy of depth measurements, and other items. It is hoped that by presenting the results of these investigations a better understanding may be obtained of certain of the factors involved in gun perforating and further investigation of the subject will be prompted. Subsurface Tests A well approximately 9000 ft deep, which was being prepared for abandonment, was selected for subsurface tests of gun-perforating experiments, In preparing the well for the experiment, 51/2-in. casing in the hole was pulled and racked in the derrick. A test section of pipe, which consisted of 65 ft of 5-in. 18-lb J-55 casing centered inside 7-in. 28-lb N-80 casing, was placed in the derrick corner and the annulus between the two pipes was cemented from the bottom up with 161/2 lb per gal neat cement, which was mixed and displaced with a cementing truck in the usual manner. After the cement had been allowed to harden for about a week, the test section was lowered into the hole on the 51/2-in. casing to a depth of 6600 ft by casing measurements. The hole was filled with drilling fluid weighing 10 lb per gallon. A perforating company was called to perforate the pipe, but was not advised that an experiment was being conducted. The company was asked to check the total depth (to cross pins in the bottom of the test section), then to raise the gun a given distance and fire a given number of shots with 1/2-in. bullets, pick up another distance and fire a given number of 3/8-in

Jan 1, 1947

By S. C. Oliphant, R. Floyd Farris

Presented in this paper is a summary of the results of experiments conducted in both the laboratory and the field during the past three years in connection with casing-perfora. tion problems. Included are studies of gun features that influence bullet performance and penetration, and studies of the effect of perforator bullets on casing and the neat cement in the annulus. Discussion and data are also presented relative to the accuracy of depth measurements in deep wells. Introduction It is a common practice in the oil industry to effect the completion of oil wells by setting and cementing casing through the producing horizons and perforating the section of casing opposite the desired interval by means of a gun lowered into the well on a cable or on the tubing. This practice has been followed for some time, and this method of completion has been given considerable study by the companies that render perforating service as well as by the oil companies that utilize their services. Through continued research on this subject, it has been possible to develop guns, bullets, and powder that will permit controlled firing at great depths, and penetration of as many as two strings of casing. It is the object of this paper to present the results of studies made of gun perforating in both the field and the laboratory. These studies were made to determine the factors that affect penetration of the bullet, burring of the casing, accuracy of depth measurements, and other items. It is hoped that by presenting the results of these investigations a better understanding may be obtained of certain of the factors involved in gun perforating and further investigation of the subject will be prompted. Subsurface Tests A well approximately 9000 ft deep, which was being prepared for abandonment, was selected for subsurface tests of gun-perforating experiments, In preparing the well for the experiment, 51/2-in. casing in the hole was pulled and racked in the derrick. A test section of pipe, which consisted of 65 ft of 5-in. 18-lb J-55 casing centered inside 7-in. 28-lb N-80 casing, was placed in the derrick corner and the annulus between the two pipes was cemented from the bottom up with 161/2 lb per gal neat cement, which was mixed and displaced with a cementing truck in the usual manner. After the cement had been allowed to harden for about a week, the test section was lowered into the hole on the 51/2-in. casing to a depth of 6600 ft by casing measurements. The hole was filled with drilling fluid weighing 10 lb per gallon. A perforating company was called to perforate the pipe, but was not advised that an experiment was being conducted. The company was asked to check the total depth (to cross pins in the bottom of the test section), then to raise the gun a given distance and fire a given number of shots with 1/2-in. bullets, pick up another distance and fire a given number of 3/8-in

