Search Documents

By Charles L. Thomas

A novel, highly sensitive, and reproducible nzetlzod for the determination of hydrogen in solid materials is presented. The procedure requires equilibration of the specimen with hydrogen gas, rapid quenching, and hot vacuum extraction of the dissolved gas with subse-quent quantitative analysis by mass spectroscopy. Good linearity is obtained for the Arrl~enius plots of the investigated metals. The advantages in the use of this method over that of Sieverts aye discussed. The solubility data for copper are in reasonable agveewzent with a considerable number of other inuestigations, wllile those fov silver are considerably lower than previously reported. The first known solubility data for gold are presented. Solubility equations and heats of MUCH of the data which are available on the solubility of hydrogen in various metals and alloys have been obtained by the classical Sieverts method.' The method involves the measurement of a decrease in pressure of a gas in a calibrated system, and the calculated contraction in volume is attributed to the solubility of the gas in the metal sample. The procedure requires several corrections, such as the solubility of the gas in the container walls and the diffusion of the gas through these walls, as noted by Steacie and .Johnson2 and others. In addition, errors may be incurred due to reactions between metal surface impurities, such as oxides, and the saturating gas. The precise calibration of the measuring system where large thermal gradients exist can present additional difficulties. Also, accurate volumetric measurements of small quantities of gas are difficult. Many of the objections to the Sieverts method were overcome on solid materials by Ransley and ~eufeld,~ who first saturated the metal with hydrogen and performed a subsequent extraction and measurement of the gas by chemical means. Eichenauer and pebler4 and Eichenauer, Kiinzig, and pebler5 measured the diffusion coefficient and solubility by following the degasification of a sample as a function of a rate of increase in pressure in a previously evacuated system. Here again, however, the procedure involves many of the corrections of the Sie-verts method. The present investigation deals with the solubility of hydrogen in solid copper, silver, and gold by a technique which eliminates many of the aforementioned corrections and possible errors. This procedure requires equilibration of the specimen with gas, rapid quenching, and hot vacuum extraction of the dissolved gas with subsequent quantitative analysis by mass spectroscopy. EXPERIMENTAL Two completely separate systems were employed to accomplish first, the equilibrium saturation of the sample and second, the extraction of the dissolved gas. Saturation Apparatus. The saturation apparatus, illustrated in Fig. l, consisted of a vertically mounted quartz tube with a three-way valve for vacuum or hydrogen near the top and an outlet near the bottom leading to a butyl phthalate seal. The bottom end of the tube was terminated with a joint accommodating an O-ring sealed "Asco Stirring Gland" (The Emil Greiner Co.). This gland facilitated movement of the thermocouple without introduction of air into the system. The upper portion of the tube (above the furnace) was water-jacketed. A Welsh 1405-B mechanical pump provided the necessary system evacu-

Jan 1, 1968

By S. L. Couling, G. W. Pearsall

MOTT and Hainesl have summarized the available techniques for the examination of aluminum and some anisotropic metals under polarized light. Many of these techniques are rather complicated and cumbersome. This note presents a simplified procedure for using polarized light to obtain information about the crystallographic orientation of any particular grain in a magnesium alloy. Since other hexagonal metals are more anisotropic than magnesium, similar methods might well be applied to them. Ernst and Laves2 produced a double-refracting layer on magnesium alloy specimens by SuCCeSSiVe etches in solutions of perchloric acid in alcohol, magnesium perchlorate in perchloric acid and alcohol, and calcium and magnesium carbonates in water. They examined their specimens under polarized light and were able to determine the direction of the hexagonal axis in any particular grain from a measurement of the extinction behavior of that grain. The disadvantages of their technique were the complexity of the etching procedure and the explosive hazard of the perchloric acid-alcohol solutions. Results equivalent to those of Ernst and Laves were obtained in this investigation after etching specimens for 6 to 8 sec in an acetic picral solution containing 100 parts 6 pct picral, 10 parts distilled water and. 5 parts acetic acid. A. similar etch has been used by George3 in earlier metallographic

