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By E. E. Gardner, P. A. Schumann

A description of a new four-point probe configuration which permits measurement of epitaxial layer resistivity is given. An analytic solution to the potential distribution due to a point current source on a multilayered structure is briefly described. Typical solutions for this probe configuration are presented. Probe spacing, layer thickness, substrate resistivity, and substrate thickness enter into the calculation. Correction factors for typical cases are given. A brief description of the construction of a probe which can achieve a small spacing of 15 is presented. The prohe is constructed so that all points are adjustable by micrometers and the probe spacing and configuration can be easily altered. Measurements of layer resistivity with the four-point probe are compared with those taken with the three-Point probe and diode-capacitance techniques. TWO techniques of obtaining profiles of N/N+ epitaxial structures are given. The reproducihility of the probe spacing and resistivity measurement is discussed. The effects upon the resistivity measurement of errors in the measurement of the lager thickness, substrate resistil)itv, and substrate thickness are presented. SINCE its introduction by valdes' in 1954, the four-point probe has been the most widely used tool for determining semiconductor resistivity. Its usefulness ranges from the evaluation of bulk semiconductor ingots to the characterization of impurity profiles in diffused structures. In general the four points, two current probes and two potential probes, are placed on one surface of the material being tested either in an in-line array or in a square array. Numerous correction factors1 8 have been worked out for these configurations which are dictated by the finite geometry of the sample being tested. One method of evaluating thin wafers has been proposed which has two probesg on each side of the wafer. Further modifications have added a fifth'' and a sixth" probe. One paper1' has discussed the accuracy of the four-point probe and the precautions necessary in its use. With the exception of the method where two points are placed on opposite sides of the wafer, the four-point probe is restricted to evaluation of wafers with a homogeneous resistivity or to the case where an isolating junction exists between the substrate and the layer (epitaxial or diffused) being evaluated. Due to the relative resistivities and thickness, the resistance of the epitaxial layer is much greater than that of the substrate, and consequently a majority of the current flows through the substrate. The potential distribution at relatively large distances from the current sources is determined by the substrate resistance, and hence the AV/I value is a measure of the substrate resistivity and not that of the epitaxial-layer resistivity. In the immediate vicinity of a current source the potential distribution is determined by the layer resistivity among other factors. Consequently, if the potential probe is placed very close to the current source, then with appropriate correction factors it is possible to determine the layer resistivity. This was the theoretical basis for using two closely spaced probes on opposite sides of an epitaxial wafer. However, due to mechanical problems, it is desirable to place the four probes on the same side of the wafer. This paper discusses the potential distribution in

Jan 1, 1965

By C. C. Furnas, S. P. Kinney

The efficient operation of a blast furnace depends primarily upon efficient contact between the descending streail1 of solid materials and the ascending stream of gas. A program of research dealing with the interior of the present-day furnace is being carried by the U. S. Bureau of Mines along two lines: (I) observations on commercial furnaces and (2) experiments in the laboratory. Through the courtesy of the officials of the Illinois Steel Co. it was possible to make a detailed investigation of the interior of the shaft of NO. 4 furnace at the company's South Works, South Chicago, Ill. The experimental work is reported in a IT. S. Bureau of Mines bulletin' which will include the results of several thousand observations on the interior of the shaft of this furnace. Such of the data as are presented later in this paper constitute only a brief summary. The second part of the work has been conducted in the laboratory. Only one phase of the laboratory investigation has been completed at the present time, namely, the flow of gases through beds of broken solids." The object of this papcr is to correlate the results of the two different lines of research and to present a. more or less complete picture of the condition of the interior of a blast furnace by giving approximate, quantitative data of the actual size-distribution of solid particles in a typical furnncc, and of the efficiency of contact between the gas and solid phases. With such data before him the operator or the experimenter not only has a much better idea of the actunl conditions inside a furnace, hut he also knows in what direction to look for possible improvement. The discussion which follows presents only a few of the items studied and reported; those persons who are particularly interested in all the result's of this investigation must refer to the aforementioned publication.

Jan 1, 1929

By C. A. Mitke

(Butte Meeting, August, 1913.) 1. Character of Gases which Caused Helmets to Get Out of Order. DURING September, -1911, the fire area in the Lowell mine continually increased and gases resulting from the fire came through the upcast shaft. These gases contained such a large percentage of sulphur dioxide that the men were unable to go up and down on cages, and, within a comparatively short time, repairs in the shaft were found to be necessary. Since the fire was in sulphide ores and extended into certain timbered sections, the gases contained varying amounts of SO2 CO2, and perhaps, at times, CO. The temperature in the shaft was generally about 97°, and the relative humidity from 97 to 99.5 per cent. The corrosive action of the fumes became apparent when the cables had to be changed more often than usual, the heads of lag screws .in the guides of the shaft disappeared, and the cages needed frequent repairs. It also became necessary to repair two compartments of the shaft by putting in 150 ft. of new guides between the 600 and 800 levels and lag screws in nearly all the old guides from the surface to the 800 level. 2. Ordinary Methods of Testing Helmets which were Unsatisfactory. These conditions required all work to be done by men wearing oxygen helmets. The Draeger type was tried, and was used until all repairs were completed. At first the helmets were. tested for air circulation and air tightness and the injector was tested by water gauge according to the methods recommended by the Draeger Oxygen Apparatus Co. Six arrangements, covering .these different tests, are illustrated in the catalogue and circulars of the company.