Jan 1, 1947

By I. W. L. Finlay, H. R. Ogden, R. Jaffee, D. J. Maykuth

Aluminum has been found to be soluble in a titanium to about 26 pct, and to raise the temperature range of transformation from a to 8. Two intermediate phoses exist in the system, a new face-centered tetragonal phase, designated as 7, which occurs between 34 and 46 pct Al, and TiAI Metallographic and X-ray diffraction data were used to determine the diagram. ALUMINUM is one of the useful alloying additions for titanium-base alloys. It is an important constituent in two commercial alloys released in 1950, one containing 4 pct A1 and 4 pct Mn, and the other containing 3 pct A1 and 5 pct Cr as the metallic alloy content. It is probable that, in the future, other titanium alloys containing aluminum will be released. In the course of alloy development work, some of the features of the constitution of titanium-rich Ti-A1 alloys have been developed. These are described in the present paper. The only available information on the Ti-A1 system concerns the aluminum-rich end of the diagram. In summarizing the early work, Hansen' indicated that there is little solubility of titanium in aluminum, and that a two-phase region exists up to the intermediate compound, TiA1a (37.2 wt pct Ti), which has a congruent melting point at 1355°C. Fink' has reported that a peritectic reaction occurs at 665°C between the melt and TiA1³ to form the terminal solid solution of titanium in aluminum. The solubility of titanium in aluminum has been established at 0.24 pct at 510°C and is estimated to be between 1 and 1.5 pct at the peritectic temperature. No information has been published on the diagram above TiAl,, other than a statement- hat aluminum raises the a to ß transformation temperature of titanium. Materials and Preparation of Alloys Iodide-type titanium and high-purity aluminum were used in this investigation. Typical analyses of these materials are given in Table 1. Alloys were prepared by arc melting on a water-cooled copper hearth, using the techniques described previously for contamination-free melting.' Weight losses during melting were very low, ranging from 0 to 0.02 g in a 10 to 15 g charge, indicating that little or no loss of aluminum occurred during melting. This permitted the use of nominal compositions for these alloys. Alloy ingots containing from 0 to 7.5 pct A1 were rolled in air at 850°C to 0.040 in. sheet. Alloys containing from 7.5 to 16 pct A1 could only be rolled about 25 pct reduction at temperatures up to and including 1200°C. Alloys containing above 16 pct A1

Jan 1, 1952

By Ballard H. Clemmons

THE future of the steelmaking industry of the Birmingham, Ala., district is closely related to and, in a large measure, dependent on the development of workable, economic processes of ore concentration. Operations thus far in the area have been possible only because of the fortuitous occurrence of iron ore, fluxing stone, and coking coal-all the primary iron-making materials- within a 25-mile radius of the blast furnaces. Commercial ore of the district consists mainly of a 10 to 20-ft hematite-calcite-silica bed locally known as the "Big Seam," a component of the Clinton formation of Silurian Age. At present mining rates, this ore will be available for a number of years. It is largely mined under 1000 to 2000 ft of cover and transported on 15 to 20" slopes that, in some instances, are as much as 10,000 ft long. Under these conditions, particularly with increasing distances from face to portal, mining costs are gradually becoming disproportionately high. Although not a major factor thus far, it should also be noted that the average annual ore output of the district is gradually be- coming more siliceous.

Jan 1, 1950

By Walter V. Knopp, Laurence Delisle

INTRODUCTION THE aim of this work was the preparation of nickel-steels from elemental metal powders by powder metallurgy techniques. It was known that plain carbon steels could be made from a mixture of iron powder and graphite and that the effect of carbon on iron in powder form was of the same nature as that produced in fusion metallurgy. The problem in making nickel steels from elemental powders consisted therefore in finding out whether sufficient diffusion of the nickel and other incidental metals normally present in such steels could be induced in the solid state to modify the properties of plain carbon steels made from powders and produce the beneficial effect of alloying. The composition selected originally was that of an S.A.E. 2330 steel. Metal powders, in the proportion corresponding to that composition, were mixed with graphite, pressed, and heated at different temperatures for different periods of time, to produce bonding of the metal particles and mutual diffusion of the various elements without melting. Temperatures up to 1325°C and sintering periods as long as 6 hr were first investigated because it was expected that such conditions would produce maximum diffusion with an accompanying improvement in the properties of the alloy. It was found that, although diffusion proceeded to a large extent under the conditions investigated, it would not be complete unless sintering were carried out at a high temperature for much longer than 6 hr. Relatively high temperatures and long sintering times are objectionable from a practical point of view, particularly when a low cost material is to be produced, because they necessitate the use of special, costly equipment. Work could be done to improve the diffusion of iron and nickel by changing conditions other than the sintering temperature and time, i.e., finer primary or alloy powders could be used. However, a marked change in the properties of the steel had been observed even with only partial diffusion. It was thought, therefore, that instead of trying to improve the diffusion, advantage might be taken of its incompleteness to produce a special structure consisting, in the unquenched condition, of a hard constituent, rich in nickel, dispersed in a tough pearlitic matrix. Steels with such a structure, not readily obtainable by fusion, should have desirable mechanical properties. Besides, it should be possible to prepare them from elemental powders under economical conditions. This latter alternative was therefore adopted for the second phase of this work. This report is divided into four parts: 1. General Procedure. 2. Effect of Sintering Temperature. 3. Effect of Varying the Nickel Content. 4. Effect of Alloying Elements. GENERAL PROCEDURE The general technique of cold pressing as used in powder metallurgy was applied.

