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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 C. Norman Bowers, Blaine B. Wescott

MARKED improvement in the serviceability of sucker rods has been effected in the last two years, partly because of the insistent necessity for greater economy in the operating costs of crude oil production growing out of the general industrial depression and partly because many of the recently developed fields have imposed more severe operating conditions upon both surface and underground equipment. The latter is particularly true of Kansas, where practically all of the oil produced. is associated with damaging amounts of hydrogen sulfide brine and where the method of establishing potential production demands equipment capable of being operated at maximum capacity without interruptions. The decline of flush production in the Oklahoma City field created new problems in deep-well pumping on a scale heretofore unequaled and the increased proportion of water it has been necessary to produce in the fields of the Greater Seminole area presented conditions that were acutely in need of betterment. The problem in the latter fields was complicated by the shift towards sulfide characteristics, which accompanied water encroachment, and it is probably true that nowhere, at the present time, are pump¬ing conditions generally as severe as in this territory. The Mid-Continent district, therefore, has become the proving ground for the numerous materials that have been proposed for sucker-rod fabrication. The information that ultimately will be obtained from an unprecedented amount of field experimentation will pay ample dividends when the decline of East Texas increases the demand for the vast reserves of sour crude in West Texas. It is a rare occurrence in industry that the use of such a simple piece of equipment as a sucker rod presents so complicated a problem for solution. As proof of this, it is only necessary to consider the numerous types of sucker rods on .the market at the present time and contrast this condition with that of less than four years ago, when it was the common aim of manufacturers to develop a single sucker rod for all conditions of

Jan 1, 1935

By E. B. Burwell, R. H. Nesbitt

Designed by army engineers, the NX borehole camera provides the most economical method of subsurface exploration so far devised. Continuous cylindrical color photographs now reveal minor flaws in foundation bedrock not always disclosed by borehole samples. A unique projector transforms the photographs into true-to-scale images of three dimensions. ANEW milestone in the progress of photography and subsurface exploration was reached when the Chief of Army Engineers announced the development of the NX borehole camera. In obtaining continuous undistorted cylindrical color pictures of dry or water-filled borings the device surpasses all other cameras designed for photographing interior surfaces of pipes, wells, and conduits. The usefulness of the camera and the unique projector that comes with it are at once apparent. To the geological, mining, and civil engineer alike it signifies the end of guesswork with respect to underground conditions that have eluded identification by conventional core-drilling methods. To the medical profession it may well signal new progress in photo optics which could result in cylindrical color photographs supplementing the X-ray and existing photographic methods used in exploratory surgery. The pilot model of the camera has more than paid for itself as a result of its success in bringing to the surface at two dams information previously obtainable only by costly drilling of mansized boreholes for subsurface on-the-spot examination. Such bores cost as much as $200 per lineal foot as against $10 per ft for the conventional 3-in. or NX exploratory core borings from which the present invention derives its name. The NX camera can now photograph completely the interior surface of these borings. Research and development for the first camera and projection equipment were conducted by Engineering Research Associates, Division of Remington Rand, Inc., under the technical supervision of the Geology and Geophysics Branch, Office of the Chief of Army Engineers in Washington, in accordance with plans and specifications furnished by this branch. Subsequent modifications of the camera-lowering device, transporting equipment, and special field tools were made in the Corps of Engineers' Ohio River Division Laboratories in Cincinnati. The background of this development is interesting. Among the more difficult foundation problems involved in construction of concrete dams are those resulting from bedrock imperfections that escape disclosure by conventional exploration methods. Often these imperfections are of sufficient magnitude to introduce costly changes, especially when their presence is discovered only after foundation excavation is well in progress. Bedrock flaws most frequently camouflaged may be ruptures resulting from the enormous stresses to which rocks have been subjected, or they may be planes or zones of weakness related to chemical alteration and underground erosion. Obviously, detailed information on their location, dimensions, and structure is important, as these factors can affect the stability of a dam and the security of life and property downstream. Their discovery and appraisal entail extensive subsurface exploration. At present the most economical exploratory tool available to geologists and engineers is the small-diameter diamond core drill by means of which cores of the foundation bedrock are recovered for examination and testing. All too often, however, these samples fail to disclose minor foundation flaws that may be of major importance before a structure is completed. As a result, the small-diameter drillings are supplemented generally by more reliable but much more costly shafts, tunnels, or large-diameter calyx drill holes that permit the investigator to examine the foundation rocks in place. It was to reduce the number and cost of these expensive and time-consuming investigations, as well as to obtain more complete information on rock structure from the smaller borings, that the NX borehole camera was developed. That it has been eminently satisfactory in accomplishing that purpose is demonstrated by its success most recently at the Folsom dam, under construction on the American River, 23

