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By Louis D. Huntoon

The Porcupine gold area, located on the Hudson Bay slope of northern Ontario, has produced over $100,000,000 in gold and has paid more than $28,000,000 in dividends, since the first real production in 1912. The character of the ore has been studied by the geologists of the Bureau of Mines of Ontario, the geological staffs of the operating mines, and engineers commissioned to examine properties there. What information the Government has is free to everybody; the geological staffs of the several properties also give to the visiting engineer what information regarding ore deposition they possess, and the author wishes to express his indebtedness to the geologists of the Ontario Bureau of Mines and the staffs of the operating mines for their free discussion of geological questions. This paper is based on the examination of several properties, various petrographic reports, not only on specimens from Porcupine but from elsewhere in northern Ontario, and interviews with Government and mine staff geologists. The petrographic work has been done by Prof. R. J. Colony, of Columbia University. Geological History The geological history of the district may be summarized as follows: The outpouring of great floods of lava accompanied by beds of tuff, flow following flow; the contacts of different flows can be seen in various parts of the camp. This period mas followed by an uplift and the production of the Temiskaming sediments by erosion. Later, dynamic action turned the sediments and underlying lavas on edge; this was followed by the intrusion of igneous rocks—in the Porcupine area the quartz porphyry, which is of such great importance in connection with the gold deposits. Doctor Burrows says: "The intrusions of quartz porphyry have in some way influenced the deposition or location of the gold but it is not likely the porphyry has been the source of the gold-bearing solutions." This statement of Doctor Burrows I indorse. The formation of non-gold bearing quartz veins followed the intrusion of the porphyry. These veins occur along or near the contact of

Jan 1, 1923

By Louis D. Huntoon

The Porcupine gold area, located on the Hudson Bay slope of northern Ontario, has produced over $100,000,000 in gold and has paid more than $28,000,000 in dividends, since the first real production in 1912. The character of the ore has been studied by the geologists of the Bureau of Mines of Ontario, the geological staffs of the operating mines, and engineers commissioned to examine properties there. What information the Government has is free to everybody; the geological staffs of the several properties also give to the visiting engineer what information regarding ore deposition they possess, and the author wishes to express his indebtedness to the geologists of the Ontario Bureau of Mines and the staffs of the operating mines for their free discussion of geological questions. This paper is based on the examination of several properties, various petrographic reports, not only on specimens from Porcupine but from elsewhere in northern Ontario, and interviews with Government and mine staff geologists. The petrographic work has been done by Prof. R. J. Colony, of Columbia University. Geological History The geological history of the district may be summarized as follows: The outpouring of great floods of lava accompanied by beds of tuff, flow following flow; the contacts of different flows can be seen in various parts of the camp. This period mas followed by an uplift and the production of the Temiskaming sediments by erosion. Later, dynamic action turned the sediments and underlying lavas on edge; this was followed by the intrusion of igneous rocks—in the Porcupine area the quartz porphyry, which is of such great importance in connection with the gold deposits. Doctor Burrows says: "The intrusions of quartz porphyry have in some way influenced the deposition or location of the gold but it is not likely the porphyry has been the source of the gold-bearing solutions." This statement of Doctor Burrows I indorse. The formation of non-gold bearing quartz veins followed the intrusion of the porphyry. These veins occur along or near the contact of