Jan 1, 1948

By J. T. Mackenzie

HENRY MARION HOWE, in whose memory we are gathered together, was one of the great thinkers who develop from time to time to whom is given the rare gift of synthesis. Analysis is given to few, but synthesis, the ability to show the relation of all parts to each other and thus to give a clear picture of the whole, is reserved for the very few. Analysis can be achieved by honesty, intelligence, and industry, but synthesis is only given to genius Professor Howe's crowning achievement is the picture of the whole iron-carbon series shown in Fig. I, which places steel, malleable, gray iron, mottled and chilled irons in their proper relation to each other and shows the essential unity of the series. Perhaps his best statement of the case is found on page go of the Metallography of Steel and Cast Iron in these words: "Each member of the gray cast-iron series consists of the metallic matrix approximately equivalent to that member of the steel-white-cast-iron series to which it corresponds in percentage of combined carbon with its continuity broken up-by masses of graphite . . . " Apparently he had taken considerable interest in this idea around the turn of the century, for he refers to a discussion at the Franklin Institute in 1900 in which he said: "Though many others had probably conceived this relation between the steels and cast irons, it was here enunciated for the first time, so far as I know. It was received with great incredulity." The concept was explained in some detail in a paper on 'The Constitution of Cast Iron" presented before the A.S.T.M. in 1902 when Professor Howe was retiring president of that young society. In the discussion Dr. Sauveur stated that he was "very well acquainted with Professor Howe's theory of the constitution of cast iron," and went on to say that while he "shared it to the fullest extent, some foundrymen . . . claim cast iron is a metal entirely different from steel . . . that steel and cast iron have very little in common, and that therefore the knowledge gained in the study of steel is of little or no value in the study of cast iron." Dr. Moldenke, in discussing the same paper, said he had been working on the same theory for 12 years but he laid no claim to publication. Discussing the difference in the micro- structure of the metallic matrix, Professor Howe pointed out that "such minor struc- tural differences are indeed to be expected, because of the difference in the conditions under which these constituents are generated. "One difference in these conditions is that the steel of most micrographs has been either forged or at least treated thermally in such a way as to give a new structure radically different from that which formed during the initial solidification, whereas the cast irons have not. Hence what we see in the steels is a transformation structure, but in the cast irons a solidification structure. By giving the cast

Jan 1, 1944

By Norman Carmichael, John Kiddie

The problem of transportation in the Clifton-Morenci district of Arizona has been one of peculiar difficulty and consequently has been an important factor in the cost of mining and treating the ores produced. From the crude beginning made over 50 years ago, many changes have been necessary to keep pace with the increased output of copper. A heavy-duty haulage system has developed on the original 20-in. track gage to meet the existent metal-mine conditions. Topography The transportation difficulties of this district may be readily appreciated from the relief map shown in Fig. 1. The northern half of the district is high mountainous country and there is a general but irregular drop toward the southern part, where the country, although still rugged, is in reality a great sloping plain. This is cut by numerous ravines from which the waters, in the rainy season, discharge into the channel of the San Francisco River. A chasm, 1000 ft. deep, has been eroded through the center of the district by Chase Creek, which is flanked by high irregular mountain masses, notably Copper Mountain, American Mountain, Coronado Mountain, and Markeen Mountain. The latter rises 2300 ft. above the bed of the creek, The San Francisco River has also cut a deep channel, though it is somewhat broader than Chase Creek. Eagle Creek traverses the extreme southwest portion of the area, where it has carved picturesquely through vast volcanic flows. Faulting has left its mark upon the topography of the district by adding to the irregularities caused by erosion. Strong faults occur at the Coro-