Jan 1, 1958

By James Douglas

In discussing the waste upon which hinges, or is supposed to hinge, so largely the preservation of our national resources, the conclusions reached would be more reliable if actual experience were consulted, and fewer deductions were drawn from general statements, which are often the product of the imagination. It cannot be questioned that the value of by-products has .not been sufficiently appreciated by us, and that our tardiness in recovering the useful ingredients of the escaping gas of our coke-ovens is one of the most glaring instances of shortcoming in that direction. And yet even for that sin there is some palliation in the immature condition of affiliated industries. I presume that it is admitted, without argument, that, except under very exceptional conditions, all the elements cannot be recovered from most of the ores or natural products which we treat. While it is a shame that the by-products from our coke-ovens should be dissipated, Edward W. Parker's report to the U. S. Geological Survey for 19061 supplies a fairly good excuse in justification of this appalling waste. He says (pp. 773 to 774.): " What has been already commented on in previous reports about the slowness of manufacturers to change from the better known but wasteful beehive practice to the by-product recovery method of coke manufacture is particularly emphasized in the statistics presented in this chapter. For it would appear from the table following that the construction of by-product ovens had about come to a standstill, especially when the records for the preceding five years are taken into consideration. At the close of 1901, when there were only 1,165 by-product ovens completed in the United States, there were 1,533 in course of construction, 498 of which were completed during the following year. At the close of 1902, 1,346 retort ovens were building, 293 of which were added to the completed plants in 1903. At the close of 1903, 1,335 new ovens were building and 954 of these

Jan 1, 1910

By Brian F. Dyson

The surface tensions at 1550°C of some Fe-S alloys (in the range 0.008 to 0.052 wt pct S), Fe-Sn alloys (0.31 to 48.4 wt pct Sn), Fe-P alloys (0.038 to 2.38 wt pct P), Fe-Cu alloys (2.15 to 22.8 wt pct Cu), and Fe-1 pct C-S alloys (0.005 to 0.076 wt pct S) along with the surface tension of the base iron have been measured by the sessile-drop method. A mean value of 1754 dynes per cm was found for the surface tension of the base iron. Sulfur was found to be highly surface-active, the surface-tension results being in quantitative agreement with existing data. Tin and copper were found to be less surface-active than sulfur while phosphoms was completely nonsurface-active. The surface tensions of Fe-1 pct C-S alloys were found to be lower than those of the Fe-S alloys containing the same sulfur content. This was shown to be a mmzifestation of the increase in the thermodynamic activity of suZfur by carbon. It is only in recent years that attempts have been made to measure the surface tension of liquid iron of known high purity.1-3 Earlier measurements4-7 were made on liquid iron containing variable amounts of what are now known to be surface -active solutes. The exact value of the surface tension of liquid iron is still, however, open to some doubt. Halden and Kingery' reported a value of 1720k 34 dynes per cm at 1570°C, Kozakevitch and Urbain8 gave 1790k 25 dynes per cm at 1550°C, while Van-Tszin-Tan et al. obtained a value of 1865k 37 dynes per cm at 1550°C. The first systematic investigation into the effect of controlled solute additions on the surface tension of iron was made by Halden and Kingery.' They showed that sulfur and oxygen were highly surface-active, whereas nitrogen was only slightly active, and carbon inactive. A subsequent investigation by Kingery indicated that two other group-6B elements, selenium and tellurium, were also surface-active. This highly surface-active nature of sulfur and oxygen has recently been substantiated by Kozakevitch and Urbainla and Van-Tszin-Tan et al. l1 Kozakevitch and Urbainl2 have also conducted an experimental survey of the effects of a number of metals on the surface tension of liquid iron. Their surface-active nature was, in all cases, less than that of the group 6B elements. The present investigation was undertaken to study in more detail the surface tensions of dilute Fe-S alloys and to measure the surface tensions of binary alloys of iron containing phosphorus, copper, and tin. The effect of sulfur additions on the surface tension of Fe-1 pct C alloys was also determined. EXPERIMENTAL PROCEDURE The sessile-drop method was employed in the present investigation. An apparatus was built similar in principle to that described by Humenik and Kingery.lS It consisted of a horizontal silica tube, which could be evacuated to pressures less than 10-5 torr, with its central portion surrounded by a water jacket within which was a high-frequency coil. This generated heat in a tantalum susceptor placed inside the silica tube, which in turn radiated heat to the specimen mounted on a recrystallized alumina plaque. Temperatures were measured by an optical pyrometer and photographs of the molten drop were taken on a fixed-focus plate camera giving a magnification of X2. Surface-tension values were determined from the resultant drop using the method described by Baes and Kellogg.l4 The high vapor pressure of molten iron made it necessary to conduct all the experiments under a 1/4 atm of argon (greater than 99.995 pct purity). The analysis of the base iron used in the investigation is given in Table I. Each sample was approximately 3 g in weight and had a hemispherical base to ensure a uniform advancing contact angle on melting. The iron alloys were prepared individually in the sessile-drop apparatus by drilling a hole in the top of each sample and adding the required amount of solute, the drops being analyzed after the experiment. This method of preparation had the advantage of ensuring a consistent minimal contamination by oxygen due to refractory attack and also allowed surface tension to be measured at the same time. Every precaution was taken to ensure that the specimen was not contaminated by grease when it was introduced into the apparatus, the samples being cleaned in acid, dried in alcohol, and rinsed in petroleum ether. All handling was done with tweezers. Once the specimen had been placed inside the susceptor, the furnace was evacuated and the Sample leveled. The furnace was then degassed at approximately 1000"C before the argon was introduced. In every case the surface tension was determined at 1550" C.

