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By R. D. Russell, R. M. Farquhar

ISOTOPIC tracers have become an important aid in following the progress of chemical processes in the laboratory. It has recently been found possible to utilize a system of naturally existing isotopic tracers to obtain information about the geo- logical history of lead ores. Common lead, such as is found in lead deposits, is a mixture of four stable isotopes having atomic weights 204, 206, 207, and 208. Of these, the last three are identical with the lead isotopes produced as stable end products of the radioactive decays of uranium and thorium: the first, lead-204, is not known to be produced on the surface of the earth by any process. Since uranium and thorium occur in the surface regions of the earth in amounts comparable with lead, and since the half-lives of uranium and thorium isotopes are of the same order as the age of the earth, they produce the radiogenic lead isotopes in amounts com- parable to the amount of nonradiogenic lead present. Every significant exposure of a sample of lead to uranium and thorium will therefore lead to the permanent alteration of the lead isotope ratios in that sample.

Jan 5, 1957

By S. A. TAYLOR

THERE is probably no other mineral industry of which the public has as much information and misinformation as it has of the coal industry. Unfortunately, however, the general public's knowledge of the coal industry, outside of the particular kind of coal it is accustomed to, by reason of use, is largely made up of information received from newspaper and popular magazine articles, in which the mine workers are depicted as overworked and mistreated men, and the coal operators as "coal barons." Those who have any specific knowledge of exact conditions in the coal industry know how unjust and un- fair such an opinion of the coal industry is, not only to the miner but to the operator as well. Many reporters and writers of magazine articles are misled by statements regarding the condition of the miners that are exaggerated and not founded on facts and, if an investigation of the conditions of the miner's work, his habitation and surroundings were fairly made, it would at least compel more truthful statements by those who write for public reading. That such an investigation would not reveal anything that was wrong, or anything to be censured or cured, no one, I think, would maintain, but I do think that any fair investigation of the facts would show that conditions in and around the newer and later-developed coal mines and communities would compare favorably with those of manufacturing districts, and that where the mines and com- munities are old and not very attractive places to work, or live in, they carry with them other considerations, compensating for these conditions, and cannot be remedied by reason of a lack of sufficient coal to warrant economically any costly changes.

Jan 1, 1926

By Henry Knox

AMIDST the tumult and the shouting of the times, there are perceptible certain tendencies, quiet though serious, to take stock of the situation with a view to putting our house in order, and of these none is more encouraging than the awakening, interest in the higher education, and especially in technical education. Various committees of the professional organizations have cast much light on the matter and have pointed the way to progress and reform, but their scope is necessarily restricted by the requirements of precision and any excursion beyond these bounds must be undertaken by the unfettered individual who is free to rush in where responsible committees fear to tread. A discussion of the bearing of the higher education on character scarcely lends itself to objective treatment and yet, fraught as it is with imponderables and abstractions, the theme cannot be escaped in any com-prehensive scheme of education. The question is being pressed with growing insist-ence, why these United States, relatively to Europe, are deficient in intellectual output, and the ready reply, "Because America is a new country and Americans are too intent on developing their natural resources," is too facile and too false to carry conviction.

Jan 12, 1922

By H. J. Hager, P. H. Haskell

Fox the past 20 years Alabama has probably led all other coal-producing districts in the proportion of coal prepared by wet washing. All rail mines, with one exception, and a high percentage of truck mines now wash all coal under 3 or 4 in. Most of this coal has been cleaned by jigs, though within the past few years one or more wettable plants have been installed for cleaning some of the coal from practically all the major seams. These tables supplement either single or multicell jigs usually for one of the following purposes: (I) to wash the finer sizes of raw coal, (2) to rewash the finer sizes of washed coal after they leave the jigs, (3) to retreat jig middling products. The main purpose of this paper is to present cleaning data and operating factors involved in the preparation by tables of the finer sizes of raw coal. The specific information and data pertain to the Mary Lee seam of coal as extracted at three of the mines of the Alabama By-Products Corporation, which produces coal for both by-product coke-oven consumption and the general steam market. The Mary Lee seam has long been recognized by coal-preparation authorities as presenting a very difficult ash-reduction problem. Washing characteristics and physical structure of the seam vary widely. Its thickness ranges from 32 in. with no rock parting to l00 in. with from one to three partings. Over the entire field the bed contains bands of bone and rash. These are distributed throughout the seam cross section. A portion of this bone or bony coal occurs as definite bands 1 in. or more thick; however, some bone is interlocked as layers within the coal and consequently breaks into flakes when the coal is broken. This material is relatively high in ash and its specific gravity varies widely. It has been observed that in most cases in the washing of Mary Lee coal from 10 to 18 per cent of the raw coal is within ±0.10 specific gravity of the attempted point of separation. Therefore with the average wet jig, only with extreme difficulty can a low-ash product be obtained without loss of much marketable coal in the refuse. Without entering into the controversial question as to whether modern washing equipment can efficiently handle simultaneously all sizes up to a given maximum, suffice it to state that the comparatively old-type jigs in service at the Alabama By-Products Corporation's mines could not clean the fine sizes satisfactorily. Therefore, in 1931 that company installed six diagonal-deck tables at the Barney mine, which were installed as an addition to a complete plant cleaning all coal below minus 3 in. The primary washed product is shipped as steam coal and another portion may be prepared as washed nut for domestic trade. These tables are washing 9 tons per hour of raw coal sized to ¼ in. to 0. The washed table coal is mixed with the 3 to ¼ -in. jig product to constitute a 3 in. to o steam coal.