Jan 1, 1923

By Carl Scholz

During November and December, 1907, four serious mine-explosions occurred in the Appalachian coal-field, which resulted in the loss of nearly a thousand lives and caused an eliormous damage to propcrty. These accidents attracted more than the usual attention; coal-trade and engineering papers contained many comments and suggestions on the cause and prevention of accidents; the daily press in many instances condemned the coal-operators and charged these accidents to their negligence, or their anxiety to make money without adopting precautionary measures. Immediately after cach accident the respective State authorities ordered close investigations to be made, with the view of establishing the cause and suggesting remedies to prevent recurrence. Representatives of the Technologic Branch of the IT. S. Geological Survey, to whom the investigation of mine-accidents had recently been delegated by the Secretary of the Interior, visited the mines and co-operated with the local authorities in their determinations. It may be safe to say here that an investigation of a mine after an explosion has occurred discloses but little, because the causes hare been removed and conditions have been entirely changed. On Jan. 8, 1908, the coal-operators of West Virginia organized an association at qTashington for the purpose of making extensive investigations, and sufficient funds were pledged to carry out this work. At this organization meeting, the representatives of the Geological Survey present had no suggestions to offer as to the cause of these accidents. An examinatiou of the various reports concerning these accidents indicates that the explosions were caused by the ignition of gas or dust; they show the point of origin and the direction in which the force was expended, and give a detailed description of the damage done. Very little has bee11 said as to what

Jan 1, 1909

By C. B. Smith, A. G. Guy

The power and convenience of tensor analysis are employed in deriving the equations that describe three-dimensional diffusion in an n-component system plus vacancies. A "Kirkendall coordinate system, '' defined in principle by Kirkendall markers, is used in defining the intrinsic diffusion coefficients that are of primary interest. The defining equations are then transformed to local cartesian coordinates and to fixed cartesian coordinates, the latter being convenient for experimental measurements. Finally, it is shown how the intrinsic diffusion coefficients can be calculated from the experimentally determined quantities. It is generally recognized that any treatment of the essential diffusion phenomena in metallic systems—the jumping of atoms from one lattice position to another—must be based on movement of the atoms past Kirkendall interfaces.' A logical extension of this idea is the proposal that, fundamentally, diffusion must be described mathematically in terms of "Kirkendall coordinates." The basic equations thus obtained may then be transformed into other coordinate systems, when such transformation leads to simplification of either the experimental or mathematical treatment of diffusion data. Tensor analysis is clearly the appropriate mathematical tool for this purpose, since it provides methods both for determining general equations that are valid for all coordinate systems and for conveniently transforming the equations from one coordinate system to another system related to the first in some known fashion. For the present purpose three coordinate systems are used, and it is convenient to begin with a description of the relations among these three systems. FICK LAW FOR KIRKENDALL COORDINATES The reference coordinate system, and the one that is useful for most experimental measurements, is a cartesian coordinate system, xi (i = 1, 2, 3), fixed with respect to some point in the specimen, such as an end of the alloy bar undergoing diffusion. A second set of coordinates, the Kirkendall coordinate system, is one that in principle can be described by the location of inert markers (Kirkendall interfaces). A convenient mathematical relation between Kirkendall coordinates, x'i, and the reference cartesian coordinates, ii, is obtained by specifying that the Kirkendall coordinate system coincide with the cartesian system at time, t = 0. After diffusion has occurred for some time, t = t, the Kirkendall coordinate system will differ from the reference system in the manner shown schematically for the one-dimensional case in Fig. 1. The third coordinate system is Darken's1 local cartesian-coordinate system, xi, which is identical with ii in orientation and units, but which moves with the point under consideration in the Kirkendall coordinate system. Even though most diffusion problems are essentially one-dimensional, there is an advantage in first carrying out the analysis of the three-dimensional problem to gain a clearer insight into the assumptions that are made in the usual one-dimen-