Jan 1, 1963

By W. J. Shearer

A COMPARISON of statistics relating to coal min-ing in Great Britain and the United States leads one to suspect widely differing conditions and practice. A brief review of some of the conditions may enable American mining men to appreciate more fully the difficulties with which British engineers are faced, and to some extent explain why American, coal can be sold f.o.b. mine at the present time at about 50 to 60 per cent of the cost of British coal at the mine, and why British man-shift outputs fall far below American at present being less than 30 per cent. Bulman gives the average depth of 6-ft. seams. in Britain at 1350 ft., and of 2-ft. seams at 517 ft. George S. Rice states that 90 per cent of American coal 'is taken from less than 600 ft. Much English coal is taken below 2000 ft. and some below 3000 ft. The total influence of depth on cost is not always evident. Room work as known in America becomes less advisable with increasing depth, as pillars crush badly if left -for any length of time. A limited amount of bord and pillar work, taking very small amounts of coal in the first working, takes the place of room work, with rapid working of the pillars as soon as the panels are broken. Ventilation difficulties increase tremendously with depth and thinning coal. In America the chief use of air underground is to dilute gas. In Britain it serves a dual purpose, in many cases the amount of air cir-culated being far in excess of the quantity necessary to dilute gas to reasonable proportions. At great .depths rock temperatures exceed-95 deg. F., and great volumes of air are necessary for rock cooling. At these high temperatures humidity becomes an important factor. At present a great deal of research is under way to find methods of overcoming the troubles experienced with high temperature and humidity in deep mines.

Jan 8, 1928

By C. D. Thompson, D. C. Violetta, C. A. Czako

The mechanics of the continuous sintering process are briefly reviewed and the application of this process for the beneficiation of principal minerals used in making cement is shown. Pilot plant tests using pyrobeneficiation techniques were conducted with mixtures of limestone and shale in various ratios. Results are illustrated and show the percentage removal of carbon, carbonates, sulfur, alkalies, and volatiles as a function of the limestone-shale ratio. Tests with varying quantities of solid fwls, added to mixtures containing limestone and shale in a 4 to 1 ratio, were made to attain optimum elimination of the volatile constituents. Experimental results show that 90 pct of these constituents were removed during the calcination sintem'ng process. The advantages of using the beneficiated material for making cement are discussed with regard to prepam'ng, handling, and clinkering operations. A sintering process for treating raw materials or kiln waste products which contain high amounts of alkaline materials is described. Tests were performed with a high alkaline waste dust mixed in a 1 to 1 ratio with raw cement meal. The data from these tests and others using different halides for aiding alkali removal are evaluated by the alkali content of the cement clinker. Test results showed that the Dwight-Lloyd process could be applied with facility in beneficiating raw materials for cement making. Substantial quantities of deleterious volutile constituents were removed by calcining and sintering techniques. The continuous sintering process has been applied for a number of years as a means of beneficiating minerals for subsequent conversion to merchantable products. The process was developed and first used for nonferrous metallurgical applicatfons. However, it has risen to prominence for ferrous metallurgical applications where last year in the U.S. and Canada nearly 40 million tons of iron ore were treated by grate firing processes. Through the years of process development many investigators have realized the versatility of the sintering process and have directed experiments toward the use of it for applications with nonmetallic minerals. These have included calcining limestone, carbonizing coal, expanding shale, and burning cement raw meal. Today commercial sintering plants produce cement clinker from mixtures of limestone and shale, lightweight aggregate from shale or clay, and calcined products from phosphate shale. The mechanics of the downdraft sintering process have been presented by many authors. In general practice the materials to be agglomated are mixed as moistened fines with a solid fuel and this mixture is spread uniformly on the grates of the sintering machine. The charge is then momentarily directed under an ignition furnace. After ignition a continuous downdraft of air promotes combustion of the fuel and through heat transfer particles become partially fused into a coherent mass. This is cooled from continued draft induced after combustion. Many investigators have shown that distinct zones are formed during the process of sintering iron ores. At the midway point of the sintering process these are prominent and are, respectively, from the top of the bed to the bottom, comprised of a cooling zone of sintered material, a combustion zone of sinter formation, a calcination zone, a drying zone, and a zone of unreacted materials. Completion of sintering occurs near the discharge end of the machine where the firing zone approaches either the grates or grate dressing material called hearth layer. Here the peak draft temperature usually can be noted in the windboxes. The zonal pattern has been illustrated with the use of graphs which show thermal gradients as they progress through the bed of materials during sintering. Fig. 1 shows, in simplified form, thermal gradients existing when clinkering cement on a sintering machine. The thermal gradients illustrated are for periods of initiation, midway and completion of the clinkering process. The occurrence of these zones has importance for the beneficiation of cement raw materials. A research program was performed at the Dwight-