Jan 1, 1924

By William B. Plank

IN my studies during the past twenty years of the enrollments in the mining and metallurgical schools of the United States and Canada, I have been struck with the great diversity in the curricula offered by these schools. In 1933 when I made my first complete study of the schools (Mining and Metallurgy, May 1934, p. 211), I discovered 19 different curricula or programs of study, leading to almost as many different bachelor degrees, in the 49 schools in the United States and the 4 schools in Canada. These were: (1) Mining Engineering, (2) Coal Mining, (3) Metal Mining, (4) General Mining, (5) Mining Administration, (6) Mining and Metallurgy, (7) Metallurgical Engineering, (8) Metallurgy, (9) Petroleum Engineering, (10) Petroleum Refining, (11) Petroleum Geology, (12) Petroleum and Natural Gas, (13) Ceramic Engineering, (14) Ceramics, (15) Geological Engineering, (16) Mining Geology, (17) Economic Geology, (18) Geo- physics, (19) Fuel Technology.

Jan 3, 1950

By Walter P. Jenney

An investigation, conducted by the author, was begun in September, 1889, by the United States Geological Survey, having for its object the study of the questions bearing upon the occurrence and manner of formation of the deposits of lead- and zinc-ores in Missouri and the adjoining States. The field-work was completed in December, 1891. During the first season the State Geological Survey of Missouri furnished an assistant, and in other ways co-operated in the research within the boundaries of that State. In order that the ore-deposits of the southwest might be compared with those of other sections of the Mississippi valley, an examination was made of the lead- and zinc-mining area of Wisconsin-Iowa, and of the argentiferous lead-mines of the region extending westward from Hot Springs, Arkansas, to Indian Territory. In the discussion of the general geology, and in comparisons between the ore-deposits of the Mississippi valley and those of the Rocky Mountains, the writer has drawn largely from his personal experience, having been engaged for many years in professional work as a geologist and mining engineer in that region. The Director of the U. S. Geological Survey and the Scate Geologist of Missouri have kindly consented to the publication of the present paper. While giving the more important economic results, an endeavor has been made to set forth the unity of plan which appears in the formation of the deposits of lead and zinc of the Mississippi basin, and to show their relation to the argentiferous ores of the Rocky Mountains—that the ores of gold, silver, and mercury, and also of copper, antimony, zinc, and lead, have a universal common origin, irrespective of the geological formations in which they occur.

Jan 1, 1894

By C. W. Mac Gregor

THE observation of the flow layers, or Lüders' lines, produced in mild steel when it is stressed into the plastic range often provides considerable useful information for the study of the fundamental mechanism of the plastic flow of metals. It is a commonly observed fact that as soon as the upper yield point in a mild-steel tensile-test bar is passed, an unstable condition develops in the equilibrium, the load on the testing machine drops and if the surface of the bar contains a thin mill scale, the latter begins to flake off rapidly along certain "lines." These "lines" are in reality traces of wedge-shaped flow layers and are formed by the inter-section of the surface of slip and the surface of the bar. The average plane of the flow layer itself has been found by various experimenters to be inclined at an angle of approximately 45° to the axis of the test bar. In a body of more complicated shape stressed in possibly a different man-ner, the tangent planes to the flow layers at each point seem in many cases to be inclined at an angle of about 45° to the principal stress direc-tions at the point. As examples of the latter may be mentioned the logarithmic spirals obtained when a rivet hole is punched in a thin plate, or when a tube is subjected to internal pressure only, etc. Hence if the flow layers are observed from an experiment, the shear-stress trajectories -the curves indicating the directions of the maximum shearing stresses in the body-may then be approximately determined. Since the latter curves form an orthogonal family inclined at 45° to the principal stress directions, the family of principal stress trajectories, or the curves indicating the directions of the principal stresses, may be thus obtained. Although the discontinuous type of stress-strain curve at the yield point is commonly observed with test bars of mild steel, more recent experiments have shown that this is by no means the only material exhibiting this interesting phenomenon. A similar effect has been observed in zinc and cadmium crystals, by Becker and Orowan;1 in duralumin and other aluminum alloys, by Dawidenkow, 2 Elm,3 Fell, and others; in copper and copper-alloy crystals, by Elam;5 in brass by Elam;5 in brass wires by deForest;6 in higher carbon steels, tungsten steel, and