Jan 1, 1962

By ANDREW CARNEGIE

Although the noble building provided in New York City by Mr. Carnegie for the United Engineering Society has been pushed to about half-completion, the ceremony of laying its corner-stone was not performed until Tuesday afternoon, May 8, 1906. The stone lies just back of the southeast corner of the building, on the north side-of West 39th Street. Among those present were Mr. and Mrs. Carnegie, Miss Whitfield, the sister of Mrs. Carnegie, Ralph W. Pope, Secretary of the Institute of Electrical Engineers, Frederick R. Hutton, Secretary of the. Society of Mechanical Engineers, Rossiter W. Raymond, Secretary of the Institute of Mining Engineers, Charles H. Haswell, the first Chief Engineer of the United States Navy (1836-1851), now in his ninety-seventh year, John Fritz, of the Bethlehem Steel Company, William H. Fletcher, President of the Engineers' Club, E. E. Olcott, President of United Engineering Society, and other interested friends. After an inspection of the interior of the building, the group formed about the corner-stone, which had been draped with the American flag. The exercises were opened by Mr. Olcott, who appropriately welcomed Mr. Carnegie, and briefly expressed the essential value of the building, saying, in part " The societies to be housed underneath this roof have as their aim the pre¬serving and putting in tangible form of the records of scientific accomplishments so as to avoid the repetition of mistakes. The possibility of finding the records of these results all at one center, so near the great Public Library of our city, will be an inestimable advantage to all professions. It is an occasion of no ordinary moment, therefore, when we can welcome Mr. Carnegie and have him lay for us the corner-stone of this great building which his liberality has provided." Mr. Carnegie responded in happy vein, thanking the committee for their greeting, and expressing his pleasure. in being able to do what he had done to further so worthy a cause. Among other things, he said

May 1, 1906

By Charles A. Ashburner

DURING the early part of August, 1880, I was directed by Prof. J. P. Lesley, State Geologist, to assume charge of the geology and mapping. of the Second Geological Survey of the anthracite codfields. I visited the region uninaumbered by any instructions other than this,—that I should submit a plan for making the sur-

Jan 1, 1881

By E. H. Mohr

AT the McGill concentrator of the Nevada Consolidated Copper Co., all flotation operations have been carried out in Forrester cells since November, 1926. In respect to cost of operation, the new cell has proved to be superior to the Callow, which it supplanted, and its incorporation in the flow sheet has resulted in a marked improvement in the metallurgy. Before citing the advantages of the new machine over the old, it should be explained that the Forrester has not only replaced the Callow, but it has made possible the elimination of a number of tables as well. When Callow cells were in use, table concentration preceded flotation. The ball mill pulp was elevated, by means of air lifts, to roughing Wilfley tables situated two floors directly above the flotation floor. On an intermediate floor were additional tables which cleaned the concentrate from those above. The finished table concentrate constituted approximately 60 per cent. of the total mill production, and contained about 40 per cent. of the recovered copper. The table tailings were returned to the classifiers, the overflow from which went to the flotation cells and the oversize to the ball mills. As soon as the Forrester cells were installed, this tabling operation was discontinued. The ball mill pulp now discharges into the classifiers direct, without the intermediate tabling. It was impracticable to employ the present flow sheet when Callow cells were in use, for the reason that unless the greater part of the heavy mineral was first removed, it accumulated on the mats and adversely affected the flotation operation. By tabling ahead of flotation, it was practicable to maintain the concentrator at 10 to 20 per cent. greater capacity (depending up on the pyrite content of the ore) than was possible by flotation alone. This was due to the necessity for finer grinding in the latter case. Even though the table concentrates contained only 6 to 8 per cent. copper con- tent, the low smelting costs made it advantageous to operate at high mill capacity, at the cost of low grade of product. STANDARD SECTION EQUIPMENT With the old-flow sheet, a standard section consisted of four ball mills and classifiers, one air lift, 20 roughing tables, 10 cleaner tables, 12 primary