Jan 1, 1955

By P. H. Thornton

MaNY intermediate phases are solid solutions which have a solute-solubility range greater than 3 at. pct. These phases, which are generally very strong and often have simple crystal structures, are usually extremely brittle so that specimens of simple shape cannot be produced by the usual mechanical-deformation techniques. Furthermore, single crystals of reasonably uniform composition are difficult to grow by the Bridgman technique because the phases generally form by a peritectic reaction, which causes pronounced segregation. In this note, a technique is described for the preparation of thin-rod specimens of brittle intermediate phases, which may be used for physical-property studies such as resistivity changes' and for the conversion of such rods into single crystals. The method has been used for the preparation of rod single crystals of the phases and Ingots, of about 100 g weight and 11 mm diam, were made by melting together the appropriate amounts of high-purity materials (usually 99.999 pct) in sealed

Jan 1, 1967

By J. B. Hiskey, G. Ramadorai

This paper presents the kinetics of leaching pure wulfenite (PbMoO,) with sodium sulfide solutions. Wulfenite dissolves in the presence of sulfide ion according to the following reaction: PbMoO , + S= PbS + MOO;. Synthetic galena is formed and molybdenum is released to solution as molybdate ion. The reaction follows the shrinking core model and the leaching mechanism involves mixed kinetics where both diffusion and chemical reaction are rate controlling. Molybdenum extraction is explained in terms of temperature, particle size, and sodium sulfide concentration.

Jan 1, 1977

By L. Moussoulos

Pyrite concentrates produced at the Olympias mines, Northern Greece, show an unusually high gold and silver content (16-20 and 25-40 ppm respectively), associated with the presence of arsenopyrite; their high As content (5-8%) has hindered their utilization so far. In the present paper a simple and environmentally safe method that permits their complete utilization for the production of SO2 gas, As203, and the recovery of Au and Ag is described. According to this method, the pyrites are subjected to a single-stage oxidizing roasting in a fluid bed reactor. The precious metals, and approximately 45% of the contained As, remain with the cinders, while the rest of the As is removed with the SO2 - bearing gases and can be recovered by suitable treatment. The gases, after further cleaning, can be utilized for the production of sulfuric acid.

Jan 1, 1984

By C. W. Schulties, W. J. Mallio, L. J. Petrovic, J. A. L. Campbell

Roof control comprises about 35% of direct and indirect underground mining costs. In addition, difficulties in estimating roof control costs for new areas lead to the greatest uncertainties when negotiating coal contracts. And obviously, coal cannot be mined if the roof can't be held. Accordingly, there are strong incentives to attack this problem on as many fronts as possible. One successful geological modeling technique for predicting future roof conditions was recently applied at Peabody Coal's Simco mine No. 5, located in Coshocton, Ohio. Benefits derived from it included: - A better identification of areas where poor safety conditions may be encountered. - Improved roof control cost estimates for contract negotiations. - Estimates of time-duration while mining in bad roof areas. - Labor and materials cost predictions in an existing mine. - Productivity increases through prior knowledge of areas to avoid.

Jan 10, 1975

By C. Richard Tinsley

Mineral economists debate whether to call the deep-ocean nodules "manganese nodules," "nickel nodules," "polymetallic nodules," or even "ferro-manganese nodules." It is nickel and copper that are generally regarded as the main targets in the nodules. Processing considerations are thought to virtually dictate that Deepsea Ventures will produce high-purity manganese metal (at least if it follows a hydrogen chloride leach), whereas other groups have been focusing on the selective extraction of copper, nickel, cobalt, zinc, and molybdenum, while rejecting manganese to tails. Solvent extraction appears to be the primary multimetal extraction technique (except for manganese). These processing considerations indicate that metal production f, or Deepsea Ventures is essentially a co- product system (manganese recovery is necessary to recycle chloride ions) while the other groups can more easily approach the metals as selective co-products (e.g. recovering nickel and copper, and rejecting cobalt). Some zinc may be produced as a co-product, as it may have to be removed in the solvent extraction process.