Jan 1, 1961

By C. S. Herzig

In the Engineering and Mining Journal of Jan. 27, 1900, there appeared an article by Fred T. Greene, describing a method of measuring stopes by the use of strings, a clinometer and a tape. In the early part of 1899 I had occasion to use a somewhat similar method, for the purpose of accurately ascertaining the volume of a very irregular drift connecting two mines. This drift was an important factor in a lawsuit for $150,000, in which it was necessary to determine accurately the volume originally occupied by the material extracted from the drift. While it is unnecessary to give all details of the controversy, some explanation of the conditions is required for a clear understanding of the following description. This drift was started by the a E." Co. from its workings, in about 7 ft. of ore, and headed toward the " G " property, the plan being to extract all the ore between foot- and hanging-walls, but to take out nothing but ore. As the " G." workings were approached; the ore-body became very irregular and much thinner. It was, however, very closely followed, and where the drift broke through into the " G." workings, the hole was only 11 inches high by 14 inches wide, or just about the size of a man-hole in a boiler.. Thus, this connection-drift tapered sharply; and the very irregular foot-wall sloped toward the " G." workings, and entered them at a place where the stope was only about 3 ft. high, and the ground had already commenced to cave. It may be added that the ore-body was a nearly flat deposit of lead carbonate in limestone, the ore and gangue being quite soft. I was called upon by the " G." people to make the survey

Jan 1, 1901

By Konrad Stern

The terms asphalt and bitumen have been applied interchangeably, although incorrectly on occasion, for centuries to various bituminous materials that were found in nature. Native bituminous materials of only the solid types, deposits of which are found on or near the surface of the ground, together with the principal asphaltic type petroleum bitumens will be considered in this chapter. The international dictionary compiled by the "Permanent International Association of Road Congresses" still gives the full name as "Asphaltic Bitumen" but of recent years the word "Bitumen" has been recognized as most appropriate and is defined by the American Society for Testing Materials as follows: "Mixtures of hydrocarbons of natural or pyrogenous origin, or combinations of both, frequently accompanied by their nonmetallic derivatives, which may be gaseous, liquid, semisolid or solid and which are completely soluble in carbon disulfide." Asphaltic pyrobitumens, as defined by Abraham,2 is a species of pyrobitumen, including dark-colored, comparatively hard and nonvolatile solids; composed of hydrocarbons, substantially free from oxygenated bodies; sometimes associated with mineral matter, the nonmineral constituents being infusible and largely insoluble in carbon disulfide. Deposits of native bituminous materials are found scattered over the entire world, but many are relatively unimportant as far as commerce is concerned. No attempt has been made to cover all of the known deposits. The principal bituminous materials of commercial interest are: 1. Native asphalts, solid or semisolid, associated with mineral matter such as Trinidad Lake asphalt, Rock asphalt and Selenitza, Boeton and Iraq asphalts. 2. Native Asphaltites, such as gilsonite, grahamite and glance pitch, conspicuous by their hardness, brittleness and comparatively high softening point. 3. Asphaltic bitumens obtained from nonasphaltic, semi-asphaltic and asphaltic crude petroleum by distillation, blowing with air and the cracking of residual oils. 4. Asphaltic pyrobitumens of which wurtzilite and elaterite are of chief interest industrially as they depolymerize upon heating, becoming fusible and soluble in contrast to their original properties in these respects.2 5. Mineral waxes, such as ozokerite, characterized by their high crystallizable paraffine content. Native Lake Asphalt At Brighton situated in the southwestern part of the Island of Trinidad is one of the largest deposits of native asphalt in the world.3 The lake is oval in shape, covering an area of 114 acres and having a depth of 285 ft at its center. The material forming this deposit is an emulsion of water and bitumen with a suspension of mineral matter consisting of impalpably fine clay dispersed by nature in the asphalt, and small quantities of silica and vegetable matter. The entire mass of asphalt is in slow but constant motion as evidenced by the migration of islands of vegetation from one place to an-

Jan 1, 1960

George Smith, Sydney, N. S. Wales (communication to the Secretary): The very interesting paper by Mr. Emmons on " The Secondary Enrichment of Ore-Deposits " has just come under my notice; and its reference to my own paper* on " The OreDeposits of the Australian Broken Hill Consols Mine "† is therefore only noted some two and a half years after its publi-