Jan 1, 1939

By W.M. Peirce

The present work has been done in an endeavor to correlate and complete the data on the constitution of alloys of zinc with other common metals, dealing exclusively, however, with the zinc-rich alloys in which the zinc content is between 90 and 100 per cent. This investigation has included the systems lead-zinc, cadmium-zinc, iron-zinc, copper-zinc, aluminum-zinc, nickel-zinc, manganese-zinc, cobalt-zinc, tin-zinc, and magnesium-zinc. The important ternary system zinc-lead-cadmium and the zinc corners of other ternary systems have been investigated in connection with this work but will not be dealt with here. Zinc does not form a single homogenous zinc-rich solid solution over any considerable range of concentration with any of the metals mentioned. A limited range of solid solubility is said, by previous investigators, to occur in several cases and certain effects on the properties of zinc are attributed (with varying degrees of consistency among different writers) to the presence of certain other metals dissolved in zinc. The increasing use of rolled zinc and the possibilities offered by zinc as a casting alloy in certain fields have made it essential to determine precisely these equilibrium relationships. In carrying out this investigation reliance was placed chiefly on two methods, conductivity measurements and microscopic analysis. The first method proved valuable in determining the existence and extent of solid solubility. The second method stands alone as a means of determining structural characteristics and supplements the first method in the measurement of solid solubility. The scleroscopic hardness of all conductivity specimens was measured partly for its value from the point of view of mechanical properties and partly as a check on the conductivity curves in indicating the limits of solid solubility. No hardness curves are included in this paper, for in no case were they important in arriving at the constitution of any system. Conductivity measurements were in all cases made on cold-rolled strips 0.020 in. thick and 0.5 in. wide, both as cold rolled and after an

Jan 1, 1923

By W. M. Peirce

The present work has been done in an endeavor to correlate and complete the data on the constitution of alloys of zinc with other common metals, dealing exclusively, however, with the zinc-rich alloys in which the zinc content is between 90 and 100 per cent. This investigation has included the systems lead-zinc, cadmium-zinc, iron-zinc, copper-zinc, aluminum-zinc, nickel-zinc, manganese-zinc, cobalt-zinc, tin-zinc, and magnesium-zinc. The important ternary system zinc-lead-cadmium and the zinc corners of other ternary systems have been investigated in connection with this work but will not be dealt with here. Zinc does not form a single homogenous zinc-rich solid solution over any considerable range of concentration with any of the metals mentioned. A limited range of solid solubility is said, by previous investigators, to occur in several cases and certain effects on the properties of zinc are attributed (with varying degrees of consistency among different writers) to the presence of certain other metals dissolved in zinc. The increasing use of rolled zinc and the possibilities offered by zinc as a casting alloy in certain fields have made it essential to determine precisely these equilibrium relationships. In carrying out this investigation reliance was placed chiefly on two methods, conductivity measurements and microscopic analysis. The first method proved valuable in determining the existence and extent of solid solubility. The second method stands alone as a means of determining structural characteristics and supplements the first method in the measurement of solid solubility. The scleroscopic hardness of all conductivity specimens was measured partly for its value from the point of view of mechanical properties and partly as a check on the conductivity curves in indicating the limits of solid solubility. No hardness curves are included in this paper, for in no case were they important in arriving at the constitution of any system. Conductivity measurements were in all cases made on cold-rolled strips 0.020 in. thick and 0.5 in. wide, both as cold rolled and after an