Jan 4, 1975

By M. D. Cooper

Production of both anthracite and bituminous coal in 1954 was about 16 pct below 1953. Estimates on Dec. 1, 1954, indicated 27 million tons of anthracite and 385 million tons of bituminous. Decline in production was due principally to lower demand by the steel industry and the railroads, although competition from other fuels also affected coal. The year was notable for vigorous effort by the coal industry to promote the use of its product. A Cabinet Committee on Energy Supplies and Resources Policy and an Interdepartmental Committee on the Soft Coal Industry were set up by the Administration in Washington. A Governors' Fuel Conference was also organized.

Jan 3, 1955

By Harry Bapty

LONGHOLE drilling with a heavy type percussion Leyner drill, jointed steel rods, and a tungsten carbide insert bit was investigated while drilling and working a quartz barite brecciated rock. Procedure and practice were developed and its suitability for tackling pillar and sill recovery proven and extended to regular stoping at Torbrit. Torbrit, as the name implies, is a contraction of the Toric property and the Britannia Mining & Smelting Co. Ltd., the former owners. This silver property, with minor amounts of lead, zinc, and rarer sulphides of little or no economic value, was discovered in 1916 from an outcrop in the Kitsault River, 18 miles north of Alice Arm Post Office, in the Portland Canal Mining District, B. C.

Jan 11, 1954

MORE than 2500 members of the AIME from all sections of the U. S., Canada, Central and South America are expected to attend the 175th General Meeting scheduled for Los Angeles Feb. 16 to 21, 1953. The Southern California Section will be host for the meeting. It will be the first time the Annual Meeting has been held in Los Angeles. In keeping with the historic nature of the event, headquarters will be the fabulous Statler Hotel, recently opened in downtown Los Angeles. Meeting plans are under the direction of Henry T. Mudd, General Chairman, assisted by members of the Southern California Section, headed by Basil P. Kantzer. The annual business meeting is scheduled to be held Tuesday, February 17, at the Statler Hotel, at 4 pm. Minerals Beneficiation Div. has planned a very important program, with 10 technical sessions, the famous Scotch Breakfast, divisional luncheon, and participation in the Mining Branch and All-Institute activities. The MBD business meeting is set for the morning of Feb. 16, 1953.

Jan 1, 1952

By J. A. Herbst, J. L. Sepulveda, J. D. Miller

Lead cake, a zinc smelter flue dust residue, consists primarily of lead sulfate. Characteristic properties of lead cake were determined in order to aid the understanding of reaction mechanisms involved in bismuth removal from lead cake by sulfuric acid digestion. Sp gr (specific gravity) measurements, surface area measurements, and photomicrographs revealed that the particles of lead cake are quite porous and seem to consist of an agglomeration of submicron grains (0.4 pm) fused together in a manner similar to cement clinker. Analysis of experimental rate data, which was independent of particle size, indicates that the dissolution reaction involves two distinct, rate limiting steps. The initial stage of reaction appears to be limited mainly by intergranular diffusion of the reactant, hydrogen ion, while the latter stage of reaction appears to be controlled by diffusion of soluble reaction products through the reaction product layer of the individual grains.

Jan 1, 1979

By E. P. Klier

The work of Klier and Lyman1 on the bainite reaction has led to the full description of this reaction for medium-carbon low-alloy steels. Certain experimental data reported by Klier and Lyman appear, however, to be improbable of obtaining in very high-carbon steels. The study herein reported consists of an analysis of the transformation characteristics of a 3 per cent chromium, I per cent carbon steel by means of X-ray and metallographic methods. From the results obtained it is concluded that the bainite reaction in this steel is more complicated than that reported by Klier and Lyman for the low-carbon low-alloy steels. Henever, the mechanism of bainite formation in this steel appears to be essentially the same as proposed for the low-carbon low-alloy steels with the modification that the first volumes to transform are carbon-rich rather than carbon-poor. Experimental Procedure The analysis of the steel studied was: Cr, 2.89; C, 1.02; Mn, 0.33; Si, o.35; S, 0.012; P, 0.020. The stock was received from the Carpenter Steel Co. in rolled bars. Specimen Preparation Specimens were austenitized at 1200°C. (2192°F.) for 25 min. in purified nitrogen. The resultant A.S.T.M. austenite grain size was 0-1. Isothermal transformation was allowed by quenching the specimens into liquid metal baths controlled to 5°C. at 540°C. (1004°F.) and above, and to 2°C. at 490°C. (914°f.) and below. Following the desired degree of transformation all specimens were water quenched. Metallographic Examination Specimens 1/4 in. round by 1/4 in. were used for nietallographic examination. Etch-ants used were Vilella's reagent (I gram picric acid, 10 ml. hydrochloric acid to make 100 ml. ethyl alcohol solution) and alkalinc sodium picratc (electrolytic). Vilella's reagent was effective in revealing all microconstitucnts, while the alkaline sodium picrate developed the carbon-rich structures or carbides only. X-ray Examination Two X-ray techniques were used—the Debye-Scherrer method and a back-reflection method. 'The small specimens necessary for the Debye-Scherrer method were austenitized and then allowed to transform, or were cut from the larger metallographic specimens. The metallographic specimens were used for the back-reflection X-ray analysis. When it was desirable to determine the structure of the carbide present, sliver specimens were electrolytically etched to develop a carbide coating, then were exposed in the cameras. This technique was frequently necessary to allow positive identification of the carbide.

