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By Paul J. Fopiano

SOME relationships between the flow characteristics of iron single crystals of 99.9 pct purity and the behavior of imperfections have been investigated. X-ray rocking-curve measurements and etch-pit counts were made as a function of plastic strain, and compared to the stress-strain curve obtained on a modified Polyani tensile machine. Crystals grown from rolled strips of vacuum-melted iron by the strain-anneal method1 had a high preference for a (110) longitudinal direction and a (211) face normal. The tensile specimens were prepared from 2 by i by 0.040 in. single crystals having a gage area of 3 by \ in. Rocking-curve measurements were carried out with a highly perfect germanium monochromating crystal in which the dazz spacing was matched to that of the dZl1 in the ir0n.l Well-collimated CuKal radiation was used throughout. These procedures practically eliminated errors due to geometrical and wavelength resolution. Inasmuch as the rocking-curve half breadth may vary markedly from point to point in the specimen being irradiated, the crystals were strained in place by mounting a hydraulic loading device on the double-crystal spectrometer. The rocking curves were taken after each increment of strain in the unloaded condition, since no observable difference was found in the rocking-curves between the loaded and unloaded states. The rocking-curve half breadths of the as-grown specimens were in the range 90 to 120 sec of arc when the beam irradiated an area of about -£ by -& in. on the specimen. DeMarco and weiss3 have shown that, for a well-colli- mated X-ray beam, irradiating about 10"! sq in. of the very same material, half breadths within 10 pct of the Darwin natural half breadth were observed. Since the rocking-curve specimens were stressed by the load-unload technique, the strain achieved at any given stress depended on the time of holding because of low-temperature creep. Fig. 1 shows the rocking-curve half breadth (also area/peak height) as a function of plastic strain for a relatively short holding time (2 to 5 min) at each stress level. For strains less than 0.1 pct the rocking-curve breadth is essentially constant; it is only for larger strains that there occurs a significant increase in this breadth. Where the holding times at each stress level were longer (by well over an order of magnitude) there occurs a significant increase in the rocking-curve breadth only after plastic strains of the order of 0.6 pct had been introduced into the specimen. This observation is related to the time dependence of creep phenomena and emphasizes the difficulty in comparing data obtained by two such different straining methods. Etch-pit results were obtained using a 2 pct nital etch on specimens strained in the range of 0 to 1 pct. Prior to etching, all specimens were annealed for 3 hr at 150°C, the carbon content being sufficient to decorate the dislocations for strains of at least 1 p~t.~ The data points were all taken from parts of the same single crystal which had been strained with short holding times at stress in increments of strain of the order of tenths of 1 pct. The (211) plane is particularly difficult to etch-pit in vacuum-melted iron and therefore it is felt that these values are as much as an order of magnitude low. Fig. 2 shows the etch-pit density as a function of plastic strain. The smooth curve passing through the data points is not meant to infer a quantitative correlation with the rocking-curve data. What is of interest, however, is the change in etch-pit density in the region of 0.2 pct plastic strain. The first three increments in strain (points 2,3, and 4) did not produce a measurable change in the etch-pit density while subsequent increments did produce a measurable change. While the absolute values of these results do not appear to be cor-