Jan 7, 1913

By Harry M. Roeser

As a result of the publication, several years ago, of some articles on determining the constants of empirical formulas, the determining the constants of types of curves used for estimating the production decline of oil wells was brought to the writer for study. Methods requiring the minimum of time and labor and the maximum of rigor were sought, as it appeared that the nature of the data from which such curves are computed and the relative uncertainty of occurrence of the events predicted from them did not justify close adherence to the theory on which the solution of such problems is ordinarily based. The technical deficiencies of the solutions presented in this paper, from the standpoint of the method of least squares, are readily apparent to those familiar with that method, but their presentation in detail here is irrelevant to the subject matter. However, it is the author's conviction, after a rather exhaustive study of the problem, that the value of the solutions lose little by the approximate application of the conventional theory. It must be understood by those who use these formulas that the solutions herein given, and the formulas based on them, are merely facilities to aid the valuation engineer in forecasting future events. It is assumed, also, that before application is made of them, prescient judgment based on the circumstances in each case, shows that the forecast has some probability of realization. On this basis only will these formulas be found useful.

Jan 1, 1925

By D. W. Fuerstenau, L. M. Berlioz

In 1957, Charles1 first presented an analysis of a relationship between the energy expended in comminution and the extent of size reduction achieved. Subsequently, Schuhmann extended and interpreted Charles' approach to comminution. According to their analysis, the energy, E, expended in comminuting unit mass of fairly uniformly-sized material is related to the size modulus of the product, k, by where a is the distribution modulus (slope of the log-log cumulative size distribution plot) and C is a constant, which is primarily determined by properties of the solid. If there is any fundamental basis for the E vs k relationship, E must necessarily be concerned with the useful work for the size reduction process and not necessarily the work input, as discussed in detail by Harris.3 Charles and numerous other investigators tested this equation only by relating k to the grinding time, assuming expended energy to be directly proportional to time, but never directly measuring power. In our laboratories, we recently constructed a special batch ball mill with which the power could be accurately determined with torque measuring apparatus.4 With this device, a direct test of the Charles relationship could then be made for ball milling. 5 EXPERIMENTAL A stainless steel mill, 11.5 in. long and 10 in. in inside diam, lined with eight low-silhouette lifter bars, was used for these experiments. The grinding media consisted of 30 kg of single sized, 1-in. diam, stainless steel balls, which occupied about 50% of the total mill volume under static conditions. The void fraction of the static ball load was approximately 0.4, and for the dry grinding conditions used, the corresponding interstitial volume was filled when about 3300 g of the dolomite feed material was present. The 7x9 mesh dolomite used as feed was obtained as a natural, uncrushed product thus as- suring a random distribution of feed particle shapes. Charge weights of 660, 1320, 1980, 2480, 3300, 3960 and 5280 g, which correspond to 20%, 40%, 60%, 80%, l00%, 120%, and 160% of the interstitial load, respectively, were used. Grinding times of 20, 40, 60, 80, 100, 150, 200 and 300 revolutions were considered, with the mill operating at 54 rpm (approximately 60% of critical speed). The tests were made sequentially, in that the size distribution obtained after a certain grinding interval was utilized as the feed for the subsequent period of grinding. Agreement with control experiments where the mill ran continuously for the entire interval was excellent. Torque measurements were made utilizing a Baldwin-Lima-Hamilton SR-4 torque pickup in the manner that has been described previously.3 Standard wet (to obtain the -400 mesh material) and dry sieving procedures were followed using the Tyler full screen series. RESULTS The Gaudin-Schuhmann size distributions obtained in all of these experiments are characterized by distribution moduli (slopes), a, of about 0.66 and are representative of normal dry batch ball milling of a material like dolomite. As an illustration of typical