Jan 1, 1941

By George Mixter

MINING, in contrast to manufacturing, deals with a wasting asset. That which is taken out of the ground is gone, the property is depleted to that extent, and will eventually become exhausted of profitable ore. So the life of a mining company is dependent upon the ability of its management to develop improved methods to permit extraction at a profit of the lower-grade ores which remain, to extend by intelligent exploration the limits of its known ore bodies, and to find and acquire new properties to take the place of those that, for one reason or another, are no longer operated. Its history is a story of constant change, of the working out of properties here and the acquisition and development of properties there, to maintain the vitality of the whole. It is a story of estimating with the tools and the knowledge available the location and extent of hidden ore bodies and of devising the means of extracting

Jan 1, 1948

By H. Rees

This paper supplements and brings up to date a report prepared earlier this year and presented at the Eleventh Pan American Railway Congress in Mexico City. Most of the original report is contained in this paper in order to acquaint the reader with the project background. On December 1, 1961, construction of this locomotive was completed. Stationary testing started immediately, and a host of problems in various areas were uncovered. Many of these had no relation to the use of coal in a direct fired gas turbine. All of them emphasized the problems which plagued previous projects of this kind. In 1944 the Locomotive Development Committee of Bituminous Coal Research, Inc., was formed to study the problems of combustion, coal handling, and fly ash removal which would have to be solved before coal could be used to fire a gas turbine. By 1947 this committee was composed of the chief executive officers of nine eastern railroads and five eastern coal companies. All of the members of this committee were vitally concerned in a coal fired gas turbine because coal cost only one-fourth as much per heat unit as fuel oil. A number of research projects were started to develop and test components on a small scale. This included work at John Hopkins University, Battelle Memorial Institute, Institute of Gas Technology at Chicago, Purdue University, and Southern Research Institute. By 1946 a pilot plant had been installed at the Dunkirk, New York plant of Alco Products Div. of American Locomotive Co. The U. S. Bureau of Mines made available to the Locomotive Development Committee (hereafter called LDC) a Houdry process gas turbine plant, originally destined for a Russian oil refinery. The full scale pilot plant was used to evaluate the results obtained from the small scale studies under actual gas turbine conditions. Operation of this plant disclosed a number of problems which had not been discovered in the small scale tests. By 1951 four 250 hr tests had been conducted with the Houdry gas turbine to test out a variety of equipment. The major problem concerned the removal of abrasive fly ash from the products of combustion so that wear on turbine blades would not be excessive. The first 250 hr test showed that the original fly ash separating equipment was inadequate. Large ash particles passing through the turbine blading were nicking the leading edges of the first row blades. At the conclusion of the second 250 hr test, erosion was so severe that the first row of stator and the first row of rotor blades were replaced. At the end of the third 250 hr test, it was necessary to replace the first three rows of stator blading. The fourth test was used to test out a new design fly ash separator developed by LDC and named the Dunlab tube. This device gave more encouraging results than any of the others tested. Early enthusiasm for overcoming major difficulties had resulted in placing an order in 1946 with Allis-Chalmers Mfg. Co. for a 3750 hp regenerative gas turbine. The gas turbine, together with associated combustion and ash removal equipment, coal handling equipment, generators and gear reduction unit was installed at Dunkirk by 1951. A 750 hr test was made in 1952 with the LDC-Allis Chalmers gas turbine power plant. At the end of this test it was necessary to replace the first four rows of both rotor and stator blading. Rows 5 and 6 did not require replacement. In 1953 the American Locomotive Co. joined with LDC and assumed an active role in equipment development and manufacture. During 1954 LDC-Alco operated the rebladed gas turbine 300 hr to determine if a new fly ash separator was adequate. Performance of the improved separator was considerably better, but trouble was experienced with clogged blowdown lines from the Dunlab tubes. When these lines clogged it permitted the passage of abrasive particles. In 1955 a total of 1421 hr was run. This included 243 hr of cycle operation on Union Pacific coal from the D. O. Clark mine at Superior, Wyoming. During the 243 hr a total of 370 tons of coal was consumed. The purpose of this test was to determine if U.P. coal was suitable for use in a coal fired turbine. It was the unofficial opinion that it was as good or better than the eastern coals that had been tested.