Jan 1, 1967

By E. Sengier

At the Director's dinner of the A.I.M.E. on. April 22, Mr. Sengier of the Union Minière du Haut Katanga was a guest. Though a member of the Institute for sev-eral years this was the first occasion on which he had had opportunity to meet with it, and in response to an invitation from President DeGolyer, after expressing his pleasure at being present, he told informally of the present development of the Congo with which he has been so closely related. From his remarks the follow-ing has been prepared.-EDITOR. AS you know, the Belgian Congo, a fairly large colony compared with the territory of Belgium, is in the center of Africa. Natural waterways, railroads now built and new railroads under construc-tion, give increasing means of transportation and are helping toward development. The mining industry is by far the most important part of our colonial activity. Considering that we are all engineers, I will confine my figures to mining enterprise. First I will show you the relative importance of the mining industry com-pared with the total exports of the Belgian Congo. During 1925 there was exported 100,000 tons of cop-per, valued at about $25,000,000; 900,000 carats of diamonds, 8000 lb. of gold, 1700 tons of cassiterite, 300 .tons of cobalt, and 20 grams of radium, of a total value of about $35,000,000. Other products to a value of about $12,000,000 and consisting mainly of palm nuts, palm oil, cotton, ivory, copal, rubber, were also exported. From this you will see that mineral products account for about 72 per cent of the total exported value. Copper alone amounts to 52 per cent of the total and 72 per cent of the mineral exports. All minerals, with the exception of gold, which is mined by the government, belong practically toy two mining companies in which American and British capi-tal is interested with Belgian. These two companies (one called Forminière, interested in the diamond busi-ness, and the other called the Union Minière, interested in copper, cobalt, tin and radium) were formed twenty-five years ago. They started producing in 1911, but the war prevented normal operations, and active de-velopment could only be carried on after the Armistice.

Jan 5, 1927

US 4,135,913-Extraction of nickel values from iron-containing nickel sulfide ore, particularly pentlandite or nickeliferous pyrrhotite A mixture of raw ore, roasted ore, or iron powder, and coal as a reductant is heated to a temperature of 800- 1000° C in a nonoxidizing atmosphere to convert the bulk of the iron content to metallic iron while diffusing into the iron the bulk of the nickel, the mixture cooled, and the cool material separated into a magnetic fraction containing most of the nickel and a non-magnetic gangue fraction A Illis arid L S Renzoni, assigned to International Nickel Co, Inc Jan 23, 1979 7 pp (75-21) Filed 10-10-75 (621,343) Priority Canada, 10-27-72 (155,032) Same Canadian 981,910, dated Jan 20, 1976 Same British 1,389,145, dated Apr 3, 1975 US 4,135,917-In the recovery of gallium from a solution obtained by the digestion of bauxite or nepheline in an alkali solution for the production of alumina, the digestion solution is neutralized, the neutralized solution evaporated to an op¬timum caustic alkali concentration and adjusted to a ratio of alkali metal oxide to alumina of above 2, the corrected solu¬tion contacted with a gallium-aluminum alloy, arid high-purity gallium recovered from the solution by electrolysis or cemen¬tation K A Badaliants, et al Jan 23, 1979 6 pp (75-109) Filed 12-19-77 (862,201) Priority USSR, 12-22-76 (2,428,¬006) US 4,135,918-Extraction of copper from copper sulfide ore containing also one or more of the metals iron, nickel, arid cobalt Ore is roasted at a temperature of 750-800° C to expel sulfur, the sulfur-free calcine slurried in water containing a sufficient amount of sulfuric acid to supplement any sulfuric acid formed in situ, the slurry heated at 150-165° C in the presence of a reducing gas to form soluble sulfates of metals other than copper while reducing copper to elemental form, arid the slurry filtered to recover copper solids Any precious metals present in the ore will report with the copper solids V A Ettel, A P Devuyst, R Sridhar, arid C. E O'Neill, as¬signed to International Nickel Co, Inc Jan 23, 1979 5 pp (75-117) Filed 3-2-78 (882,610) Priority Canada, 5-13-77 (278,360)