Jan 1, 1903

By J. W. Marx, R. H. Langenheim

The injection of heat-bearing fluids may offer a wider application to secondary and tertiary recovery from conventional oil reservoirs than inderground combustion since the process is more easily controlled and the reservoir requirements, in general, are less critical. In all cares, conduction heat losses to overburden and un-derburden will impose an economic limit upon the size of the area which can be swept out from any one injection point for any given set of conditions. The present report describes a method for c.rtin~ating thermal invasion rates, cumulative heated area, and theoretical economic limits for sustained hot-fluid injection at a constant rate into an idealized reservoir. Full allow-ance is made for non-productive reservoir heat losses. Required solutions can be obtained directly from the numerical tables given here, as soon as all operating conditions are specified, withou extensive mathematica1 ~nanipulation on the part of the user. The injection of a heat-bearing fluid into a reservoir is frequently proposed as a means of secondary or tertiary oil production. This form of thermal recovery may offer a wider application to conventional oil reservoirs than underground combustion since the process is more easily controlled and the reservoir requirements, in general, are less critical. Because of its large gross heat capacity, steam appears to be the most efficient heat injection medium, although mixtures of steam and other gases, hot water, hot oil and hot non-condensable gases also have been employed. Whatever the nature of the injection medium, economic evaluation of such thermal recovery processes will depend upon thermal invasion rates, or rates of productive reservoir heating, at any given time after the start of heat injection. In all cases, conduction heat losses to overburden and underburden will impose an economic limit upon the size of the area which can be swept out from any one injection point, for a given set of reservoir conditions, at any given heat injection rate. The present report describes a method for estimating thermal invasion rates, cumulative heated area and theoretical economic limits for sustained heat injection at a constant rate into an idealized reservoir, making full allowance for non-productive reservoir heat losses. Required solutions can be obtained directly from the nu- merical tables given here, as soon as all operating conditions are specified, without extensive mathematical manipulation. It should be noted that ordinary water flooding may be used to move an annular-heated zone outward, even though the economic areal limit for straight heat injection has been reached. Thus well spacing need not be confined to the areal limits as determined here. However, the present calculations do not cover such supplementary heat scavenging programs. The operating element consists of a radial flow system, concentric about the point of injection, with the idealized step function temperature profile illustrated by the dashed line in Fig. 1. The solid curve shown in Fig. 1 gives a qualitative picture of the true radial temperature distribution. It will be shown later that the expressions given below, which are derived from the simplifying step idealization (dashed line in Fig. I), also can be interpreted in terms of the more realistic temperature distribution shown in Fig. 2. For this case, the thermal invasion radius is simply redefined as the distance from injection well to the mid-point of the temperature distribution.

By T. J. Nowak

The heat flow processes determining the injection and shut-in temperature logs in a water injection well have been analyzed and the theoretical basis for determining the water injectivity profiles from the temperature logs has been presented. Both the injection and the subsequent shut-in logs are necessary to resolve the injection interval into relative water intake strata; the former, to provide an accurate estimation of the thicknesses of the strata, and the latter to indicate the major and minor intake rates into the strata. A procedure is described for estimating the injectivity profile from the temperature logs and is applied to several temperature logs. For a water injection well, a comparison is made of the injectivity profiles obtained from the core analysis, the spinner survey, and the temperature logs. INTRODUCTION In secondary recovery of oil by water flooding, the injectivity profile is needed to obtain diagnostic evaluation of water intake distribution over the injection interval. If the distribution is unfavorable among the various strata, corrective measures can be taken to provide better control. Numerous methods have been developed for determining the injectivity profile from water velocity measurements in well bores. Often, dependence is placed upon core analyses and/or electric logs for estimating the relative water intakes over the injection interval. In many cases, the temperature log method described herein will give results more diagnostic than those obtained through use of the other available methods inasmuch as it is based upon the study of temperature disturbances in and around the well bore as a function of water flow in the well bore and in the formation. This method is the result of analyses of a number of temperature surveys made in water injection wells to determine the point of entry of the water into the formation. The material in this paper is presented in two sections: the first deals with the theoretical study of temperature survey data, and the second deals with the field application. PART I — THEORETICAL TREATMENT OF TEMPERATURE LOG DATA Before discussing the various aspects of heat flow relative to temperature log data, the phenomena that give rise to well bore temperatures — namely, the indigenous formation temperature and the associated rates of heat flow — will be considered. Geothermal Gradient The geothermal gradient is defined as the increment of depth at which the indigenous subsurface temperature increases by l°. It is caused by the continuous flow of heat outward from the interior of the earth. The flow of heat is an equilibrium process between the heat sources, the thermal conductivities of the formations, and the mean surface temperature. Therefore, there is no accumulation of heat energy in the path of heat transmission, and the geothermal gradient for a given formation will depend upon its thermal conductivity.