Jan 1, 1923

By C. O. Fairchild

ONE of the fundamental principles of efficiency is the use of adequate and permanent records. The rapid increase in the manufacture and use of recording pryometers is a proof of the appreciation of efficiency principles on the part of the manufacturers engaged in the various technical industries. Where recording pyrometers are not employed in an industry in which temperature measurements are necessary, one will generally find that a printed form is used upon which is written, periodically, the temperatures measured by an indicating instrument. It is no serious condemnation of the workman to state that such records are often "doctored," but it is rather a reflection upon the executive who puts such temptation in the way of a workman. One of the well-known "tricks of the trade" is to "force." a furnace so that it will be at the proper temperature during the periodic trips of the foreman or other official. Indicating instruments and recorders may be used together to great advantage. The recorder furnishes .a printed record and a check upon the operator of the furnace, and a record of value in correlating properties of the finished product with the heat treatment. The indicator should be of assistance to the operator in controlling the furnace or oven. Modern practice requires a temperature-recording instrument that is as simple as possible, rugged, reliable, and sufficiently accurate. Of these qualifications reliability is paramount, particularly in cases where the recorder is used for controlling the temperature automatically. By a reliable instrument is meant one that will run continuously with little attention and with a consistent degree of accuracy. That is, if it is in error by 5 per cent. one day, it must be in error by a like amount on any other clay, and not by 2 per cent. or 10 per cent. The earlier forms of recorders were complex and delicate, or mechanically unsatisfactory and inaccurate, and required considerable attention to keep them in operation. Within the past few years, however, the development in the manufacture of temperature recording devices has been highly satisfactory and many excellent instruments are now available. .

Jan 9, 1919

By Cyril Smith

ISOLATED alloys of copper and silicon were prepared and examined by chemical methods more than one hundred years ago, but it was not until the work of Rudolfi1 that the equilibrium relations. were studied. The early history of the alloys was well described by Baraduc-Muller2 PERCENT SILICON-BY WEIGHT FIG. 1.-COPPER-SILICON EQUILIBRIUM DIAGRAM ACCORDING TO RUDOLFI (1907). and need not be further discussed here. The diagram of Rudolfi, based entirely on thermal observations, showed silicon to be soluble in copper up to 4.5 per cent. at 849° C., at which temperature there was a peritectic horizontal resulting from the formation of a 0 phase with about 7.4 per cent. silicon from a and liquid with 7.85 per cent. silicon. The ß phase was believed to form a eutectic with Cu3Si at 820° C. and 9.8 per

Jan 1, 1928

By Homer Turner

THE nature and comparative features of anthracite and bituminous coals have been discussed by the writer in two previous papers.1 Although this paper is offered as a further contribution to the subject, it seems desirable at the outset to repeat some of the descriptive matter of the early works in order to show the actual connection between various constituents of both coals and the new photomicrographs and other physical and chemical properties.