Jan 1, 1980

By H. Siebel, N. A. D. Parlee

MIZIKAR, Grace, and parlee' studied rates of absorption of oxygen in stagnant liquid silver in a new type of open-ended gas-liquid metal diffusion cell, where the capillary diameters used were 1.5, 2, and 3 mm. They reported that the rates appeared to be controlled by the rate of diffusion of oxygen atoms in liquid silver and they used their data to arrive at the following equation as a reasonably good representation of the diffusivity (D) of oxygen in liquid silver: D = (14.7)10-4 exp (-7100 ± 3200)/RT cm2/sec Since this type of diffusion cell offers a promising method of measuring diffusivities of gas atoms in liquid metals, the senior author of this note and his students are carrying on a critical examination of the method, and are attempting to improve and extend the technique. The research reported briefly here was designed to examine more carefully the earlier conclusion1 that the absorption rate is diffusion-controlled, and to find out whether the diameter of the cell could be greatly increased and thus extend the method to systems where gas solubilities and diffusion rates are much smaller than in the case of oxygen in silver. For the purpose of these experiments, the open-ended capillary cell used by Mizikar, Grace, and Parlee was replaced by a small cylindrical crucible (1 to 1.7 cm in diam) containing pure silver (to a depth of 1.3 to 3 cm) resting in the bottom of a closed-ended vertical quartz tube, with an evacuated quartz filler tube just above the crucible to reduce dead volume. The method of measuring the rate of absorption was otherwise very similar to that of Mizikar, Grace, and Parlee and all the same precautions were taken. A much smaller and shorter tube furnace was used for heating, but simi- lar precautions about temperature gradients were observed. This technique was nothing more than the application of a Sieverts apparatus to the measurement of rates of absorption in small crucibles of stagnant liquid silver. In each run the volume of gas absorbed (V) was plotted against the square root of time (vt) and apparent diffusivities were calculated from the slope of the line, as described by Mizikar, Grace, and parlee.' Care was taken to use only the data obtained during the early part of the total absorption period while the cell functioned as one of infinite depth. The results at 1000°C are summarized in Table I and Fig. 1. The following conclusions may be drawn: 1) Diffusion cells up to 1.7 cm in diam yield, within experimental error, the same values for the diffusivity of oxygen (D) as the capillary cells of 1.5, 2, and 3 mm in diam employed by Mizikar, Grace, and Parlee. Cell diameters as large as 1.7 cm are probably not desirable for the most precise work. Intermediate sizes, perhaps 0.5 cm, will be most practical. 2) All absorptions measured were consistent with a model where the rate is controlled by the diffusion of gas atoms in the metal. The fact that runs at absorption pressures ranging from 0.1 to 1 atm (at any one temperature) give

Jan 1, 1965

By K. E. Manchester, A. H. Clark

Hall measurements have been made on three groups of silicon samples, which were implanted with boron, aluininunz, and phosphorus ions. Boron and phosphorus implants show essentially bulk properties when annealed under previously determined conditions, i.e., 15 min at 80O°C for boron and 10 mirz at 600°C for phosphorus. Bulk properties were also observed in alu?rrilzum-implanted samples when ion concentrations were below 1015 cm-'; however, strange low- terrzperalure behavior and a falloff in cavrier concenlralion was observed for sarnples with ion concenlration abozle loL5 ern-'. This can be attributed to solid-solubility effects since the average bulk concentration f0.r the sample exhibiting bulk properties was below the reported solubility limit for aluminum, while the other samples were above the limit. A detailed study of the annealirzg process indicates that mobilities reach bulk c~alues in phosphorus implants at 250DC, in alutninurn ivnplanls a1 500°C, and in boron implants at 700°C. A simple rnodel has been proposed to fit the annealing data. THE technique of semiconductor doping by direct injection of energetic ions is being actively investigated at this Center. Previously published results from this laboratory have been concerned with the investigation of implanted profiles in silicon and the electrical properties of the resultant p-n structures.1'2 Diode properties have been reported for junctions produced by implantation of boron ions and aluminum ions in n-type silicon and phosphorus ions in p-type silicon. Reverse current characteristics, as well as electron diffraction data, have indicated that the damage to the structure produced by the energetic ions during the stopping process can be minimized by a gentle anneal. The time-temperature conditions for this process have been determined by sheet resistivity studies.3 Electrical profiles of implanted phosphorus ions which have been determined by a differential sheet conductivity technique are based on the assumption that the carrier mobilities and activation energies for ionization are the same as in bulk silicon. These assumptions have been substantiated experimentally by measurement of Hall constants and resistivities of these implanted structures and the results are presented herein. After establishing the bulk property equivalence of the annealed layers, a more detailed examination of the annealing process was undertaken. The sheet resistivity technique initially used to determine anneal conditions has been broadened to include Hall constants and mobility behavior with anneal conditions. PROCEDURE The three groups of samples prepared for Hall measurements were implanted with mass-separated beams of boron, aluminum, and phosphorus ions. Ion concentrations are equivalent surface concentration and they have been determined from beam current measurements during implantation. Implant conditions for the samples are shown in Table I. In all cases, the samples had previously been angle-lapped on one edge and the junction delineated with an HF-copper sulfate solution. The surfaces of the implanted regions of the samples were exposed to the delineating solution and in the case of the "n"-type phosphorus-implanted areas it was later discovered that a finite amount of surface could be etched by this solution. This is discussed in the section on results. The implanted samples were ultrasonically cut into the conventional six-probe configuration shown in Fig. l.* In the annealing studies, for which the meas- urements were taken at room temperature, the sample holder was a Bakelite jig incorporating tungsten mechanical probes. The other measurements were taken using a conventional liquid-nitrogen cryostat, in which the temperature could be varied from 77" to about 400°K. For these measurements, 10-mil aluminum dots were evaporated onto the samples and alloyed with the silicon at 530°C for 15 min. The samples were then mounted in flat-packs, and gold wires were bonded to the aluminum dots. The electrical measurements were made with either a Leeds & Northrup K-5 Potentiometer, a Keithley 147 Nanovolt Null Detector, or a Keithley 601 Electrometer. No external bias was applied to the substrate. There is an inherent self-biasing arrangement at one or the other of the current contacts (depending upon the polarity), and this suffices to limit the current flow to the implanted layer. The magnetic field was generated by an A. D. Little electromagnet. Except for occasional checks of linearity of the Hall voltage with