Jan 1, 1953

By E. A. Anderson

THIS seems to be the year for superlatives in A.I.M.E. meetings. The programs of the various Divisions and Institute committees offered an abundance of interesting and valuable information in the form of technical papers, symposia. and lectures to large and interested audiences. The Institute of Metals Division may hold up its head with pride for its own program. With six technical sessions, three full-day symposia, and the annual I.M.D. dinner, four meeting days were not enough and many simultaneous sessions were required. The quantity and quality of the paper were equaled by the numbers and interest of those attending.

Jan 1, 1944

US 4,137,751-Aerial geophysical exploration for ore deposits by collecting and analyzing atmospheric particulates The aircraft has an Inlet duct extending outward and including a "shave-off" duct, a cyclone separator located inside the cabin which is coupled to the inlet duct, a clean air exhaust duct, and a receiver for the collected particles incoming air is divided into two fractions. The fraction taken by the "shave-off" duct and containing the bulk of the particles is routed to the cyclone Particulates are gathered on a collector tape for subsequent analysis and correlation with the areas covered J. R Rhodes, R D. Sieberg, M. C Taylor, J. C Westkaemper, and R C. Young, assigned to Columbia Scientific Industries, Inc Feb. 6, 1979 7 pp. (73-28) Filed- 2-28-75 (554,114) Same British 1,446,760, dated Aug. 18, 1976. US 4,156,138-Exploration for subsurface deposits of uranium ore Pairs of dosimeters are placed underground in a grid pattern Each dosimeter contains a phosphor which IS capable of storing the energy of alpha particles. One dosimeter is heavily shielded from alpha particles, while the other in the pair is thinly shielded to exclude dust After a period underground the dosimeters are heated to release the stored energy as light. The amount of light produced from the heavily shielded dosimeter is subtracted from the amount of light produced from the thinly shielded dosimeter to give an indication of the location and quantity of uranium underground This patent is a division of US Patent No 4,053,772, dated Oct 11, 1977 P E Felice, assigned to Westinghouse Electric Corp May 22, 1979 5 pp (250-253) Filed. 8-12-77 (824,203) US 4,180,727-Method for measuring the gamma-gamma density of uranium ore in the vicinity of a borehole A first gamma-ray detector receives only natural gamma rays from the borehole, while a second receives both natural gamma rays and scattered uranium-source gamma rays The value of the uranium-source gamma rays is calculated. W W Givens, assigned to Mob11 011 Corp Dec 25, 1979 6 pp (250- 264) Filed 10-20-77 (843,909) US 4,180,72&A neutron activation probe for determining the location and grade of uranium ore, especially where thorium or other fissionable isotopes are present, includes a pulsed neutron source in series with a plurality of delayed neutron reactors for measuring radioactivity in a well bore- hole together with a Nal(T1) counter for measuring the high energy 2 62 MeV gamma line from thorium The signal from the Nal(T1) counter IS subtracted from the signal from the delayed source detectors to ascertain the amount of uranium present in the ore body N. P Goldstein and R C Smith, assigned to Westinghouse Electric Corp Dec 25,1979 6 pp (250-264) Filed. 4-1 1-78 (895,323)

Jan 1, 1980

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 Warren W. Jamar, Philip D. Pearson