Jan 1, 1968

By W. J. Taylor

It is, perhaps, more important to put on record the particulars of experiments that are derided failures than those that are successful, as those of the latter class are certain to live, while the former may be lost sight of in a short time, and repeated by others. TO this end, I propose to give the particulars of a straight or no-bosh furnace just tried at the Chester (New Jersey) works, which was such a decided failure as to leave no doubt of the plan being wrong, and determining the necessity of a bosh of some kind, as of old. Some experiences during the past year led me to suppose that the bosh or belly of a furnace was unnecessary, and that the contraction of the walls toward the bottom for the stock to wedge in, in its descent, facilitated dirty walls and scaffolding; hence, irregularity and high fuel. I concluded, however, that a very shallow bosh for a skew-back support to the stock would be necessary, and that the proper place for this was in the tuyere-section, beginning just below the tuyeres and ending just above them, where there is nothing in the solid state but fuel, which is consuming, and no slipping or travel of stock takes place. The cubical capacity of a furnace of this design would necessarily be much less than in the old style, unless it was made very much higher. But I assumed that the loss of room for reduction could be overcome by making the size of the ore and stone charged much smaller, so that the gases would act more quickly. The next point was, what should be the size of the shaft, crucible, tuyere-circle, and tunnel-head for a given quantity of air? My first design was 12 feet diameter of shaft for 7000 feet of air, with a 9-foot crucible and 8-foot toyere-circle. This I soon reduced to 8-foot shaft diameter, which I concluded was large enongh for economical work, if regular travel of the stock on the walls could be maintained. I consulted with a number of experienced furnacemen and furnace-engineers, and the plan was well thought of by many of them; and, as I had also some offers of financial aid from them toward the risk of trying the experiment, my firm concluded

Jan 1, 1885

By P. W. Barton, A. A. Johnson, E. J. Hughes

THE only systematic work on the effect of carbon on the recovery and recrystallization kinetics of iron so far reported in the literature is that of Venturello et al.1 These workers found that doping high-purity iron so that it contained up to 86 ppm C caused a marked retardation of recovery but had little or no effect on the recrystallization kinetics. Such evidence for an effect as was obtained was inconclusive. In the course of a study of electron-beam zone-refined iron the authors have recently examined the effect of added carbon on the recrystallization kinetics of this material. The amount of carbon added was about 50 pct more than was used by Venturello et 01. and definite evidence was obtained that carbon at this level retards recrystallization. The starting material was taken from a batch of 0.2-in.-diameter Johnson-Matthey spectroscopically pure iron rods which had been further purified by being given three passes at 4 in. hr-1 in a standard MRC electron-beam zone-refining unit. The purity of this material. which was used in two other investigations of the properties of high-purity iron,2,3 was established by an extensive series of analyses. Four laboratories, the National Research Corp., Newton, Mass., the Naval Research Laboratory, Washington, D.C.. the Battelle Memorial Institute, Columbus, Ohio, and the National Physical Laboratory. Teddington. Middlesex, England. carried out analyses for carbon. oxygen. and nitrogen. and in addition a complete mass-spectrograph analysis was carried out at Battelle. In all, twelve analyses were carried out for carbon, seventeen for oxygen and twelve for nitrogen. The amounts of these elements found to be present were 10 * 7, 8 i 5, and 0.9 i 0.1 ppm, respectively. The limits given are rms deviations. Two results, one of 46 ppm of oxygen and another of 31 ppm of nitrogen, were rejected as anomalous. The mass-spectrograph analysis revealed the major impurity to be 25 ppm of tungsten. All of the other elements detected were present in amounts less than 0.5 ppm. Some of the rods were doped with carbon by being immersed in a suspension of carbon in oil, heated in a vacuum at 400°C, and then zone-leveled to make the distribution of carbon uniform. Carbon analyses carried out on three of the doped rods gave a mean value of 130 ± 45 ppm. Some of the doped and undoped rods were deformed 58 pct by swaging and cut into specimens 1/2 in. in length. Isothermal recrystallization experiments were then carried out on them at 575", 600°, 615", 630°, and 650°C, the volume fraction of each specimen recrystallized being measured by a point-counting method described by Hilliard and Cahn.4 The results for the two types of specimens are shown separately in Figs. 1 and 2. In Fig. 3 the pairs of recrystallization curves for each temper-