Jan 1, 1969

By H. A. Wahl

This paper presents methods of designing hydraulic fracture treatments in formations saturated with slightly compressible liquids. Howard and Fast describe the fluid-loss control resulting from the viscosity and compressibility effects of the reservoir fluid in terms of a fracturing fluid coefficient. However, for horizontal fractures, this coefficient is applicable to infinitely thick reservoirs. These methods of evaluating fluid loss from horizontal fractures during treatment differ from previous methods in that: (I) formation thickness is incorporated in the velocity function describing the rate of fluid loss to the formation; and (2) for a given thickness the relative position of the fracture to the horizontal boundaries of the reservoir or any interrnediate permeability barrier is incorporated in the design procedure. This theory is applied to several actual and hypothetical field cases. The results of these calculations demonstrate that the eflect of formation thickness on fluid loss from horizontal fractures may result in fractures several times larger than predicted by other methods. INTRODUCTION Hydraulic fracturing has been the dominating well-stimulation technique during the last decade. From the time it was commercially available, fracturing has had a very favorable success ratio compared to other stimulation methods. However, numerous wells that were successfully stimulated remained economic failures. Only in the last few years has the oil industry recognized the importance of designing treatments for each well which will yield the maximum profit. This implies that for a given set of treatment conditions the size and general physical characteristics of the fracture can be determined. One of the outstanding contributions in the field of fracture design was presented by Howard and Fast.' In their paper, three flow mechanisms that control fluid loss from the fracture to the formation are defined: (1) viscosity effects of the fracturing fluid, (2) viscosity and compressibility effects of the reservoir fluid, and (3) wall-building effects of a treated fracturing fluid. The rate of fluid loss to the formation adjacent to a fracture is shown to be a function of time. For each flow mechanism the velocity function v(t) is expressed as a constant or fracturing fluid coefficient divided by the square root of time. This form of v(t) can be used in the Carter equation, as developed in the Howard and Fasc paper, to estimate the areal extent of fractures. This equation may be written as In the following sections the effect of formation thickness on fluid loss from horizontal fractures is evaluated when the controlling flow mechanism is the viscosity and compressibility of the reservoir fluids. The major assumptions inherent in the Carter equation are brought out in subsequent mathematical developments. THE EFFECT OF RESERVOIR FLUIDS ON FRACTURE EXTENSION When a fracture treatment is performed using a fracturing fluid identical to the reservoir fluid, the only flow mechanism controlling fluid loss is the viscosity and compressibility effects of the reservoir fluids. In developing a fracturing fluid coefficient for this mechanism, Howard and Fast considered a segment of the formation bounded by a unit area on the fracture face and extending to infinity in the direction of leak-off as shown in Fig. 1(a). The direction of leak-off z is normal to the fracture face. The equation governing the linear isothermal flow of fluid into this segment is where a = Eq. 2 is a form of the diffusivity equation. It is derived from the equation of continuity, Darcy's law and Eq. 3