Jan 1, 1964

By J. O. Lewis

The operation of gas-condensate fields is comparatively new and involves physical principles with which the industry was not prcviously familiar. It has been necessary to devise methods for testing gas-condensate wells and to correlate laboratory and field data. In this paper new methods are advanced for interpreting well G.P.M.† tests whereby dilution by dry gas can be estimated and information supplied on revaporization of condensates by dry gas. Inaccuracies in well test data are discussed. Changes in flow rates can cause changes in the G.P.M. of the effluent and it may take some time for a well to become stabilized after an important change in flow rate. Retrograde tests as usually conducted cannot be directly compared with field G.P.M. data, because the retrograde tests usually include solution gas in the condensates, which are reported On the cumulative basis whereas field data (G.P.M.) usually report pentaneS PlUS on a rate or instantaneous basis. Introduction Though long known to physicists, the phenomena Of retrograde condensation became known to the oil and gas industry Only in recent years, when deeper drilling disclosed that the behavior of vapors under changing pressures was different in high-pressure reservoirs than under the low-pressure operations with which the industry was familiar. These deep, high-pressure reservoirs in which condensation and vaporization behaved inversely to the accustomed manner became known as "gas-distillate," or preferably "gas-condensate" fields. Partly to prevent precipitation and retention of liquids in the reservoir, but still more to prevent the waste of residue gas, the operation known as "recycling," or preferably "cycling," was instituted, in which the residue gas is reinjected into the reservoir, thus maintaining pressure and driving the wet gas to the producing wells. For lack of field experience to serve as a guide, the industry had to assume that theory and laboratory experiments could accurately forecast retrograde behaviors in operating these gas-condensate fields, but it is obvious that these assumptions should be checked at the first opportunities against actual field experience. To make such checks, it is necessary to accumulate a large quantity of reliable field data, but experience has shown that it is difficult to obtain reliable field data and that the laboratory data as usually presented are not in directly comparable form. The problems of correlation involve the complex phase behavior on the one hand, and a knowledge of field data and a visualization of underground conditions on the other hand. This paper is an approach from field experience, The purposes of this article are to discuss the sources of uncertainty in the data and to present methods of analyzing, interpreting and correlating laboratory and field data. Data mostly from lower Gulf Coast fields are presented, from which some conclusions can be derived, but better data from more sources than those available to the writer will be required before satisfactory answers to many questions can be obtained. This paper is presented to stimulate the analysis and publication of data from other fields, the reexamination of field and laboratory methods, and the taking of more complete and reliable field tests. For these purposes, the writer presents some speculations that otherwise would not be appropriate.