Jan 1, 1945

By B. D. Cullity, S. S. Hsu

The stress distribution at the surface of a twisted cylinder is analyzed along the boundary of a slip plane of arbitrary orientation and this analysis is applied to the torsion of cylindrical crystals of magnesium. A criterion for slip is developed and the critical resolved shear stress of magnesium in torsion is found to be 0.038 kg per sq mm. The mechanism of torsional deformation in magnesium and aluminum is described, as well as the relaxation of a twisted crystal at elevated temperatures. THERE has been considerable fundamental study A of the mechanism of slip occurring during deformation in tension and compression but comparatively little attention has been paid to the mechanism of torsional deformation. This paper is concerned with the way in which a single crystal deforms in static torsion and with the phenomenon of untwisting which a twisted crystal undergoes during annealing. Particular attention is paid to the application of the critical resolved shear stress law to torsional deformation. Probably the most likely mode of torsional deformation that can be imagined consists of rotation of one part of the crystal relative to another on the active slip plane. Here the most interesting feature is the slip direction. If a cylindrical single crystal is twisted about its axis and if, to consider the simplest case, the active slip plane is normal to the specimen axis, then the direction of gross slip at any point must always be at right angles to the radius drawn to that point. It follows that the crystallographic direction of slip must be continually changing, in sharp contrast to slip in tension which occurs in a crystallographically constant direction. Extensive investigations of slip in torsion have been made by Gough and his associates.' They made torsional fatigue tests on metal single crystals belonging to a number of different crystal systems and observed, with a microscope, the appearance of slip lines on the surface and of strain markings on the transverse cross section of cylindrical specimens. They concluded that the critical resolved shear stress law was just as valid in torsion as in tension, in the sense that slip occurred on that plane and in that direction in which the resolved shear stress was a maximum. They also established that the operative slip planes and directions were the same as in tension. They did not, however, measure the critical resolved shear stress in torsion nor, in fact, did they establish that a critical value of the resolved shear stress was necessary for the initiation of slip. Their investigations were, moreover, restricted to torsional fatigue tests which necessarily involve small strain amplitudes. Wilman,' studying crystal growth and the abraded surfaces of crystals, observed crystal fragments

Jan 1, 1955

By R. Adair, W. R. Hudspeth, W. T. McDaniel

ANEW method for concentrating the flake mica either from present washing plant tailings or from new feed has been developed. In this paper, flake mica refers to that which occurs in weathered granites, alaskites, pegmatites, and schists in a form too fine to be considered sheet mica. It ranges in size from 1 in. or more down to 200-mesh or finer and occurs with kaolin, quartz, and partially kaolinized feldspar. Scrap mica, a term often used indiscriminately to describe everything other than sheet mica, will be used to denote the waste product from sheet mica mines and fabricating plants. Both flake and scrap mica are used in the mica grinding plants to produce wet-ground or dry-ground mica, although some flake mica recovered from clay mining operations is fine enough to be marketed without grinding. Until 1930, ground mica was made almost entirely from scrap. From 1930 until 1935 a gradually increasing amount of flake mica was mined, and most of this was sold without grinding. A large percentage of this mica was recovered from clay washing plants. In this type of operation the recovery of any sheet mica was .of secondary importance and was considered a byproduct. North Carolina produces more flake mica than any other state, accounting for 73 pct of the total domestic production.' In the following review of current practice in jig plants, there is no intention to disparage these operations. Within the limitations under which they were built, they are examples of mechanical ingenuity. The term jig plant is a carryover from early practice since there are no jigs in operation at the present time. Current practice, as shown in Fig. 1, is based on successive stages of differential crushing with rolls followed by trommel screens to remove the more easily crushed gangue minerals. The oversize mica product then is usually dried, and passed through another set of dry rolls and a final screen to remove the remainder of the grit. This process is effective in recovering up to 50 pct of the mica in the original ore, the balance being lost in the screen undersize, usually —% in. Jigs and tables were at one time used to treat this screen undersize and were capable of recovering a part of the mica larger than about 60-mesh.V ine mica lost in these plants is normally washed away in streams and can be considered irrecoverable. There are ten or more washing plants in the North Carolina area that are losing approximately 50 pct of the mica in the feed. Since the three cooperating agencies, the Asheville Minerals Research Laboratory of North Carolina State College, the North Carolina Dept. of Conservation and Development, and the Tennessee Valley Authority, are concerned with conservation of minerals, they have investigated means for improving the efficiency of these mica plants. The mica industry has been cooperating fully with the laboratory to establish a more efficient method of recovery for flake mica. Choice of Methods The initial investigation was concentrated on finding a means of reducing the losses from plants now using the conventional flowsheet shown in Fig. 1. To accomplish this it would be necessary to collect the screen undersize products through the plant and remove from them the mica from Vs in. down to