Jan 1, 1965

By R. F. Ashton, D. S. Thompson

In reporting results of precipitation hardening experiments, it is customary to include such conditions as solution heat-treatment temperature, specimen size, and quench medium as well as the aging time and temperature. One portion of thermal history that is often overlooked is the effect of the heating rate employed to achieve the aging temperature. It is the intent of this note to demonstrate the importance of the rate of heating to aging temperatures. This work was carried out on the aluminum alloy 7075 aged at 162oC, a temperature commonly used to obtain stress corrosion resistant tempers. A 2 in. thick plate of 7075 was quenched into 24°C water after solution heat-treatment for 2 hr at 470°C. Approximately 13 in. around the periphery of the plate was discarded to minimize quench rate variations, and the remainder was divided into 0.5 by 1.8 by 2.0 in. blocks which were held at room temperature, 24oC, for 4 days. This aging, or incubation period, at room temperature allowed a copious supply of GP-zones to form. Blocks were then heated at various rates to 162oC using the practices shown in Table I. Both single- and two-step aging practices were employed for each heating rate. The single step consisted of heating directly to temperature at the indicated rate while the two-stage practice included an interruption of heating for 7 hr at 107°C. In the case of the two-stage 100°C per min heating rate experiment, the specimens were returned to room temperature after 7 hr at 107°C where they were held for 16 hr be-fore finally heating at this rate to 162°C. This devia-tion in practice is not considered to be significant. Blocks were removed after various times at 162oC, and aging curves were determined from duplicate R. F. ASHTON and D. S. THOMPSON,Member AIME, are Senior Scientists, Metallurgical Research Division, Reynolds Metals Company, Richmond. Va. Manuscript submitted December 2. 1968. IMD Table I. Aging Practices Two-step Single-Step Heating Rate* Aging Aging Heating Method oC per Min A B Programmed Air Oven 0.23 * 0.01 C D Programmed Air Oven 0.93 ? 0.03 E F Air Oven at Temp -10 G H Oil Bath at Temp ˜100 *Heating rate was measured with a thermocouple at the center of a specimen. An average value between the starting temperature and 3°C below the aging temperature is reported for practices E-H. PRACTICES 70 — A B C E and G 50 - 2 4 6 810 20 40 60 HRS.AT 162°C Fig. 1—The influence of processing variables on 7075 aging curves. Fig. 2—7075 aged according to practice H (single-step aged, fast heating rate) for 3 hr. Magnification 100,000 times.

Jan 1, 1970

THE metal iron has physical arid chemical properties which are some- what different from those of steels, but a knowledge of the pure metal is a useful starting point in studying the behavior of steels. Solid iron exists in two different crystalline forms, called alpha (a) and gamma (?) iron the former being the ordinary form at room temperature. When heated above the "A2 point," 769 C (1416 F), the metal becomes nonmagnetic, and at the "A3 point," 911 C (1672 F), it undergoes a change in crystalline form to become gamma iron. 111 the range 769 to 911 C, it is sometimes called beta (ß) iron to distinguish it from the magnetic alpha, but the two are identical in crystal structure. When gamma iron is further heated to 1392 C (2538 F), it changes into delta (d) iron, which is identical with beta or nonmagnetic alpha iron. Pure iron melts (in an inert atmosphere) at 1536 C (2797 F); the melting point is generally lowered by alloys or impurities. PHYSICAL AND THERMAL PROPERTIES OF IRON Many of the properties of iron undergo abrupt changes at the transition temperatures.1 For example, in heating through the A3 point, a sudden shrinkage in volume occurs. Similarly, melting is attended by sharp physical changes such as an increase in volume. Table 16-1 contains a summary of the measured physical properties of pure iron at several temperatures. Usually the properties change smoothly with the range of stability of a given form, but this is not always true. For ex- ample, the specific heat reaches a sharp maximum at the A2 point al- though no transformation occurs. (See Fig. 14-1.) Solvent Powers of Liquid Iron. Liquid iron is capable of dissolving most of the other metals and many nonmetallic elements as well. Of the metals that are liquid at the melting point of iron, only lead, silver, and bismuth refuse to dissolve to an appreciable extent. Table 16-2 contains a list of the common elements classified with respect to their solubility in liquid iron. Those which are very soluble or practically insoluble require no further discussion, but several of the nonmetals that are gases and exhibit limited solubility are of considerable importance to us and merit more detailed consideration.

Jan 1, 1964

By D. Harrington

One of the main functions of the United States Bureau of Mines is to obtain and disseminate information that will promote safety in and around mines, and the health and safety of employees engaged in mining. Serious health and safety conditions arising out of contamination of air in metal mines by dust, fumes from explosives and fires, and absorption of oxygen by timber and other causes, led the Bureau of Mines to cooperate with the United States Public Health Service in the study of dust occurrence and ventilation in metal mines in various parts of the country. A. J. Lanza, of the U. S. Public Health Service, and Edwin Higgins, mining engineer of the U. S. Bureau of Mines, in 1915, made a detailed study in the mines around Joplin, Mo.; their reports1 are now available. In 1916, 1917, and 1918, a similar study was made in the Butte, Mont., region by Doctor Lanza and D. Harrington, mining engineer of the Bureau of Mines; the reports of this investigation will be available soon. In 1919, the study was continued in some of the Arizona mines by D. Harrington, of the Bureau of Mines, and G. E. McElroy and R. A. Koronski, of the U. S. Public Health Service, the underground work being completed in June, 1920; these reports are now being prepared for publication. In the spring of 1920, the scope of the work was extended, with D. Harrington in charge as supervising mining engineer, and short studies were made in the mines of the Coeur d' Alenes in Idaho and around Oatman, Ariz. It is hoped soon to extend the work into mines of California, Nevada, Colorado, Michigan, and Minnesota, and ultimately to other states should the mining companies be willing to coöperate. While the coöperation of the mining companies is necessary, the companies are put to practically no expense other than supplying a guide to accompany the investigators underground, the length of time spent