Jan 1, 1947

By J. O. Lewis

The operation of gas-condensate fields is comparatively new and involves physical principles with which the industry was not prcviously familiar. It has been necessary to devise methods for testing gas-condensate wells and to correlate laboratory and field data. In this paper new methods are advanced for interpreting well G.P.M.† tests whereby dilution by dry gas can be estimated and information supplied on revaporization of condensates by dry gas. Inaccuracies in well test data are discussed. Changes in flow rates can cause changes in the G.P.M. of the effluent and it may take some time for a well to become stabilized after an important change in flow rate. Retrograde tests as usually conducted cannot be directly compared with field G.P.M. data, because the retrograde tests usually include solution gas in the condensates, which are reported On the cumulative basis whereas field data (G.P.M.) usually report pentaneS PlUS on a rate or instantaneous basis. Introduction Though long known to physicists, the phenomena Of retrograde condensation became known to the oil and gas industry Only in recent years, when deeper drilling disclosed that the behavior of vapors under changing pressures was different in high-pressure reservoirs than under the low-pressure operations with which the industry was familiar. These deep, high-pressure reservoirs in which condensation and vaporization behaved inversely to the accustomed manner became known as "gas-distillate," or preferably "gas-condensate" fields. Partly to prevent precipitation and retention of liquids in the reservoir, but still more to prevent the waste of residue gas, the operation known as "recycling," or preferably "cycling," was instituted, in which the residue gas is reinjected into the reservoir, thus maintaining pressure and driving the wet gas to the producing wells. For lack of field experience to serve as a guide, the industry had to assume that theory and laboratory experiments could accurately forecast retrograde behaviors in operating these gas-condensate fields, but it is obvious that these assumptions should be checked at the first opportunities against actual field experience. To make such checks, it is necessary to accumulate a large quantity of reliable field data, but experience has shown that it is difficult to obtain reliable field data and that the laboratory data as usually presented are not in directly comparable form. The problems of correlation involve the complex phase behavior on the one hand, and a knowledge of field data and a visualization of underground conditions on the other hand. This paper is an approach from field experience, The purposes of this article are to discuss the sources of uncertainty in the data and to present methods of analyzing, interpreting and correlating laboratory and field data. Data mostly from lower Gulf Coast fields are presented, from which some conclusions can be derived, but better data from more sources than those available to the writer will be required before satisfactory answers to many questions can be obtained. This paper is presented to stimulate the analysis and publication of data from other fields, the reexamination of field and laboratory methods, and the taking of more complete and reliable field tests. For these purposes, the writer presents some speculations that otherwise would not be appropriate.

Jan 1, 1947

By R. T. Torgerson, W. A. Baginski

Alloying studies were conducted on modifications of Cb-10W-1OHf (C-129) alloy as part of a cooperative alloy development effort between The Boeing Co. and the Wah Chang Corp. The purpose of these studies was to develop a fabricable, high- strength columbium alloy with superior melding properties. The initial investigations of alloy modifications were conducted using laboratory-melted button ingots. An alloy with the composition exhibited excellent veld ductility, elevated-ternpevature strength, and fabricability. The yttrium-modified alloy was desigrzated C-129Y and was selected for further developrnetzt. Three prodziction heats of C-129Y weve processed into sheet. Welding, forming, and tensile proper-lies are presented for this material. Tungsten-are welds of. C-129Y exhibited a minimum bend radius of 1/2T in the as-welded conditioti compared to 8T for C-129 alloy. An investigation was conducted on Disil coating of C-129Y and test data are presented on oxidation resistance and effects of re-entry environments. The excellent combination of strength, fabricability, weldability, and low transition temperature of C-129Y alloy offers potential design advantages for use of this alloy in structures of aerospace vehicles. It is atiticipated that C-129Y will rapidly supplant C-129 and similar alloys clue to the versatility provided by its impvoved welditzg properties. COLUMBIUM alloys with improved properties are required to achieve better performance and efficiency of radiation-cooled structures for re-entry vehicles and recoverable launch systems. Cooperative work by The Boeing Co. and the Wah Chang Corp. resulted in the development several years ago of C-129 alloy, a high-strength Cb-W-Hf alloy.' This alloy has received favorable consideration for many advanced designs of high-temperature structures due to its excellent combination of properties. However, this alloy exhibits low weld ductility unless given a high-temperature stress-relief treatment. For this reason the development effort was directed towards modification of the C-129 alloy composition (Cb-1OW-1OHf) to eliminate the need for post-weld heat treatment. This paper describes the successful development of an alloy meeting this requirement. This new alloy was designated C-129Y and has a nominal composition of EXPERIMENTAL PROCEDURES Alloying Studies. Various Cb-W-Hf compositions were investigated using are-melted button ingots. These buttons were hot-forged using a protective glass coating and rolled into sheet specimens. Metal-lographic examination: tensile testing, and welding studies were conducted to evaluate properties of the experimental alloys. Sheet Fabrication. Three pilot production heats of C-129Y were fabricated into sheet to establish processing techniques and to determine sheet properties. The three heats consisted of 6-in.-diam ingots weighing from 140 to 250 lb. The ingots were prepared by electron-be am melting followed by vacuum-arc melting. The hafnium and yttrium additions were made during the are-melting operation by tack welding alloy strip additions to the Cb-W master-alloy electrode. The final ingots were machined into billets with samples of the machine turnings collected for chemical analysis. Ingot breakdown methods for the three heats are as follows: Ingot Ingot Heat Size Weiaht___Breakdown Method A 6 in. 250 lb Hot extrusion B 6 in. 140 lb Hot forging C 6 in. 250 lb Hot extrusion Sheet bars from the extrusion and forging operations were conditioned, recrystallized, and rolled into sheet. Initial rolling was conducted at elevated temperatures and final rolling was conducted at room temperature.