Jan 1, 1928

By H. S. Munroe

AN elaborate discussion under this heading formed a chapter in one of the reports made by Professor Raymond as Commissioner of Mining Statistics.* In a subsequent report- was printed a paper, by Mr. William Main, Jr., of Columbia, South Carolina, containing a theoretical investigation into the effect of the velocity of impact on the effective ditty of stamps. A visit to the Lake Superior copper region last summer suggested an inquiry into the relative efficiency and economy of the enormous steam stamps of the copper-mills, as compared with the results obtained with the cant and tappet stamps commonly used in the West. The atmospheric stamp used at the Phoenix Mill promised to add interest to the inquiry, as giving an example of unusually high speed, this stamp making 160 drops per minute. In introducing his subject Dr. Raymond makes the following remarks, which are quite apropos of the present investigation : "In considering the economical application of stamping machinery, we meet, at- the beginning, with serious difficulties in obtaining accurate data for comparison. The weight and fall of stamps vary as the shoes and dies wear out; and this may lead to a change of speed also. Moreover, defects in engines, boilers, or machinery for the transmission of power, may occasion serious losses, which cannot fairly be charged to the arrangements of the stamps proper. Again, the capacity of stamp-mills is directly dependent, in some degree, upon the nature and extent of discharge, fineness of screens, and other peculiarities of the battery. Finally the hardness and tenacity of the rock crushed varies so much that comparisons between different localities cannot be implicitly trusted. The safest experiments are those made in the same mill, by changing first one and then another condition of working; but this is seldom possible for such * Mineral Resources West of the Rocky Mountains, 1871, p. 380. †- Mineral Resources West of the Rocky Mountains,, 1873, p. 345.

Jan 1, 1881

By F. J. Fayers, R. L. Perrine

For many years the problem of increasing ultimate recovery of oil from a reservoir has been a subject of interest to the oil industry. At present, a standard secondary recovery technique is to flood the reservoir with water once natural forces of the system are depleted. The permeability characteristics of the rock, together with interfacial forces which exist between the two fluids and the porous material. allow only part of the oil in the rock formation to be recovered by the water-flooding process. Laboratory experiments have shown that when detergents are added to the flooding water, the flow properties of oil in a porous rock arc improved. This improvement results in greater oil recovery. Even though higher recoveries are obtained using detergents, the extra cost associated with the method may make it economically unsatisfactory. To establish economic feasibility requires experimental laboratory measurement of fluid and rock properties together with a calculational procedure to predict field results. Pilot tests in the field may also be required. This paper presents a mathematical procedure for predicting detergent flood behavior. A number of reasonable simplifying assumptions are made to obtain a tractable system of equations. The resulting method may be regarded as a generalization of Buckley-Lev-crett' theory to solve simultaneously for water saturation and detergent concentration profiles. Consequently this type of calculation can be used in much the same manner as Buckley-Leverett theory is used to evaluate a water flood. The mathematical method employed is the so-called method of characteristics for solving hyperbolic partial differential equations. This application of the method is instructive because several other problems in reservoir analysis may be analyzed in a similar manner. FLUID FLOW EQUATIONS The flow behavior of oil and water without detergent through porous reservoir rock is usually expressed by Darcy's law and a continuity equation for each phase. If gravitational forces are neglected, vrg = kr (s)µr v p rg.........(1) vrg = kr (s)µr v p rg.........(1) ? pa va = F ?/?t (sd) where v is the volumetric flux, k represents permeability, S is saturation, and P the pressure. Fluid viscosity is denoted by 11, p is the density, 4 is porosity, and I the time. The subscripts w and o refer to water and oil. The capillary forces in the system lead to a difference in pressure between phases. This may be expressed by the relation: Pm -P0 =Pc(S).........(5) The capillary pressure? P,, is determined experimentally as a function of saturation. DETERGENT BALANCE EQUATION Addition of detergent to the water phase affects the flow properties of the system. Capillary pressure and relative permeability become functions of detergent concentration, c, as well as fluid saturation. That is: P--P (S,c) and k,,,.- - -- k,,,. At low oil saturation values, the presence of detergent reduces capillary pressure and reduces the relative permeability ratio. Detergents are surface-active and adsorb on rock surfaces. The quantity adsorbed, a, will depend on the concentration c of detergent solution and may also depend on the saturation; thus, a = a(S,c). In this analysis we have assumed that the detergents used are water soluble but not oil soluble, and their movement is therefore restricted to the water phase. The dispersion of detergent in water is neglected by comparison with transfer by flow within the system. Detergent movement is determined by the water flux and adsorption: ? cv m = -F ?/?t (cs + a) We will assume that the quantity of detergent in solution is too small to significantly change water density or viscosity. When the permeability and capillary pres-