Jan 1, 1922

By R. J. Sullivan

DURING the past twelve months the Loudon pool of the Eastern Interior Coal Basin has become established as one of the two largest discoveries since the revival of exploitation in the Illinois region and now occupies a position among the important pools of the United States. On Aug. 1, 1939, production averaged 54,000 bbl. per day from 990 wells, having accumulated a total of 10,305,000 bbl. Its very active develop-ment promises to continue for fully another year. It is the site of one of the industry's most singular large-scale gas-injection programs. LOCATION AND RESERVOIR CHARACTERISTICS At present the pool embraces an area 15 miles long by 3 ½ miles wide in eastern Fayette County, along the western rim of the now well-known Illinois Basin's deeper part, through townships 6, 7 and 8 north and ranges 2 and 3 east of the Third Meridian. It is the northernmost, and most prominent, productive structure of a group extending over a 50-mile trend southward to the Dix pool of Jefferson County. Three horizons have been proved to carry production-namely, the Weiler sandstone at 1390 ft., the Paint Creek sand at 1460 ft. and the Benoist or Bethel, at 1500 ft. Geologically, they fall in the Chester series of the upper Mississippian system, where much of Illinois' early-day oil was found, having been laid down in shallow off-shore waters as a part of the vast delta deposit underlying central Illinois and parts of Indiana and Kentucky. As a result of this type of sedimentation, followed by repeated uplifts and warping along an anticlinal axis, differ-ential deposition of sands and shales contributing to great irregularity took place. This is further reflected by wide variations in permeability, porosity and thickness of all the sands and, accordingly, in the producing characteristics of wells. Permeabilities range as high as 550 millidarcies, with the average commonly lying between 60 and 100. For the three pay horizons the mean porosity is 18 per cent, at a calculated water saturation of roughly 30 per cent. The Weiler sand has an average thickness of 25 ft., the Benoist of about 23 ft. and the Paint Creek of approximately 18 ft. Of these three productive formations the Benoist

Jan 1, 1940

By Norman B. Pilling

Practical limitations to the usefulness of silicon steels are the hardness and brittleness silicon imparts to iron, making iron-silicon alloys of more than 8 per cent. silicon content unusable except where castings can be employed. In the use of commercial silicon steel, in thin rolled sheets, as in transformer construction, when the silicon content exceeds 4.2 per cent. the sheet is too brittle for satisfactory shaping by punching or similar operations. When such a brittle steel is sheared, it frequently breaks along a haphazard path in advance of the cutting tool. In Fig. 1 is shown a slightly enlarged view of the sheared edge of a 14-mil enameled sheet of nominally 4 per cent. silicon steel. In 5 in. along the sheared edge, only 44 per cent. was actually cut; the rest was torn, with the path of fracture varying widely from the path of travel between the shears. This is probably an extreme case of such brittle-ness, but a shearing or punching test is not necessary to reveal brittle-ness of this order; narrow strips will break when bent between the fingers. In Fig. 2, the proportion of actual cut edge is greater, but secondary fractures branch off at about 30" from the line of shearing in advance of the cut. Deprived of the support of adjacent parts of the sheet, the tips of the angles are bent out of the plane of the sheet by the shears, leaving a peculiar flared effect, like the set of the teeth on a saw. An end-on

Jan 1, 1923

By Norman B. Pilling

Practical limitations to the usefulness of silicon steels are the hardness and brittleness silicon imparts to iron, making iron-silicon alloys of more than 8 per cent. silicon content unusable except where castings can be employed. In the use of commercial silicon steel, in thin rolled sheets, as in transformer construction, when the silicon content exceeds 4.2 per cent. the sheet is too brittle for satisfactory shaping by punching or similar operations. When such a brittle steel is sheared, it frequently breaks along a haphazard path in advance of the cutting tool. In Fig. 1 is shown a slightly enlarged view of the sheared edge of a 14-mil enameled sheet of nominally 4 per cent. silicon steel. In 5 in. along the sheared edge, only 44 per cent. was actually cut; the rest was torn, with the path of fracture varying widely from the path of travel between the shears. This is probably an extreme case of such brittle-ness, but a shearing or punching test is not necessary to reveal brittle-ness of this order; narrow strips will break when bent between the fingers. In Fig. 2, the proportion of actual cut edge is greater, but secondary fractures branch off at about 30" from the line of shearing in advance of the cut. Deprived of the support of adjacent parts of the sheet, the tips of the angles are bent out of the plane of the sheet by the shears, leaving a peculiar flared effect, like the set of the teeth on a saw. An end-on