Jan 1, 1967

By Howard N. Eavenson

DURING the past year, as in the preceding ones, prices continued to fall, production to decrease, and more mines were closed. Much attention is being given by the industry to suggested plans for betterment of its position, and if the scheme recently brought out for consolidation of sales agencies into district agencies is loyally carried out, it cannot but help to improve conditions. The progress in the anthracite industry is shown in the report of its chairman, E. H. Suender; changes in coal preparation are outlined in the report of J. B. Morrow, chairman of Committee on Coal Preparation, while increased mechanization of the western mines is described by Eugene McAuliffe, chairman of the Committee on Machine and Strip Mining. In spite of the depression, interest in the Coal Division has been increasing, its meetings have been well attended, and its committees are active and have been doing excellent work.

Jan 1, 1932

By B. W. Frazier

At a recent meeting of the North of England Institute of Min ing and Mechanical Engineers, during a discussion upon the com pression of air, attention was called to an apparent anomaly in the phenomena attending the compression. At a subsequent meeting this apparent anomaly was explained by Prof. Herschel, and all the facts observed shown to be strictly in accordance with the laws of thermodynamics. Upon reading the report of the discussion in the published transactions of the society, it occurred to me that an attempt to determine mathematically the amounts of energy (whether in the form of heat or of work) expended and absorbed in compressing air, and causing it to perform work by expansion, might prove of use to some who have not access to any treatise upon the application of the laws of thermodynamics to the compression of air, and who have not the time or the inclination to make such application for themselves. The apparent anomaly noticed was this: If air be compressed, and at the same time, by the sufficient application of a cooling medium, kept at a constant temperature, the indicator diagrams in the

By E. H. Greener, M. E. Fine

The internal friction (1/Q) of cobalt Fig. 1 (measured by an electrostatic dynamic method1) near 250°C begins to increase rapidly on heating and continues to increase until 560°C, the highest tem- perature measured. In the plot of log of 1/Q against 1/T, above 250°C the data nearly fit two straight lines intersecting at 400°C, approximately the temperature of the hexagonal-cubic transformation. The higher temperature branch corresponds to an effective activation energy of 6500 cal per mole, the lower temperature branch 11,000 cal per mole. Young's modulus Fig. 2 increases approximately

Jan 1, 1959

By R. G. Weavind, R. S. Young, I. Wolf

ONE of the most important fields of investigation at the Diamond Research Laboratory in Johannesburg is concerned with improvements in metallurgical practices for the diamond mining companies, with particular reference to increased recoveries of the smaller industrial stones. Considerable work has been done on the possible application of flotation processes to the diamond industry. From the viewpoint of recovery processes, diamonds in their natural state may be grouped into two classes, the water-repellent diamonds, which adhere to a grease surface, and the water-avid diamonds, which, because of their wettability, will not adhere to a grease surface and must be recovered by means other than the grease tables used for water-repellent diamonds. Experiments in the flotation of small diamonds from both kimberlite and alluvial deposits indicate the following conclusions: Water-repellent diamonds: Satisfactory flotation of —16 mesh diamonds, which are naturally water-repellent, may be accomplished using either Aero-float 25 together with cresylic acid, or Du Pont B23 as frother together with kerosine as auxiliary oily conditioner or froth stiffener. The quantities of reagents required are of the order of 0.15 lb per ton Aerofloat and 0.18 lb per ton cresylic acid. The use of acid circuits is detrimental, and for best results a pH between 7 and 9 should be maintained. R. G. WEAVIND and I. WOLF are with the Diamond Research Laboratory, Johannesburg, South Africa, and R. S. YOUNG, Member AIME, is Director of Research, Diamond Research Laboratory. TN 76B. Manuscript, March 23, 1951. A flotation period of 5 to 10 min is necessary to insure that all floatable diamonds are removed. Diamonds larger than 16 mesh cannot be recovered satisfactorily by flotation. Xanthates do not act as collectors for diamonds, and this is probably associated with their inability to impart a water-repellent surface to this mineral. Water-repellent diamonds smaller than 28 mesh can be floated quite well by the addition of a frother alone, such as pine oil or Du Pont B23. Water-avid diamonds: Partial flotation of the smaller sizes of wettable diamonds can be achieved by preconditioning with fatty acid soaps, cationic amines, and similar reagents, which will impart a water-repellent film to diamonds. Washing to remove excess reagent, followed by flotation, will result in a fair recovery, but the latter is much lower than for water-repellent diamonds. Crushed boart: Recovery of crushed boart from the waste products of industrial uses is best accomplished by first conditioning the diamonds present in the mixture with fatty acids, cationic amines, etc., removing the conditioning agent by washing, and floating in a cell of the pneumatic type. Flotation reagents found to be most suitable are Du Pont B23, and Aerofloat 25 together with cresylic acid. The optimum quantities are 1.2 g Du Pont B23, and 0.55 g Aerofloat plus 1.4 g cresylic acid, per liter of pulp in the cell. A solids-to-water ratio of 1 to 4 is found to be the most suitable, and alkaline circuits are necessary for best results. Diamonds larger than 28 mesh are not recovered satisfactorily by this procedure, but for finer sizes flotation offers an excellent procedure for the reclamation of this strategic industrial material.