DURING the early part of August, 1880, I was directed by Prof: J. P. Lesley, State Geologist, to assume charge of the geology and mapping of the Second Geological Survey of the anthracite coal-fields. I visited the region unineumbered by any instructions other than this, that I should submit a plan for making the sur- * In the practical application of this method I wish to acknowledge the valu¬able aid rendered by my assistant, Mr. A. W. Sheafer.

Jan 1, 1881

By Richard E. Chism

SAN DIMAS, in the State of Durango, Mexico, on the frontier of the State of Sinaloa, is the centre of an extensive and rich mining region, which has been exploited for over a hundred years; and the patio process for working silver ores has there attained the highest perfection of which it is capable. Local modifications have been engrafted upon the underlying principles of the process, but, as a whole, the San Dimas practice so fully illustrates its typical capabilities, that I have undertaken to describe its workings in the hope of lightening, to some degree, the labors of my professional brethren who may have occasion to visit Mexico." As is tolerably well known, the patio process, like all other systems of free amalgamation, is not successful with ores containing more than a trace of zinc or lead, the presence of zincblende being especially obnoxious. Iron and copper in small quantities are not particularly disadvantageous. The process succeeds very well with all sulphide ores which do not contain much more than a trace of arsenic and antimony, provided the tailings are concentrated, although, of course, it is best adapted for free milling ores. For suitable silver ores that contain small amounts of free gold the process is still a good one, but where the gold is combined with sulphurets, a considerable and even an excessive loss is inevitable. Hitherto the Mexicans have submitted to this loss, but, since the introduction of American mills, they are gradually abandoning the patio process in favor of the other. The San Dimas ores have a gangue of quartz and feldspar. They are composed principally of silver sulphides, with some chloride and

Jan 1, 1883

By H. C. Chao, Y. E. Smith, L. H. Van Vlack

ThE phase relationships for the MnO-MnS system have been investigated only in the eutectic region. wentrupl reported a eutectic at 1280°C (2345°F) with approximately 50 wt pct of each component, as based on the earlier work of Andrew, Maddocks, and Fowler.2 More recently silverman3 corrected these figures to 2275° ±10°F (1246°C) with 63 wt pct MnS and 37 pct MnO. Neither Wentrup nor Silverman investigated the solid-solution limits in this system. However, Wentrup did suggest with his phase diagram sketch that the maximum solubility of MnS in MnO is 10 wt pct, and the solubility of MnO in MnS is nearer 20 wt pct, Fig. 1. These figures have been utilized in subsequent publications without further verification.4 There had been evidence found in this laboratory that the above solid-solution figures were high. An investigation was therefore conducted using the following procedure. Samples containing MnO and MnS were contained in platinum foil, heated just above the eutectic temperature in a purified nitrogen at- mosphere, and quenched into distilled water. The MnO had been prepared by calcining reagent grade MnCO3 in nitrogen at 1400°C. Only MnO was detected in subsequent X-ray diffraction analyses. The MnS had been prepared by sulfur deoxidation of reagent grade MnSO4 according to the reaction: MnSO4 + S2 ? MnS + 2SO2 The details of the sulfide preparation procedure, which utilized atmospheric sulfur pressures at 950°C, are discussed elsewhere.5 The sulfur content of the sulfide was determined to be 36.8 * 0.2 pct, which matches the stoichiometric value of 36.9 pct. No evidence of either MnO or MnSO4 was detected microscopically or by X-ray diffraction. The single-phase combinations of MnO and MnS at the eutectic temperature indicate the limit of solid solution as shown in Fig. 2(a) and (c), and the revised phase diagram is shown in Fig. 2(d). The melting temperature for MnO is that provided by Glasser.6 The eutectic temperature of 1232° ± 5°C and eutectic composition of 64 wt pct MnS are in close agreement with Silverman's correction of Wentrup's work. The maximum solubility of MnO in MnS was determined to be 1.7 ± 0.2 wt pct. The maximum solubility of MnS in MnO was determined to be 1.8 ± 0.2 wt pct. These figures represent the lower limit for the presence of liquid at 1260°C and are significantly lower than the earlier estimated solid-solution figures. The authors wish to acknowledge the support of U.S. Steel's Edgar C. Bain Laboratory for Fundamental Research. The comments and critical suggestions of Drs. A. S. Keh, R. Rickett, and R. B. Snow are appreciated.