Jan 1, 1929

By R. Ebeling, M. F. Ashby

The paper is in two parts. The first develops the formulae and method needed to calculate the size, nu)nber, spacing, and volume fraction of hard or inert particles in the interior of a specimen from measurernents made on an extraction replica; throughout, the spread of- particle sizes in a single specimen is taken into account, and the extraction efficiency of the replica is considered. A method for testing whether the particles are randotnly distributed in space is described, and the spacing of randomly distributed particles is discussed. The second Part describes the application of the method to copper containing spherical particles of silica; the description includes an estimate of the errors involved, and a comparison of this with alternative methods. All parameters except uolume fraction can be determined satisfactorily, and the method offers advantages over other electron-,rzicroscopic techniques when dealing with hard particles in a softer matrix, or inert particles in a chem-ically less inert matrix. 1 HE experimental measurement of sizes and numbers of discrete particles of a second phase embedded in a matrix material from opaque, plane sections has been considered by many authors, notably by Fullman.' It is assumed that, when the specimen is sectioned, the particles are also sectioned, so that the diameters of the circles of intersection of particles with the plane of the cross section ("surface diameters") are measured. It is difficult to derive the distribution of true particle diameters ("volume diameters") from measurements of the distribution of "surface diameters" on a plane section. The measurement of size and numbers of small second-phase particles by transmission electron microscopy through thin foils of matrix containing the particles has been described by Cahn and ~uttin~' and by ~illiard.~ Because of overlap and the fact that particles which intersect the foil surface may be sectioned whereas those in the bulk of the foil are not, it is again difficult to measure the true distribution of particle sizes. The use of replicas for this sort of measurement has not been analyzed in detail. A replica made from an opaque cross section, thus replicating the circles of intersection of particles with the plane of section, is analyzed by Fullman's method and suffers from the same difficulties. Under certain circumstances, however, extraction replicas can be used, and offer a special advantage in that they make the determination of the true distribution of particle diameters particularly simple. It is the purpose of this paper to describe this extraction replica method. Consider the example of an alloy consisting of SiOz particles, whose mean diameter is about 1000A, dispersed in a copper matrix. When the alloy is sectioned and mechanically polished, the particles are not sectioned, because they are much harder than the matrix, and so will be either left in the surface or pulled out whole, and because the particle size is smaller than the abrasive size of even the finest abrasive. The particles are chemically inert in solutions which chemically etch or electropolish the matrix, so that chemical treatments do not section the particles either. (Experimental measurements of particle shape in this alloy confirm this—truncated particles are never seen.) Small, hard or inert, particles are therefore not sectioned when the specimen is sectioned and polished. An extraction replica taken from this polished surface shows the true "volume" diameter of each extracted particle; the distribution of diameters seen on the replica is the surface distribution of true "volume" diameters, and the volume distribution of true "volume" diameters is easily derived from it. The extraction replica method is not subject to the difficulties associated with sectioning of particles, and avoids the problem of overlap from which the transmission method suffers. The method is well-suited for studying hard particles in a soft matrix. Examples are provided by internally oxidized alloys, oxide-dispersion strengthened metals like T.D. Nickel, and carbides, nitrides, and strong intermetallic compounds in metals. It should be possible to adapt polishing techniques in alloys containing softer but inert particles to avoid sectioning the particles (say by electropolishing or etching). The method is tested and illustrated in Sections 8 and 9 by applying it to a dispersion of spherical SiO2 particles in a copper matrix. I) SYMBOLS Symbols are defined where they first appear in the text. Volume fractions of particles are denoted by the symbol f, particle diameters by x, center-to-center particle spacings by D, and numbers of particles by N. Mean particle diameters and standard deviations about these means are denoted by x and a. Both arithmetic (subscript A) and geometric (subscript G) means are employed. In this paper we measure the distribution of true diameters of particles which touch or pass through a random-plane section of the specimen. We may want to know the distribution of particle diameters in the

Jan 1, 1967

By C. E. Wood, E. P. Barrett, T. L. Joseph

The invention of the Bessemer converter process in 1856 added great impetus to the manufacture of steel and is one of the outstanding contributions to process metallurgy. Although the process of refining pig iron by passing air through the molten metal bears the name of Henry Bessemer, it should be mentioned in passing that William Kelley of Eddysville, Ky., worked on the process as early as 1847. Kelley was granted a patent on the process in 1857, inasmuch as he was able to prove priority in discovery.' After considerable litigation in 1865 the respective interests of Kelley and Bessemer were combined. On Sept. 10, 1856, Robert Mushet of England obtained his first patent on the application of manganese to cast steel. Mushet anticipated trouble in purifying iron by passing currents of air through it: His patent specified that steel made in this way often contained flaws and was red short or cold short. Mushet understood the refining of pig iron into steel well enough to realize the difficulties likely to be cncountered from oxidation of the iron. Mushet was not only an inventor; he was also an investigator. He understood the principle of selective oxidation which takes place in the converter process, and he realized therefore that the remedy for over-oxidation was attainable if a suitable metal could be found at a reasonable cost and in sufficient quantities. His first experiments were made in small crucibles holding a few ounces of metal. Later his work was conducted on a larger scale and with complete success. Manganese had been used in making steel a quarter of a century before the converter