IN recent years, there have been many changes in mining operations in the Lake Superior district. To follow these trends on the Menominee Range of Michigan, information has been assembled from all of the iron informatior]mining operations in the area. There are 15 operating underground mines in the Iron River-Crystal Falls area of the Menominee Range. Within the past two years, two idle properties were reopened pasttwoyears,and are now producing, and a third and fourth are being reopened. Also, there are two siliceous openpits operated by independent companies outside this immediate area. Six companies operate the underground mines, employing some 1850 employees. Table I shows pertinent facts about these properties. During 1949, the largest mine in Iron County shipped 571,287 tons, and one of the newer mines shipped 39,378 tons, with a range total to 3,535,-373 tons. Since the Menominee Range was opened in the 1870's, the mines in Iron County have shipped 85,890,922 tons. From an operator's viewpoint rather than a geologist's, the ore is' classified as semi-hard, composed of hematite and limonite. It is not as soft as the ores of the Marquette Range nor is it as hard as the hard ores of the Marquette and Vermillion Ranges. The ore bodies have slate hanging walls and slate footwalls. In most cases the hanging walls and footwalls are soft and high in sulphur. The sulphur comes from pyrite, and these slates will ignite when piled more than 6 to 8 ft high. Ore is mined on this range by: 1—Sub-level stop-ing; 2—Shrinkage stoping; 3—Sub-level caving; 4— Block caving; 5—Top slicing. The predominance of these methods is in the order named. Underground drilling is important in the mining cycle. Some changes made and trends toward future changes fall into four categories: Drill bits, drill steel, drill machines, and compressed air pressures. Several types of bits have been tried and are in use. They include the detachable tungsten carbide, insert bit; the intraset steel bit, which is a conventional steel rod with tungsten carbide insert; the one-use bit; and the multiple-use bit. For many years, detachable multiple-use bits have been standard. In tests conducted recently to im- prove drilling efficiency, this bit was used as the basis for comparison. Under existing conditions, a multiple-use bit can be resharpened about three times before it is discarded. A thorough test of 2-in. tungsten carbide threaded bits was conducted under various ground conditions. 1—The drilled footage ranged from 48 to 600 ft per bit; averaging 357 ft per bit. Under these same conditions, a multiple-use bit ranged from 8 to 80 ft per bit. 2—The bit cost was greater for the insert bit in each case. 3—The average drilling speed for the insert bit was 12 in. in 62 sec and for the multiple-use bit was 12 in. in 64 sec. In a second test, 2V4 -in. tungsten carbide bits with the large 1 3/16-in. thread were used in moderately soft ground on a 152-lb drifting drill on a long feed jumbo. 1—The drilled footage ranged from 450 to 5000 ft per bit, averaging 1810 ft per bit. Under these same conditions, a multiple-use bit averaged 64 ft per bit. 2—The bit cost was reduced by the use of the insert bit. 3—No increase in drilling speed was recorded. 4—Minimum footage obtained was caused by thread failure. To improve the thread life, thread size on the rod was increased and the bit was attached to the rod with a pipe wrench. After this, bits failed in equal proportions because of cracked skirts, broken inserts, and gage loss. Tungsten carbide bits are now used in the operation where this second test was conducted because labor costs were lowered as a result of reducing the number of bits being changed by the miners. At the same operation and under the same conditions as the second test, 1Y4-in. insert bits with standard 1-in. threads were used. These bits did not drill much more than 300 ft before thread failure and were then welded to the rods and used until total failure. Sometimes this footage was considerable, sometimes it was not. Chisel-type 2%-in. insert bits were

Jan 1, 1952

By W. O. Philbrook, L. D. Kirkbride

IN the normal operation of the iron blast furnace, reduction of the iron oxides is accomplished almost entirely above the tuyeres.' Blast furnace slags usually contain less than 0.5 pct FeO, although higher values may occur with abnormal operation. There is reason to conjecture, however, that incompletely reduced ore may sometimes reach the hearth and enter the slag as a result of heavy slips or, perhaps, even from cores of excessively large lumps of a charge material of poor reducibility. The possibility of reoxidation of iron droplets falling in front of the tuyeres has been considered by several writers. It would be of interest, to know how rapidly iron oxides reaching the slag for any of these reasons could be reduced by reaction with coke or with the high carbon liquid iron in the hearth. In comparison with the hundreds of papers that have appeared on various aspects of the reduction of solid iron oxides by gases and in the presence of several forms of carbon, little work has been published on the reductioin of liquid oxides or slags. Dancey measured rates of reaction of the pure liquid oxides, both FeO and Fe,O,, with molten iron containing about 4.3 pct C. The oxide was dropped into the cup formed in the upper surface of the iron by rotating the crucible and melt. Under these conditions, reduction of either FeO or Fe,O., was completed in less than 10 sec. The present study was concerned with the reduction of FeO from blast furnace-type slags containing less than 5 pct FeO and melted over carbon-saturated iron in stationary graphite crucibles. The results were considerably different from those found by Dancey, as will be discussed later. Although this work is of interest in relation to hearth reactions in the blast furnace, interpretations must be made with caution because the experimental conditions do not duplicate those within a furnace and may not even lead to the same reaction mechanism. The authors were motivated in undertaking this work by an additional interest—the part played by FeO reduction in the mechanism of de-sulphurization of iron by slags under similar experimental conditions. Derge, Philbrook, and Goldman eveloped detailed experimental evidence to support a three-step mechanism for desulphurization like that originally proposed by Holbrook and Joseph' (These reactions are written in molecular form for convenience, but this is not intended to imply the existence of molecules of FeS in the bulk metal phase nor to deny the likelihood of ionic reactions in the slag.) Earlier work by Chang and Goldman" had shown that the overall reaction follows first-order kinetics with respect to sulphur and that the rate of reaction is proportional to the slag-metal interface area, which observations have been confirmed by subsequent work. Later studiese,' have established the influence of al.loying elements on the first and last steps of the reaction. This paper reports a study of step 3 alone, uncomplicated by the simultaneous process of sulphur transfer. Apparatus and Procedure The experiments were made in a conventional high frequency induction furnace powered by a 35 kva Hg spark gap converter. The graphite crucibles used for most of the runs were 14 cm (5.5 in.) deep and 4.8 cm (1.9 in.) ID with 0.75 cm (0.3 in.) wall. An insulating cover with a small opening for withdrawing samples was used to minimize heat loss and infiltration of air into the furnace. The crucible was charged with 300 g of carbon-saturated iron and either 65 or 100 g of prefused slag analyzing 38.0 pct SiO,, 15.4 pct A10 and 47.1 pct CaO. To obtain the cleanest possible interface at the start of the reaction, the metal and slag were brought to temperature together to prevent the rejection of kish graphite that would have been caused by the chilling effect of a large addition of cold slag to carbon-saturated iron. After temperature control had been established, the desired amount of iron oxide was added in the form of a prefused slag of composition 73.6 pct FeO, 7.7 pct AWX and 19.0 pct SiOl. This slag addition was observed to be molten in somewhat less than 1 min, and a very vigorous reaction proceeded for 1 to 2 min after its introduction. Zero time was taken as 2 min after the ferrous silicate slag addition. Slag samples weighing about 0.5 g each were taken periodically by a copper chill sampler." The weight of the initial slag was large relative to the weight of samples removed, so that the slag weight never varied by more than 5 pct during any run. Temperature was measured by a calibrated W/Mo thermocouple immersed in the metal, with a graphite tip cemented over the fused silica protection tube to prevent attack by slag and metal. After some difficulties with uncertain temperatures during the first two runs, the practice adopted to position the thermocouple for reproducible results was to lower the protection tube to touch the bottom of the crucible and then raise it 0.5 cm. The apparent temperature gradient between the bottom of the crucible and the top of the slag was found to be 15°C (27°F). but much of this spread was probably the result of inadequate immersion of the protection tube to off-set conduction losses along the graphite tip when the thermocouple was inserted only into the slag. The temperature of the bath was controlled within 25°C (9°F) during a run.