ALEXANDER, JOHN S, M,'74-6,'81-3 *ASHBURNER, C A, M, '85-7 ASMUS, GEORGE, Dl, '78-80 BACON, D H , M, '00-2 BAYLES, JAMES C , M,'80-2,'91-3 P, '84-5, V,'88-9 BIRKINBINE, JOHN, M, '83-5, V, 'S7-J, P, '91-2 BLAIR, THOMAS S , M, '74-43 BLAKE, WILLIAM P , V,'71-4,'76-7,'05-6 *BLANDY, JOHN F, V,'71-3,'78-9 BLOW, A A, C, '05-7 BOWIE, A J , JR, V,'93-4 *BRAMWELL, J H , A1, '89-91 BROOKS, THOS B , M, '72 BRUNTON, D W , V, 97-8 BUCK, STUART M , M, '83-5 *BURDEN, JAMES A, V,'80-1 BURNHAM, WILLIAM, M, '82-4. CAMPBELL, H H, M, '93-5 CHAMBERLAIN, H S , V, '96-7 CHANNING, J PARKE, V,'08 CHRISTY, S B , V. '91-2, '07-8 CHURCH, JOHN A, M, '79-8l,'94-6, V, '07-8 COGSWELL, W B, V, '74-5,'86-7

Jan 1, 1910

By R. J. Linney

Reserve Mining Co. produces 5 million tons of iron ore pellets per year. The finished product runs about 65.50 pct Fe, with 7.75 to 8.00 pct SiO2. Less than 12 pct arrives at the blast furnaces smaller than % in. This plant was originally designed to produce 3.75 tons annually—not 5 million. To handle the increased tonnage a fifth fine crushing line was added, and some very minor changes were made. When production can be stepped up 33 1/3 pct without extensive additions or changes—within the short period of a year—basic engineering has been sound. Operators of the plant consider it the best design job they have seen or heard of, and competent authorities have said that start-up was quicker and easier than for any previous large-scale minerals beneficiation plant. One big advantage is the elbow room allowed. Generally speaking, there is an eternal conflict between operator and designer over space. The designer has his costs per cubic foot, and he is keenly aware that if he permits the number of cubic feet to rise unnecessarily, total costs will be too high. But this was a new operation, and on a large scale. There were no proven standards to go by. Realizing this, Reserve's engineers provided ample and efficient access to machinery, allowing extra space for unanticipated situations. In three years of production this planning has paid off handsomely. Gravity Flow Saves Time and Money: This plant is on a rocky hillside, the car dumper about 270 ft above Lake Superior. In locating buildings and placing machinery the designers mad= good use of gravity flow, at considerable financial savings. In the concentrator building from rod mills to filters, gravity carries the material between all stages of the operation except one—the closed circuit pumping of concentrate between cone classifiers and ball mills. Since no machine is located directly above any other, an observer can stand on the truck ramp adjacent to the offices and laboratory and see practically every phase of activity in the huge building. The first mill section started in August 1955. After a day's run several modifications were made on auxiliary chutes and launders where spillage had occurred. This procedure was followed for the first