Jan 1, 1952

By Evan Evans

IT is appropriate to evaluate 1947 in review as a year of a peacetime record production of about 676,000,000 tons of coal (anthracite and bituminous), closely approaching the extraordinary wartime output in 1944. Considering the general price-wage inflation, it is in point to note that the coal industry sustained the highest wages paid to workers in any major industry, but that coal prices at wholesale levels have risen much less percentage wise than the average for all commodities. The sellers' market continues to prevail. In addition to serving our own country's enormous needs, our coal industry is exporting extraordinary tonnages overseas. This unusual export demand is likely to continue for a while. Moreover, the demand in Europe for American coal mining machinery is a real tribute to the management efficiency of our modern mechanized coal industry. Competitively, the petroleum industry is concerned over its long-term supply, and already a synthetic fuels industry is being publicly advocated. In due time coal and lignite are bound to be

Jan 1, 1948

By P. W. Bakarian, John C. McDonald

Three magnesium alloys were processed in various ways to exhibit a wide variation in the ratios of yield strength and tensile strength in the rolling direction compared to the cross-rolling direction. Basal-plane pole figures were prepared from several specimens. A fair correlation was observed between the property ratios and the ratio of percent of poles oriented in the cross-direction quadrants compared to the percent oriented in the rolling-direction quadrants of the pole figures. THE modes by which magnesium crystals deform are such as to lead to marked preferred orientations in all forms of wrought products. The effect of the active modes at room temperature, coupled with these orientations, is often to produce a lower compressive yield stress compared to the tensile yield stress. The phenomenon is due to easy twinning in compression, and has been well-related to the preferred orientations as described by basal-plane pole figures of the hcp magnesium single crystal. The literature contains some information on the variation with test direction of the tensile properties of sheet, but no quantitative relationship to the observed pole figures has been established. These effects have been reviewed in the few com- prehensive treatises in English which have been written on magnesium technology and metallurgy.1°3 Roberts presents several pole figures, but no tensile-property data in the plane of the sheet. Raynor has no pole figures, but quotes Frommer's4 results. The information in Beck's compendium more or less parallels the results of Jones and powell.5 In both a Mg + 1.5 Mn alloy and a Mg + 4.6 A1 alloy, cold rolling was found not to change the general situation of higher properties in the cross-rolling direction,* than in the rolling direction. Thomas'6 X-ray studies of Jones and Powell's specimens did not permit correlation of properties and preferred orientation. Ansel and Betterton7 report tensile and compressive properties on three other alloys as a function of degree of cold rolling, plus a recrystallizing anneal. As rolled, there was a change in anisotropy with degree of reduction, but all alloys were reasonably isotropic in tension when annealed. X-ray diffraction photograms illustrated the kinds of orientations present, but were not correlated with the properties. Bakarian8 has described a method of determining quantitatively a preferred orientation, and illustrated the method by applying it to pure magnesium and two of its alloys. This method was used in the present work as a basis for correlating the strength properties with the texture.