Jan 1, 1923

T.B.King (Depaytment of Metallurgy, Massachusetts Institute of Technology)— A valuable contribution of the authors is in the factual information which they have been able to gather; this type of information is quite difficult to obtain. In many respects, however, it would have been better if they had not subsequently embarked on a discussion of the chemistry of the converter process. It seems inconceivable that the authors do not refer to the papers of Schuhmann and his associates14 which have set the thermodynamic foundation for the whole copper smelting operation. In addition, a very useful review on the physical chemistry of copper smelting by Ruddle 5 appeared as long ago as 1953. An examination of this literature would have convinced the authors that there is no cause to be surprised at a correlation between the magnetic content and the silica content of converter slags, though they rightly point out that one should distinguish between the total magnetite content of the slag and the amount of magnetite which may be considered to be in solution. It is not true that the lowest melting converter slag is that corresponding to the eutectic between ferrous oxide and silica. The simplest slag system which can be considered is a three-component system, since both ferric and ferrous iron are present. As Schuhmann, Powell, and Michal have shown, there are lower melting compositions than this eutectic in the ternary system. The most unfortunate impression given by this paper is that the driving force for chemical reaction is determined by the heat of reaction: of course the entropy change must be taken into account. It would have been more correct to list, in Table VI, values for free energies of formation. Nor can it be said that the data in Table VI represent the "best available data." They do not corregtond with any of the recent, acknowledged sources. F. E. Lathe and L. Hodnett(author's reply)— We are pleased that Dr. King finds the factual information in our uawer of some interest. Dr. King suggests that it would have been better if our analysis and discussion of the data had been omitted, largely because our list of references is so. incomplete. If he will carefully read our introduction, he will see that the questionnaire was sent out in the hope of obtaining data which would throw light on certain questions relating to the use of converter refractories. We did not attempt (nor would the AIME have published!) a complete review of the literature on copper converting, as Dr. King has apparently assumed, nor indeed a complete analysis of the data submitted, but tried only to find a sound basis for the choice of refractories, taking into consideration common variations in converter practice. We hope our paper indicates that, by raising the silica content of the converter slag and operating at a higher temperature, the normal circulating load of magnetite can be greatly reduced, and the whole reverberatory-converter operation improved to a major degree, with resultant important savings. Under such operating conditions, chrome-magnesite brick may be expected to stand up better than those of straight magnesite. Regardless of the choice as between these brick types, however, we find the cost of converter refractories to be so low in comparison with other converter costs as to justify operation under the more severe conditions suggested. Valuable as are the papers by Schuhmann and associates and the book by Ruddle, we make no apology for omitting reference to them, nor for using heats of reaction without mention of entropy changes or free energies of formation. Our primary object was to interest the practicing copper metallurgist, with whose language we may claim to be fairly familiar; we think it would have been unwise to include the highly theoretical phases of the subject which Dr. King suggests. The interest shown in our preliminary paper presented at the New York meeting in 1956, and the trends in practice whtat we have observed since that time, suggest that we did not wholly miss the target. In conclusion, we sincerely hope that Professors King and Schuhmann will independently review the data obtained in our questionnaire and submit a paper giving their own recommendations as to the choice of refractories and the particular converter operating conditions which will result in the lowest overall cost of copper smelting and converting.

Jan 1, 1960

By G. Derge, M. Bourgon, G. M. Pound

A STUDY of electrical conductance in molten Cu-Fe sulfide mattes' has shown that pure molten Cu,S behaves like a semi-conductor in that it is an electronic conductor and its specific conductance, of the order of 100 ohm-' cm-', increases with increase in temperature. On the other hand, pure molten FeS, another electronic conductor, behaves like a metallic conductor in that its specific conductance, about 1500 ohm-' cm-', decreases with increase in temperature. Molten solutions of Cu,S and FeS follow a roughly additive rule of mixtures with respect to both specific conductance and temperature coefficient. The behavior of molten Cu,S may be understood, by analogy to the situation in solids, in terms of semiconductor theory.' It is thought that, although the melt consists of cuprous and sulfide ions, the bond between these atoms has a certain degree of cova-lency. According to the simplest concept the electrons in the partially covalent bonds are thermally promoted to a conduction band. In another concept, small amounts of impurities (undetermined) provide donor or acceptor levels in the forbidden zone between the valence and conduction bands and thus facilitate semi-conduction in the usual way. However, the metallic behavior of molten FeS is difficult to explain, because one might expect from similar reasoning that it too should act like a semi-conductor. It was suggested that the apparent metallic behavior of molten FeS might be explained by a large negative temperature coefficient of density. Thus if molar conductance instead of specific conductance were plotted versus temperature, the slope might prove to be positive, indicating semi-conduction instead of apparent metallic conduction. Accordingly, density measurements were made in order to answer this question in regard to molten FeS and also to provide data for conversion of specific conductance to molar conductance for molten Cu,S and a molten 50-50 wt pct Cu-Fe sulfide matte. Experimental Diagrams of the apparatus are given in Figs. 1 and 2. A 3 x 8-cm dense alundum crucible containing the prefused specimen is positioned in the uniform temperature zone of an induction furnace tube and melted under a helium atmosphere. Then the cell assembly, consisting of two 3-mm spectro-graphite rods, one of which is in a 1-cm ID open