Jan 1, 1960

By W. R. Toeplitz

Probably a more descriptive title would be "Much Ado About Nothing." By "nothing," of course, I refer to the porosity which is the main feature of this type of bearing. Porosity has a decided effect on the manufacturing techniques, the structure and physical properties, the oil content, and on the installation and service of oil-retaining porous bronze bearings. A simple curve can be drawn by plotting specific gravity along the abscissa and percentage of porosity by volume on the ordinate. A bronze composition, analyzing 89 Per cent copper, 9.75 Per cent tin, and 1.25 per cent graphite, has an absolute solid specific gravity of 8.5. At this specific gravity, of course, occurs the point of zero porosity. Conversely, at loo per cent porosity, the specific gravity is zero. A similar curve can be drawn for bearings impregnated with oil; the only change being that the specific gravity at loo per cent oil will be 0.89 if we assume that that is the specific gravity of the lubricant. The curve is useful in determining the oil content by volume for any specific gravity. The normal range of oil content for porous bronze bearings of this composition is from 35 to 16 per cent, which is in the specific gravity range of from 5.8 to 7.3. In addition to the amount of porosity, the type of porosity is important. The first consideration here is that the porosity must be intercommunicating. This can be determined by a number of simple tests. The first method, which is very accurate, is to extract the oil in the bearing by cycling

Jan 1, 1945

By Nicholas J. Grant, John S. Benjamin

A series of composite alloys containing a high volume of NiAl, Ni3Ah or CoAl, bonded with 0 to 40 vol pct of a ductile metal phase, were prepared by powder blending and hot extrusion. The binder metals were of four types: pure nickel or cobalt, near saturated solid solutions of aluminum in nickel and cobalt, type 316 stainless steel, and niobium. Sound extrusions were obtained in almost all instances. Studied or measured were the following: interaction between the alunzinides and the binders, room-temperature modulus of rupture values, 1500° and 1800°F stress rupture properties, hardness, structure, and oxidation resistance. Stable structures can be produced for 1800°F exposure, with interesting high-temperature strength and good high-temperature ductility. Oxidation resistance was excellent. A large number of experimental investigations have been made of the role of structure on the properties of cermets and composite materials. Gurland,1 Kreimer et al.,2 and Gurland and Bardzil3 have indicated the preferred particle size in carbide base cermets to be about 1 µ, with a hard phase content of 60 to 80 vol pct. The optimum ductile binder thickness was noted to be 0.3 to 0.6 µ.1 Complete separation of the hard phase particles by the binder is important in reducing the severity of brittle fracture.' The purpose of the present study was to produce structures comparable to the conventional cermets, using a series of relatively close-packed intermetal-lic compounds rather than carbides as the refractory hard phase, and to study the effects of binder content and composition on both high- and low-temperature properties. The selected intermetallic compounds were particularly of interest because of the potential they offered in yielding room-temperature ductility. The highly symmetrical structures are known to possess high-temperature ductility and room-temperature toughness. Based on a ductile binder, the alloys were prepared by the powder-metallurgy route to avoid melting and subsequent alloying of the matrix, and were extruded at relatively low temperatures. It was expected that the composite alloy would retain useful ductility. In contrast, infiltration and high-temperature sintering led to alloying of the matrix and to decreased ductility. The systems Ni-A1 and Co-A1 were selected for this study. In the Ni-A1 system the compounds NiA1, having an ordered bcc B2 structure, and Ni3Al(?1), having an ordered fcc L12 structure, were chosen. In the system Co-A1 the intermetallic compound CoAl with an ordered bcc B2 structure was used. ALLOY PREPARATION The intermetallic compounds, see Table I, were prepared by using master alloys of Ni-A1 and CO-A1, with additions of either cobalt or nickel to achieve the desired compositions. The master alloy in crushed, homogenized form, was melted with pure nickel or cobalt in an inert atmosphere, cold copper crucible, nonconsumable tungsten arc furnace. The resultant intermetallic compounds were homogenized at 2192°C in argon, crushed, and dry ball-milled in a stainless mill to -100 and -325 mesh for the Ni-A1 compounds and to -325 mesh for the CoAl compound. Finer fractions were separated for some of the composite alloys. Several ductile binders were utilized. These included Inco B nickel, 5µ ; pure cobalt, 5 µ, from Sher-ritt Gordon Mines, Ltd.; fine (-325 mesh) niobium hydride powder; fine (15 µ) type 316 stainless-steel powder; and near-saturated Ni-A1 and Co-A1 solid-solution alloys, also in fine powder form. The niobium hydride was decomposed above about 700°C in processing of the compacts in vacuum to produce niobium powder. The Ni-7.1 pct A1 and the Co-5.3 pct A1 solid-solution alloys were prepared from pure nickel or cobalt and pure aluminum by nonconsumable tungsten arc melting under an inert atmosphere. The ingots were homogenized, lathe-turned to fine chips, and dry ball-milled in air to -325 mesh powder. These solid-solution alloys are designated NiSS and CoSS; see Table I. Subsequently the hard and ductile phases were dry ball-milled as a blend. Experiments clearly established the need to coat the hard particles with the ductile binder to optimize subsequent hot compaction by extrusion. Ordinary dry mixing usually resulted in nonhomogeneous alloys which were quite brittle. Conventional cermets are consolidated by liquid phase sinteiing or infiltration, which resulis in undesirable and uncontrolled alloying of the binder phase. For this study, a loose (unsintered) powder-extrusion process was emploved, minimizing reactions between binder and hard particle, thereby permitting much greater control of composition and structure. The constituent powders were first mixed in the desired