Jan 1, 1963

Executive SIDNEY J. JENNINGS, Chairman GEORGE D. BARRON J. E. JOHNSON, JR. EDWIN LUDLOW ROBERT M. RAYMOND Membership. EARL EILERS, Chairman. LEWIS W. FRANCIS J. E. JOHNSON. JR. LOUIS D. HUNTOON ARTHUR L. WALKER Finance GEORGE D. BARRON, Chairman CHARLES F. BAND BENJAMIN B. THAYER Library E. GYBBON SPILSBURY,1 Chairman ALEX C. HUMPHREYS3 GEORGE C. STONE2 J. H. JANE WAY4 BRADLEY STOUGHTON Papers and Publications BRADLEY STOUGHTON, Chairman

Jan 8, 1918

By Ernest R. Lilley

While American scientific literature contains much information upon geologic conditions controlling the production of oil in Rumania, copper in Chile, and other fuel and metallic resources in many foreign countries, it is singularly lacking in data about the nonmetallics outside of the United States. Thus, though the United States is the outstanding market for European high-quality refined kaolin, and for the chinaware, porcelain, and other products of the European ceramics industries, American literature contains only the briefest references to the deposits from which the raw kaolin utilized is obtained. To the writer, to whom has come in the past year the opportunity of visiting a number of these deposits personally, they have proved of extreme interest both commercially and geologically. It is the latter phase that is discussed in this paper. The older and now largely crystalline rock areas of France, Germany, and other parts of western Europe contain numerous pegmatite dikes of which the upper portions have been subjected to surface weathering and kaolinization in much the same way as those of the eastern portion of the United States. Like the latter, the European pegmatite kaolins have long been known for their freedom from iron and other impurities offensive to the china and porcelain manufacturer. Unfortunately, they are also, like the American deposits, individually of small size and noted for their high costs of production. Deposits of sedimentary clay similar in many respects to the high-quality sedimentary kaolins of Georgia and South Carolina are known and worked, notably in southern Germany and in the Newton Abbott district of Devon and Dorset in England. In general, their relationship to the parent rock from which they were derived is more evident than in the United States and the individual deposits are of smaller areal extent and less regular in outline. While these deposits are of considerable economic importance they did not, because of their similarity to deposits in America, attract and hold the interest of the writer to the extent that several other types of deposits did. It is to the latter, which are so different from the kaolin

Jan 1, 1932

By B. M. Larsen

SEVERAL articles have recently been published discussing the conditions necessary for accurate measurements of temperatures in the open-hearth steel furnace. In the course of a study of refractories service conditions in steel furnaces, the present writers have taken tempera; tunes in several open-hearth shops in the Pittsburgh district. The conclusions, as to conditions necessary for accurate measurements of temperature, are somewhat at variance with those of other investigators. The subject is closely connected both with the close-control of steel-making and the prevention of overheating of the silica refractories used in roofs and walls. It is becoming more and more important to obtain furnace temperatures of fairly definitely known accuracy. At present, the most useful instrument for such measurements is the disappearing-filament type of optical pyrometer. This method of measurement has formed the basis of most other discussions on the. subject and was also used by the writers.