Jan 1, 1952

By O. B. Bennett

WHEN diamond drilling was introduced in the Rhokana mines in 1939 it was used principally for pillar removal and for completion of the upper portions of shrinkage stopes which were being affected by increasing pressure. This method of drilling long blastholes proved so successful that it was extended gradually to cover stoping, pillar recovery, and hanging cave work. By 1949 virtually all the production of Mindola and Nkana was being obtained by this method. At the present time 87,500 ft are drilled each month by the 80 diamond drills in daily operation. Responsibility for control and issue of diamond drilling equipment and crowns, as well as tabulation of all performance figures, was taken over by a specially formed Roto drill department, which also investigated the problems encountered with this new method. To assist this department a fully equipped test chamber, Fig. 1, was established underground where performances of various types of machines and equipment could be studied under conditions as nearly uniform as possible.

Jan 12, 1954

By George E. Aiken

Subzero temperatures of the Arctic pose some critical engineering problems for the developer and operator of open pit mines. Undoubtedly, the single most troublesome manifestation of this climate is permafrost. Underlying about 20% of the world's land area and 85% of the state of Alaska, permafrost has not only made its impact on building construction and mine excavation, but has created a legitimate threat to the delicate balance of nature existing within the Arctic environment. The recognition of permafrost areas by geomorphology and an understanding of its other complex developmental factors are the basis for two major concepts in building construction. The active method involves the eventual thawing of the complete permafrost section and is only useful in shallow areas. However, in some areas of coarse, well-drained material, vegetation may be stripped well ahead of construction and shallow permafrost allowed to method, leaves the perenially frozen ground undisturbed and is to be preferred. In selecting construction sites aerial photos may clearly reveal typical permafrost features.