Jan 1, 1957

By Howard L. Hartman, Eugene P. Pfleider

The paper relates to the laboratory and pilot plant studies that have been carried out by Sherritt Gordon Mines Ltd., Metallurgical Research Div., in developing the ammonia pressure leach process for extracting Cu, Ni, Co, and S from high grade Ni concentrate produced from Lynn Lake ores and describes in some detail the chemistry of the process. In the leaching stage air, ammonia, and sulphide minerals react in a sequence of inter-related steps to produce soluble amines of Ni, Cu, and Co in a solution containing sulphate, thiosulphate, polythionate, and sulphamate ions and a controlled amount of free ammonia, the iron and other components of the concentrate remaining as an insoluble residue which is separated from the leach solution by filtration. The pregnant solution produced in leaching is further treated by boiling to precipitate and remove Cu as cuprous sulphide, leaving a copper-free solution with a composition suitable fir subsequent precipitation of Ni and Cu by H,. The progress of individual reactions in leaching and copper removal is discussed. The effect of variables such as temperature, pressure, ammonia concentration, particle size, and agitation is outlined and the technique of thionate control in leach solutions is described. Data is given for the physical and chemical reactions involved in precipitating copper from leach solutions as Cu sulphide by boiling.

Jan 1, 1956

Mining headlines in 1952 dealt mainly with expansion as the industry aimed for an ever increasing production to meet the nation's needs. Huge sums were expended for equipment, research, and development. Headlines told part of the story. Negotiations between San Manuel Copper Co. and the RFC finally resolved in a $94 million loan for the development of low grade Arizona ores. Magma Copper, parent firm was to supply an additional 8 million. Kennecott Copper Co., deepening its Deep Ruth Shaft of its Ruth, Neyy mine, announced that the shaft would be in full production in 1953.

Jan 2, 1953

By C. F. Jr. Nagel

THIS paper is written primarily for those who are familiar with the processes mentioned but who desire a further insight into some of the fundamental principles. It does not give a complete description of the various practices employed in the working of aluminum and its alloys, but presents a few illustrations of the essential respects in which aluminum differs from other common metals, and emphasizes the controlling factors of the processes under consideration. HEAT TREATING Certain aluminum alloys are capable of having their mechanical properties greatly altered by a heat-treatment process. The degree of this improvement may be illustrated by the typical properties of duralumin (Table 1). It is essential that the material be in the wrought condition in order to obtain maximum heat-treatment effects.

Jan 1, 1927

By Chester N. Truax

Still another shadow was cast over coal's largest market-the electric utilities-when President Johnson signed into law the Federal Clean Air Act of 1967. Air pollution-sulfur reduction-was thus brought into sharper focus as one of the central problems of the coal industry. Industry executives testified in both Houses of Congress to enable the lawmakers to develop a workable and economic law. The new legislation calls for the Secretary of Health, Education and Welfare to establish air control regions. After the regions are outlined the Department will publish air quality criteria on pollutants. Anticipating this legislation, the coal and utility industries have for the last several years been involved in extensive research programs to develop solutions to the air pollution problem. Even though the coal industry has been under strong attack for its part in adding contaminants to the atmosphere, it is by no means the major contributor.

Jan 2, 1968