Jan 1, 1967

By William Fink

Two of the aluminum-alloy systems previously studied-the alumi-num-titanium and the aluminum-chromium-exhibit a peritectic reaction at the extreme aluminum end of the diagram. Preliminary work indi-cated that the aluminum-zirconium and certain other aluminum systems were similar in this respect. The present paper, the twentieth of a series from the Aluminum Research Laboratories, reports the results of a recent investigation of equilibrium relations in aluminum-zirconium alloys of high purity, which confirm the preliminary observations. PREVIOUS INVESTIGATIONS There has been only one investigation of the aluminum end of the aluminum-zirconium system. Sykes1 prepared and studied alloys containing 0 to 70 per cent Zr. The lowering of the freezing point of aluminum by the addition of zirconium was found to be very little, if any (less than 2°C.). He placed the solid solubility of zirconium in aluminum at room temperature between 0.57 and 0.97 per cent. A few other investigators have attempted to determine the com-position of the intermetallic compounds occurring in this system. Hönigschmid2 obtained the compound ZrAl3 as a by-product during the preparation of ZrSi2. He made no attempt to prepare other aluminum-zir-conium compounds. Weiss and Newmann3 prepared an alloy by heating aluminum with a double fluoride of potassium and zirconium. When this alloy was treated consecutively with caustic soda and hydrochloric acid, there was a residue, which contained approximately 72 per cent Zr and 28 per cent Al (Zr3Al4). Marden and Rich4 prepared an alloy in the same way, treated it with caustic soda, and obtained a residue of silver-white crystals, which contained 70 per cent Zr and 30 per cent Al (Zr3Al4).

Jan 1, 1939

By Harold R. Bradford

EXPANSION initiated during and after the war has placed industrial plants in new areas and increased reduction and manufacturing facilities in communities already established. With added expansion interest has grown in possible area contamination from waste products. Evolved flue waste contains many chemical contaminants that may or may not cause concern; however, atmospheric pollution has always been a problem to industrial communities. For some time effects attributed to small quantities of compounds of fluorine in various waste gases have been studied by industrial, medical, agricultural, and associated interests.1'2 Aside from an article by Churchill, Rowley, and Martin in 1948," little has been published on the subject of fluorine in coal except by foreign investigators. The first indication of fluorine compounds in coal was noted in England in 1934 by R. Lessing,4,5 who found that the presence of fluorine in Midland and West County coals was definitely established by etching of glass and by severe corrosion of porcelain fillings in a gas works scrubber. Etching of glass in a direct contact annealing kiln initiated research, and in 1944 four papers were published by H. E. Crossley,6-9 giving results of investigations of fluorine in coal of England by the Fuel Research Board, Department of Scientific and Industrial Research. These investigations studied methods of determining fluorine, the quantities present in various coal deposits, the geographical distribution of fluorine in British coals, occurrence of fluorine in minerals associated with coal, amounts of fluorine compared to other constituents of coal, the nature of fluorine compounds, and industrial significance of fluorine in coal. It was shown that British coals contain from 5 to 200 ppm of fluorine, which is probably present as fluorapatite [Ca10F2(PO4)6], often written as [3Ca3P2O8.CaF2]. The fluorapatite is intimately associated with shale in some coals and can often be separated from these coals along with the shales. H. E. Crossley8 also reported no correlation between the amounts of chlorine, sulfur, or ash and the amount of fluorine in different coals. He found, however, a relationship between the content of fluorine and phosporus in many British coals. Thus it should be possible to anticipate likely fluorine-rich coals from existing data giving phosphorus content. Behavior of the fluorine compounds of coal was compared with that of 12 fluoride-phosphate minerals in sink-float separations and solvent ex-