Jan 1, 1965

A B Cummins President James C Gray, President-Elect J W Woomer, Past President C E Lawall, Eastern Regional Vice-President Donald W Scott, Central Regional Vice-President H C Weed, Western Regional Vice-President Nathaniel Arbiter, Treasurer John Cameron Fox, Secretary AIME 29 W 39 St New York 18, N Y

Jan 1, 1960

By J. Chipman, N. J. Grant, J. H. Walsh, T. B. King

WITH the development of adequate sampling and analysis techniques, much information has been obtained concerning the behavior of hydrogen in the steel bath during the course of steelmak-ing operations. From studies of this type it has become clear that the slag has an important role to play in determining the hydrogen content found in commercial products. A knowledge of the behavior of hydrogen in slags is necessary to round out our knowledge of hydrogen in steelmaking practice; with this information we are better able to assess practical methods of control. In this paper a method developed for analyzing slags for hydrogen content, studies of the solubility of hydrogen in synthetic slags, and studies of the variation of hydrogen content in slag and steel in industrial heats will be described. Previous Work—While very little has been done in the past to determine the hydrogen content of metallurgical slags, measurements have been made on such slag-like materials as geologic magmas and glasses. Goranson as made extensive studies of the solubility of water in natural and synthetic granites. Many workers have investigated the solubility of gases in synthetic and commercial glasses, but the recent work of Russell" is the most extensive. Russell found that the solubility of water in glass was proportional to the square root of the water vapor pressure in water vapor-oxygen mixtures. It was found that the solubility could either increase or decrease with temperature depending on the glass composition. Wentrup, Fucke, and Rief,' and Piper, Hagedorn, and Backes' have extracted hydrogen by holding a slag at 1300" and 800°C respectively in vacuum. Wentrup et al. reported hydrogen and water vapor as evolved together while Piper et al. passed the evolved gases from the hot extraction treatment over hot ferromanganese to reduce the evolved water vapor to hydrogen and, therefore, reported the analyses in terms of total dissolved hydrogen. Yavoiskii has reported hydrogen and nitrogen analyses on steelmaking slags. Dobrokhotov, Povol-skii, and Khan have studied the hydrogen content of basic open hearth steel under slags of varying viscosity. These authors reported that the hydrogen content of the steel bath increased as the fluidity of the slag was increased by the addition of bauxite. They recommended that a viscous slag be used and the steel tapped without deoxidation in the furnace to ensure a low final hydrogen content. Analysis of Slags for Hydrogen Development of Apparatus—The vacuum fusion analysis equipment described by Shields, Chipman, and Grant" was modified for the analysis of slags." This method depends upon the reduction of water in the slag to hydrogen, which is readily determined by the method used for hydrogen in steel. Preliminary experiments were made with a eu-tectic ferrosilicon melt as the reducing agent. Other experiments included the use of graphite and molybdenum crucibles. The ferrosilicon alloy bath was found to produce a thick coating on the furnace tube which could adsorb hydrogen. Graphite produced CO by the reduction of FeO, MnO, and SiO2 in such quantities that analysis for hydrogen was virtually impossible. Molybdenum, while giving a low blank value, could reduce the slag sufficiently to produce a volatile oxide which again was found to adsorb hydrogen. The arrangement finally adopted is shown in Fig. 1. The molybdenum sheet served as the induction-heated susceptor, and was separated from the escaping gases by alumina guide tubes. An outer jacket of alumina protected the quartz furnace tube, and alumina and quartz stools completed the assembly. The falling sample is shown wrapped in aluminum foil, 0.002 in. thickness, which acted as the reducing agent' This foil was careful'~ washed in acetone and an d and then dried in hot air before wrapping the weighed slag sample for charging into the apparatus. Investigation of the hydrogen content of the aluminum foil itself showed that a small quantity of hydrogen was released in vacuum, but had no relation to the weight of the aluminum charged. This quantity of hydrogen was