Jan 5, 1972

By Voyle R. McFarland, Robert A. Burmeister, David A. Stevenson

The distribution of lead between phases in the Ag-Sb-Te system was studied using microautoradio -graphy. Two compositions were investigated, both containing an intermediate phase Known as silver antimony telluride as the major phase, and one containing AgzTe and the other SbzTes as the minor phase. For both compositions, two thermal treatments were used: nonequilibrium solidification from the melt and long equilibration anneals of the as-solidified structure. For each composition, lead was segregated in the minor phase of the as-solidified structure, but was distributed in the matrix after anneal. The electrical resistivity and carrier type were insensitive to the distribution of lead in the two-phase structure. ThERE has been considerable interest in the Ag-Sb-Te system because of its thermoelectric properties. The major interest has been in compositions on the vertical section between AgzTe and SbzTes, particularly the 50 mole pct SbzTes composition AgSbTez (compositions are conveniently expressed as mole percent SbzTes along the AgzTe-SbzTes section). One of the major problems in the proper evaluation and utilization of this material is the inability to control the electrical properties through impurity additions: all alloys prepared to date have been p-type, even with the addition of large amounts of impurities. It has been shown Wit all the compositions previously studied contain an intermediate phase of the NaCl st'ructure as a major phase (denoted by b) and a second phase, either AgzTe or SbzTe3, as a minor phase.'-3 One explanation for the unusual electrical behavior of this material is that the impurity additions have a higher solubility in the second phase than in the matrix; the impurity would segregate to the second phase, leaving the bulk matrix essentially free of impurity.4 In order to investigate this mechanism with a specific impurity element, the distribution of lead between the two phases was determined using autoradiography. Lead 210 was chosen because of the suitability of its 0.029 mev 0 particle for autoradiography and also because of the interest in lead as an impurity in this system.5'6 EXPERIMENTAL PROCEDURE Two compositions were taken from the vertical section between AgzTe and SbzTes, 50 mole pet SbzTes (Viz. AgSbTez) and 75 mole pct SbzTes, in which AgzTe and SbzTes appear, respectively, as the minor phase. Lead containing radioactive lead (pb210) was added to the above compositions to provide a concentration of 0.1 wt pct Pb. The material was placed in a graphite crucible in a quartz tube which was then evacuated and sealed. The samples were melted and solidified by cooling at a rate of 8°C per min and then removed and prepared for microa~toradiography. After autoradiographic examination of these samples, they were again encapsulated and annealed in an isothermal bath at 300°C for a number of days and prepared for examination. An alternate method of preparation employed a zone-melting furnace; the molten zone traversed the sample at a rate of 1.2 cm per hr and the solid was maintained at a temperature of 500°C both before and after solidification. This treatment had the same effect as solidification at a slow rate followed by an anneal for several hours at 500°C. In order to obtain the best resolution, thin sections of the alloy were prepared by hand lapping to a thickness of approximately 20 p. Other samples were prepared for examination by lapping a flat surface on the bulk sample. The resolution, although somewhat better in the former procedure, was adequate in both instances and the majority of the samples were treated in the latter fashion. A piece of autoradiographic film (Kodak Experimental SP 764 Autoradiographic Permeable Base Safety Stripping Film) was stripped from its backing, care being taken to avoid fogging due to static-electrical discharge. A small amount of water was placed on the sample, the film applied emulsion side down on the surface of the sample, and the sample and the film dipped into water in order to assure smooth contact. After drying, the film was exposed for 2 to 5 days, the period of time selected to give the best resolution. The film was developed on the specimen and fixed and washed in place. Two major factors must be considered in establishing the reliability of an autoradiograph: the in-

Jan 1, 1964

By S. Frederick Ravitz

FOUR liquids are ordinarily present in the lead blast furnace during lead smelting. At the bottom is the lead bullion, which is metallic lead containing about one per cent of impurities, including gold, silver, copper, bismuth, arsenic and antimony. Above this is the speiss, which consists essentially of arsenides and antimonides of iron and copper. The speiss is followed by the matte, which consists principally of sulfides of iron, copper and lead1. The top layer is the slag, of which the major constit-uents are silica, lime, alumina, zinc oxide and iron oxide. Similar products are obtained from the dross furnace, which treats the dross obtained in decopperizing lead bullion. The distribution of gold and silver among these various products is of considerable importance in the smelting of lead. In general, the matte and speiss cannot be treated in the lead smelter, and usually are sent to a copper smelter. It is usually desirable, therefore, to keep their gold and silver contents as low as possible, and to collect the precious metals in the bullion. If the bullion, speiss, matte and slag exist together in equilibrium, the gold and silver should distribute themselves among these four liquids in a definite manner, which, other conditions being equal, should depend only on the amounts of gold and silver in the charge to the furnace. It is thus apparent that a knowledge of whether such equi-librium exists is necessary before attempting to study the effects of various compositions of matte and speiss on the distribution of gold and silver among the furnace products2. Moreover, systems consisting of four liquids in equilibrium are very rare, and are of considerable scientific interest.

Jan 1, 1936

By John T. Schamaun

Recent applications of explosives and blasting agents to rubble rock have led to requirements for more elaborate design and analysis methods. In most blasting uses, it is necessary not only to fracture the rock, but also to move the broken rubble in a predictable manner. Many in situ extraction techniques require rubblization to take place in a confined region where rock motion is a predominate factor in creating a permeable broken bed. In this paper, two analytical methods are presented which describe the large rubble motion during blasting. These methods provide the blast designer with a tool for evaluation and further refinement of blasting patterns and timing sequences. In both these methods, the rock medium is represented by a series of discrete, discontinuous regions. The use of discontinuous techniques rather than the classical continuum methods, results in better approximations to the rubble motion. These regions are set in motion by pressure loads from the explosive. The motion of these regions is then calculated numerically using interaction laws between regions in contact. The basis for these models or methods is presented along with the background for selecting explosive pressure loads and rock mass material behavior. Typical examples, including both cratering and bench blasting geometries, are discussed which illustrate the use of these models to predict rubble motion. Such engineering representations appear to provide a practical method for use in predicting rubble motion and a tool for design evaluation of blasting in confined geometries.

Jan 1, 1984