Jan 1, 1927

By Gunnar Thaning, Borje Bjorkvall

At LKAB Central Division for Metallurgical Research at Malmberget, Sweden, fired pellets are examined in respect to mechanical and reduction properties. The paper deals with descriptions of the test methods. It also involves the rationale for the choice of these tests. Their correlation to the blast furnace operation will be examined. The mechanical tests used are the ISO-tumbler test and the cold compression strength test. Concerning the metallurgical properties, experiments have shown that some superbasic pellets in particular have different disintegration properties in different temperature ranges. Pellets which have favorable reduction properties when tested under isothermal reduction at high temperature may disintegrate to a large extent under low temperature reduction. This is also valid for some types of acid pellets. Consequently, it was found to be necessary to determine the reduction strength both at high and low temperatures. In the low temperature range, the disintegration is measured by tumbling the pellets in soft reducing conditions at 600°C in a modified Linder test equipment. The high temperature reduction strength is determined under load in the Burghardt-Grebe equipment. However, in order to get more information of the high temperature strength, LKAB intends to introduce a softening test. The tendency of high temperature disintegration will also turn up in the swelling test. The swelling properties are examined according to a procedure developed at LKAB. In this test the pellets are subjected to free swelling without mutual contact. The reducibility of the pellets is recorded in the swelling test.

Jan 1, 1974

By Gilbert Santoro

In this study tantalum carbide filaments of various compositions in the fcc region were prepared by heating a tantalum wire in a measured amount of hydrocarbon vapor. Such properties as tensile strength, transverse-rupture strength, microhard-ness, lattice parameter, electrical resistivity, and magnetic susceptibility were measured as a function of carbon content. Some of these properties showed a maximum or a minimum between a carbon-to-tantalum molar ratio of 0.80 and 0.85, the composition range at which the color changes from metallic gray to gold. The recent literature has shown that in the large homogeneity range for the fcc phase of the Ta-C system there is a marked variation for such properties as microhardness,' electrical resistivity, ' thermodynamic properties,z'3 lattice parameter and superconductivity. In addition to the technological interest of these variations within a single phase, important theoretical benefits may ensue from a continuous investigation of properties vs stoichiometry in tantalum carbide and other refractory defect compounds, for example the effect of the metal-metal distance and crystal structure upon bond formation and electronic structure. Whether there is a similar variation of the tensile strength is of practical importance. Of theoretical interest would be the knowledge of how the magnetic susceptibility varies with carbon composition. Both of these properties, as well as the transverse-rupture strength, were determined for tantalum carbide filaments in the fcc phase region. The lattice parameter, the electrical resistivity, and the microhardness were also investigated and compared with values appearing in the literature. EXPERIMENTAL PROCEDURE Material Preparation. Tantalum carbide specimens of various carbon content were prepared by statically carburizing high-purity tantalum filaments in measured quantities of pure hydrocarbon gas. The filaments, which were 10 mil in diameter and 20 or 40 cm long, were heated by their own resistance at temperatures from 1800" to 2200°C using alternating current in some cases and direct current in others. Tantalum wire from two sources was used. One had a reported purity of 99.96 wt pct Ta. The ingot from which this wire was drawn had been electron beam-melted as the final step in its purification. The reported purity of the other wire, which was prepared by a powder metallurgical process, was 99.88 wt pct Ta. The impurities of both tantalum sources are listed in Table I. Spec-trographic-grade toluene or research-grade propane was used as the source of carbon. The apparatus for the carburization of the filaments is shown schematically in Fig. 1. The system was evacuated to 1 x l0-' mm of Hg when using the electron beam-melted tantalum and to less than 1 p when using the less-pure tantalum. Neither the difference in the base vacuum, nor in the hydrocarbon gas, nor in the tantalum filaments resulted in any detectable difference in the properties studied in this work. However, only the carbides prepared from the higher-purity tantalum were used in the magnetic-susceptibility determinations. Once the base vacuum had been reached, the system was flushed with the hydrocarbon and re-evacuated. For any desired composition of the carbide, hydrocarbon gas was allowed to leak into a constant-volume flask to a predetermined pressure. These pressures were measured by a Cartesian diver-type mercury gage with a range from 0 to 20 mm and with a scale expanded to nine times. The hydrocarbon gas was allowed into the reaction tube and the filament was quickly raised to the reaction temperature. The slack in the filament due to thermal expansion was taken up by drawing out the movable electrode with a screw mechanism. The filaments were kept at temperature from a few minutes to 200 hr. In the majority of cases the heating time was 6 hr. The reaction tube was cooled by cascading water on its outer surface. By means of an ammeter and a voltmeter the electrical resistance at the reaction

Jan 1, 1963