Jan 1, 1957

By M. Khorouzan, L. Thomas

Designers of semiconductor devices have been strivi,ng to resolve problems associated with Au-A1 alloys in bonded in.tercomzeclions. One approach now being- used is that of waintaining a physical seyav-atioz between the two metals in bond areas. This is accolrzplished by alunzincnz-plating a bonding area on the tips oJ the kovar leads and using alcminurn wires to join the senzicondictor device to the leads. The portion of the kovar lead which is on the externul side of the sealed package is gold-plated to provide an oxide-free surface for soldering or welding. A discoloration condition originally thought to be sinilar to purple plague, occuving in the yluled uluninur bonding area after package sealing, has been investigated to determine its efiects ipm bond integrity. Electron-micro-probe analysis determined that no1 only gold, but lead, zinc, and silicon were also present in the discolored area. A series of samples conlaining' conkrolled umonts of these inzpitrities weve prepared and subjected to a sil.zuluted sealing process. The investigations swcued that, of the contawiinants, only zinc toas detrinenlul to Lhe bond integily. The discoloration condition itself was found not to be detrimental to the bond integrity. DESIGNERS of semiconductor devices have been striving to resolve problems associated with Au-A1 alloys in bonded interconnections. One approach now being used is that of maintaining a physical separation between the two metals in bond areas. This is accomplished by aluminum plating a bonding area on the tips of the kovar leads and using aluminum wires to join the semiconductor device to the kovar leads. The portion of the kovar lead which is on the external side of the sealed package is gold-plated to provide an oxide-free surface for soldering or welding. Contamination as evidenced by discoloration of the aluminum-plated area was observed in a number of integrated circuits undergoing examination for defect characteristics which cause electrical failures.' This paper contains the results of an investigation to determine the nature of this discoloration, its cause, and its effect upon the integrity of the interconnection bond. I) THE NATURE AND EXTENT OF ALUMINUM-BOND CONTAMINATION The initial hypothesis in the investigation was that the discoloration was caused by reaction of the aluminum film with some unknown contaminants during the sealing of the hermetically sealed integrated-circuit flat package. The package is a rectangular ceramic container sealed with glass which surrounds the kovar leads as well as joining the top to the bottom. The seal is made hermetic by heating and cooling the package to devitrify the glass. In the case of the packages under investigation, the hermetic sealing had been accomplished with dry air as internal atmosphere. The apparent effect of contaminations as observed by microscopic examination was the formation of surface oxides having variations in color encompassing the whole spectrum of visible light. The contamination appeared to be related to one of the more notorious examples of these colorations, the so called purple plague.' In addition to purple plague, Fig. 1 shows the tarnish in the luster of the aluminized surface in the bond area which had been observed in many of the integrated circuits. To identify the contaminant in the bond area electron-probe microanalysis techniques were used.3 Fig. 2 shows the result of this analysis. The contaminants identified were gold, aluminum, zinc, lead, silicon, and cobalt. Fig. 2(a) is a back-scatter display of the area under study. The back-scattered electrons provide a general indication of the distribution of elements in the specimen surface. Elements with higher atomic number scatter more electrons back from the surface and are seen as light areas in the picture. The sample current, Fig. 2(b), is the amount of current conducted by the specimen as a result of electron-beam striking it and is an indication of element distribution. The Sample current is the reverse of back-scatter and complements it. Other pictures in Fig. 2 are produced by characteristic X-rays generated by the elements, allowing the isolation of the element of interest. The isolated element appears white and all other elements are dark. In this manner a comparative study provides a correlation between different surface areas and the elements which are in these areas. The area covered by the gold film, Fig. 2(c), shows that the boundary between the gold film and the kovar is not sharp as expected and that some sort of diffusion has taken place. Fig. 2(c) shows that some gold particles have been carried to the bond area and are in the proximity of the bonded wire in spite of the presence of a physical barrier in the form of the un-

Jan 1, 1967

By R. B. Tippin

Laboratory and pilot plant studies showed that supergrade iron ore concentrates (containing less than 2% SiO2) can be made from standard grade magnetic iron ore products by cationic silica flotation. Continuous tests were run using various flowsheet arrangements. whereby (1) super and standard grade products were made simultaneously or (2) only a superconcentrate was produced. After a caustic scrub and desliming pretreatment, the silica in a magnetic taconite concentrate was reduced to 1.8% SiO2 by amine flotation. Approximately 75% of the iron was recovered in the single flotation stage, and by additional beneficiation 95% of the total iron was ultimately recovered,

Jan 1, 1973

YEAR OF ELECTION 1944. SELWYN GWILLYM BLAYLOCK Trail, B.C., Canada 1922. FEDERICO GIOLITTI Torino, Italy 1917. HERBERT HOOVER New, York, N. Y. 1941. DANIEL COWAN JACKLING San Francisco, Cal if. 1939. HENRY KRUMB New York, N. Y. 1942. ESSINGTON LEWIS Melbourne, Vic., Australia 1921. C. McDERMID London, England 1942. PAUL DYER MERICA New York, N. Y. 1913. EZEQUIEL ORDONEZ Mexico City, Mexico 1938. A. M. PORTEVIN Paris, France. 1937. JOHN V. W. REYNDERS New York, N. Y. 1937. GEORGE S. RICE Washington, D. C. 1911. ROBERT H. RICHARDS Cambridge, Mass. 1934. T. A. RICKARD Victoria, B.C., Canada

Jan 1, 1944