Jan 1, 1959

By Ionel I. Gardescu

In connection with some of the experiments carried out by the writer on the behavior of gas and oil in a sand reservoir,' an interesting phenomenon was observed which may throw some new light on the problem of recovery of oil from a natural reservoir. The experiments are intended to show the effect of the surface area of the occluded gas masses, originally present in a reservoir, on the further evolution of gas from the oil and its consequent effect upon the rate of production of oil. The apparatus used in the experimental work is shown in Fig. 1. It consists primarily of a sand reservoir R and a displacement chamber D, which is used to induce small variations in volume. The reservoir and displacement chamber form a unit, and a lowering of the plunger D is equivalent to increasing the volume occupied by the oil and gas in the reservoir. The reservoir was first filled with dead oil and maintained under pressure until it was ascertained that most of the free gas had gone into solution. The volume of free gas present in the reservoir was computed from the coefficient of compressibility of the fluids by means of the displacement chamber D, reading to 0.005 c.c. and a special gage J reading to 0.02 lb. per sq. in. The oil was saturated with gas under pressure in reservoir S by circulating the oil for a long period of time through the gear pump B. Subsequently, the saturated oil was circulated through the sand reservoir following the circuit S6, B, S6, R4, the sand reservoir R, R1, R², F4, F1, back to reservoir S. In the following experiments the sand reservoir R was filled with gas-saturated oil at a pressure of 415Ib. per sq. in. with no free gas present. This was ascertained by closing off all the outlet valves and determining the coefficient of compressibility of the system by means of the displacement chamber D. Much difficulty was encountered in eliminating all of the free gas masses from the oil reservoir. The dead oil originally present in the

Jan 1, 1932

By C. H. Mathewson, Robert Maddin, W. R. Hibbard

A SATISFACTORY mathematical relationship between shear, elongation and change of orientation in the axial straining of a single crystalline rod or wire may be based on a simple model in which blocks, representing glide lamellae, glide over one another and rotate so as to maintain the original fixed position of the axis as the wire elongates.1 Obviously such a model gives no information concerning strain-hardening or the atomic adjustments at the sliding surfaces and their influence on the internal structure of the blocks. Moreover such an operation could be conducted with rigid blocks only by using self-aligning grips or a flexible attachment which would permit the adjacent blocks to freely assume their changing orientations. There are many unsolved problems (see Andrade2) concerning the manner in which nature departs from the simple model in permitting the essentials of slip, rotation and elongation to occur along with strain-hardening and the appearance of glide lamellae of various dimensions and special characteristics, not fully appreciated at the present time. This paper describes part of an extensive investigation on the development and characteristics of glide ellipses in single crystalline alpha brass rods and is especially concerned with the observation of cross-slip in crystals oriented wholly within the range of slip on a single system according to the generalizations first presented by Taylor and Elam in 1923.3 EXPERIMENTAL PROCEDURE Half inch rods of alpha brass (nominally 70 pct Cu, 30 pct Zn) * were converted into single crystals by melting and gradual solidification in a graphite mold according to the Bridgman method.' In order to remove any coring, the crystals were homogenized at 800°C for 16 hr and tested by etching with a 50 pct nitric acid solution. The back-reflection Laue technique as described by Greninger5 was used for determining the orientations of the crystals. Standard stereographic operations were employed to locate the specimen axis in a triangle of the Taylor and Elam3 projection so that the slip plane and direction could be predicted. The lineage structure reported by Buerger6 was present in the crystals used in this investigation. However, only crystals were used in which the internal differences in orientation did not exceed two degrees. Very little is known concerning the effect of the presence of a lineage structure on the detailed mechanism of plastic deformation.

Jan 1, 1948

By R. F. Mehl, W. Batz, C. Wells

Diffusion coefficient values for carbon in austenite covering a wide range of temperature and composition have been determined employing statistical methods. In addition, the relation between concentration and each of the following, D (diffusion coefficient), Q (activation heat of diffusion), and A (the constant in the diffusion equation), has been obtained. A study of the rates of diffusion of austenite was published in Metals Technology in 1940.' The present investigation is an extension of the earlier work, undertaken (1) to obtain values of the coefficient of diffusion, D, over a much wider range of carbon concentration, and (2) to provide data in all ranges of concentration and temperature in such abundance that statistical methods could be employed to evaluate the accuracy of the data with unusual precision. Composition of Materials: Composition of materials used in this research program are listed in table I. These materials, all forged to about 1 1/4 in. rounds, consist of a high-purity iron, Armco iron, a large number of laboratory-made plain carbon steels containing amounts of impurities normally expected in high-quality commercial steels, and three silicon steels. Since it was known at the time these steels were being made that impurities in the amounts present were unlikely to affect carbon diffusion rates' significantly, the effort made to obtain high-purity steels was not as persistent as it otherwise would have been. Procedure: In general, the procedure followed by Wells and Mehl and described' in detail in an earlier publication' is the one used by the present authors. However, certain modifications have been made which it is believed allow diffusion data to be interpreted more objectively and correctly. These are described completely under appropriate subheadings which follow. Experimental Procedure: Experimental procedure includes (1) the preparation of specimens by welding steels of different carbon contents, (2) the heating of these for certain times at selected temperatures in order to diffuse carbon along the specimens across the welded "interface," and (3) the determination of the carbon distribution across the diffusion zone. Preparation of Specimens: Prior to welding steel of one carbon content to iron or steel of another carbon content, surfaces to be welded are machined perpendicular to the longitudinal axis of cylinders which are about 3/4 in. in diam and 1 1/2 in. long. The prepared, flat, parallel surfaces are brought together and butt-welded electrically. Evidence of a good weld is given in fig. 1. Welding temperature