Jan 8, 1926

By Richard P. Rothwell

REVOLING slime-tables with stationary sprays and oscillating brushes have for many years been a favorite apparatus used for working slimes in German dressing-works, often displacing Rittinger tables and the many variations of Cornish buddles. The difficulty of building these tables larger than 5 1/2 meters (17 feet) in diameter, increasing the cost and making them unwieldy, rendered it necessary also to concentrate the slimes in several operations, because the travel over so short a length of hearth would not suffice for close concentration. A preliminary sizing is effected in a system of spitzkasten. Herr C. Linkenbach, general manager of the Ems Lead and Silver Works, Germany, devised a buddle, in 1878, which has since worked well and found much favor in Germany, and has been in one instance copied here, at Colorado Springs, without any credit having been given to the original inventor. Linkenbach's plan has been to reverse the functions of the table and the washing apparatus of the old German revolving table. He makes the tables stationary and rotates the washing apparatus,, thus enabling him to save in power, and, within certain limits, to increase the dimensions of the table, without in any way affecting its durability or materially increasing its cost. In its earlier form, the buddle was single, and that type is still

Jan 1, 1883

By F. W. Bloecher

D ETERMINATION of the surface area of finely divided minerals is of interest to mineral engineers engaged in flotation, comminution, and dewatering studies. In the industrial minerals field, many materials are classified as to fineness according to their specific surface (surface area per unit weight). A method of surface area determination has been tested and used in the Richards Mineral Engineering Laboratories at M.I.T. It involves low temperature krypton adsorption measurements using the technique described by Beebe.1

Jan 3, 1951

By I. Cornet

With the greatly expanding use of magnesium during the war, it appeared necessary to the War Metallurgy Committee that the notch sensitivity of magnesium alloy extrusions be further investigated and the influence of various factors upon notch sensitivity be noted. Accordingly, the National Defense Research Committee of the Office of Scientific Research and Development placed a research contract with the University of California, supervised by the War Metallurgy Committee. The work discussed herein was done under "Restricted" Project NRC-21, reported in Dec. 1943~; it has been released for publica-tion by the O.S.R.D. Scope of the Investigation The notch sensitivity of various magnesium alloy extrusions was determined under axial tension, and also under several conditions of nonaxial tension. Hardness, grain size and other metallographic features were observed; stress-strain data were obtained, and the chemical compositions of the alloys were determined, in order to correlate these quantities with thc notch sensitivity. Notch sensitivity under axial tensile load was determined for a few specimens which had been cold worked to various degrees by tensile prestraining. Magnesium alloy extrusions studied included Dowmetal 0, X, J, and A(. For comparison, extrusions of aluminum alloy 24s-T, cast bars of aluminum alloy 122-T2, and cast bars of magnesium alloy C were also tested. The specified chemical composition of these alloys is given in Table I. All bars tested were within specification limits of composition. Investigation of thc tensile notch sensitivity of various magnesium alloy extrusions, under conditions of axial and eccentric load, showed little or no correlation with stress-strain or other conventional data. Since the many uncontrolled variables present might mask significant relationships, one alloy was selected for intensive study. Magnesium 0 alloy extrusions were subjected to experimental heat treatments, and the ,Changing hardness, tensile strength, microstructure, and notch sensitivity observed. Experimental Techniques and Procedures Tensile Testing Bars used for axial loading were machined with % in.- and with 34-in. minimum diam1 and included specimens with 60" V notches (Fig I and 2). Each V-notched specimen was roughed out carefully and then finished with a honed tool. These Y-notched bars were sampled frequently, sectioned, polished, and examined at 500 X magnification to control

Jan 1, 1949

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

[Admissions: Aurel E. Smith, Chairman Edmond F. Egan Lawrence S. Fennell John S. Fuller Howard J. Ritts, Jr. Gene E. Roark Kenneth W. Robbins Ben M. Gottlieb Advertising: Bernard F. Klein, Chairman Henry N. Lyle R. E. Howard H. M. Krause, Jr. Mrs. Evelyn R. Robertson]

Jan 1, 1961