Jan 1, 1951

By H. F. Easter

(San Francisco Meeting, September, 1915) THE lead department of the El Paso Smelting Works at El Paso, Tex., is operated strictly oil a custom basis. The ores treated are drawn from the surrounding territory, comprising New Mexico, Arizona, western Texas, and northern Mexico. Ores received from the last-named section originally amounted to a very large tonnage, but of recent years have dwindled into comparative insignificance so far as this plant is concerned. This has been clue partly to the establishment of a lead-smelting plant at Chihuahua, which is much closer than El Paso to most of the important mines, and partly to the recent revolutionary troubles in Mexico. There are no mines of either lead or copper in the immediate vicinity of El Paso. In general, it may be said that the lead-ore supply of recent years has been uncertain and precarious, with a general tendency toward an excess of silica and a shortage of iron. This latter requirement has been met in large part by the use in El Paso lead furnaces of considerable amounts of roasted heady copper matte from the Chihuahua smeltery and of converter slag from the El Paso converters. These two materials, coupled with complex lead-copper ores from Bisbee, Ariz., have introduced into the lead-smelting operations a most unusual amount of copper, which has had an important bearing upon the smelting practice of the plant. This matter will be discussed later. The ore, loaded in either box cars or gondolas, enters the storage yard on four tracks elevated about 8 ft. above the ground. As all unloading is clone by hand, unloading platforms at the height of the car floor parallel the tracks on each side to afford a runway for wheelbarrows. At frequent intervals these lengthwise platforms are joined together by others running crosswise to facilitate the distribution of the ores evenly over the beds, which are located below and between the tracks. At present much of the bedding space formerly used for lead ores is given over to the copper department, but 20 bins of various sizes are retained for the use of the lead furnaces and the Huntington & Heberlein roasting plant. The largest of these holds about 1,000 tons, while the smallest holds not over

Jan 8, 1915

By N. J. Grant, K. M. Zwilsky, J. T. Blucher

DISPERSION strengthening has been studied in a number of metal-metal oxide systems. To date those pure metals available as fine particles (less than about 5 p) have received most of the attention whereas solid solution alloys, generally unavailable as fine powders, have not been examined in detail. The present work was undertaken as a preliminary study to evaluate combined effects of solid solution and dispersion strengthening. The technique used was that of dry mixing of elemental powders with the oxide, followed by a diffusion treatment to obtain the solid solution. The average particle size of the powders used was: Ni, 3.2 p (1nco B); Mo, 1.3 p (Fansteel Metallurgical Corp.); and y alumina, 0.027 \i (G. L. Cabot, Inc.). The particle size of the metal powders was determined by Fisher subsieve measurements while the size of the alumina was calculated from a surface area determination. Prior diffusion studies on small compacts pressed from mixtures of nickel and molybdenum powders with and without 7.5 vol pct A1203 indicated that diffusion was complete after sintering for 100 hr at 1800" , or 50 hr at 2250", or 20 hr at 2550° F. The progress of diffusion was followed by microstructural examination and micro-hardness measurements. Two observations made during the diffusion experiments were: 1) That diffusion proceeded faster in the presence of alumina, confirming similar findings by Seith and Loepman on "SAP'';4 2) That diffusion at temperatures above 1800°F resulted in coarsening of the alumina in agreement with results of other authors reporting on the growth of alumina in nickel above 1800"F. Similar experiments in the Ni-Cr system using 6 and 20 p Cr powders of 0.7 and 0.025 pct 0, respectively, did not result in significant solid solution formation even after long time exposures at 2550° F. It must be concluded that chromium oxide films around individual particles interfere with normal diffusion. A nickel alloy containing 5 wt pct Mo and 7.5 vol pct alumina was fabricated by dry mixing of powders, isostatically compacting at 30,000 psi, diffusing for 120 hr in dry hydrogen at 1800" F, and extruding at 1950"~ with a 30 to 1 reduction of area ratio. The resulting structure, presented in Fig. 1

Jan 1, 1963