Jan 1, 1958

By D. W. Rudd, D. W. Vose, J. B. Vetrano

In an earlier paper the permeability character of Mo-0.5 pct Ti to hydrogen was described.' It was shown that this alloy is a more effective barrier to the passage of hydrogen than previously studied systems, i.e., copper,2 nickel,3 and several stainless steels.4 The permeability of Hastelloy B to hydrogen was investigated as a material having promising high-temperature structural properties which might have a low permeability to hydrogen. The general theory of permeation has been previously discussed,' and here only a summary of the more important results are given. It is found that except for very thin membranes, at low temperature, permeation of a gas through a metal barrier is determined by the rate of diffusion of the gas through the crystal lattice of the specimen, and that for hydrogen and the common diatomic gases, this passage involves dissociated particles as the diffusing species. The rate of permeation for hydrogen is therefore proportional to the square root of the pressure. It has also been found that the rate of permeation is inversely proportional to the thickness of the barrier. The apparatus used in this investigation was fundamentally the same as that employed in previous studies,' except that several simplifications result in the case of Hastelloy, since oxidation at the temperatures investigated is no longer a problem and welding of the specimen is relatively easy. A cross section of the membrane assembly is shown in Fig. 1. When finished, the assembly is about 5 in. long. The wall thickness is about 6 times the membrane thickness. The membrane (A) can be maintained at

Jan 1, 1963

By R. P. Rothwell

The milling of silver ores has arrived at a great degree of perfection in the mining districts of our Western States and Territories, and I hare thought the record of the practical results obtained at the present time, in a few of the principal districts, would prove of value arid interest to many of our members, both at home and abroad. An American silver mill is composed, in descending order from where the ore is dumped, of: 1st. A rock-breaker, usually of the Blake or Alden pattern; 2d. The battery of stamps, the number of which varies from 5 to 120, generally in batteries of 5 or 10 heads, so arranged that a single battery may stand while the others are running; 3d. The tanks where the crushed ore settles (if it is a met stamping-mill), or of a drying-floor if the crushing is done dry; 4th. Amalgamating pans ; 5th. Settling pans ; 6th. Agitators or pans in which mercury escaping in the tailings is caught; 7th. Blanket sluices, over which the tailings run, and where mercury and unamalgamated sulplides are saved. A reference to the engravings (see plate), which show one of the latest forms of an 80stamp silver-mill run by a turbine water-wheel, will show clearly the arrangement of the several parts. THE ONTARIO, UTAH, SILVER MILL. One of the best examples of a silver-mill, and at the same time one of the most successful concerns in the West, is the mill of the Ontario Silver Mining Company, near Salt Lake, in Utah. This mill treats the ore from the Ontario mine, ore which at present is very base, being composed of zinc, lead, and silver sulphides and silver chloride in a quartz gangue. This ore has become baser as the mine attained greater depth, though the vein holds its own, or rather increases, both in thickness and richness. The mill is managed in a skilful and economical manner, though the necessity for

Jan 1, 1880

By Milo Krejci

(Butte Meeting, August, 1913.) THE plant and quarries of the Inland Portland Cement Co. are located at Metaline Falls, Wash., about 128 miles north of Spokane, on the Pend Oreille river, and within 10 miles of the Canadian border. The plant is one of a chain of cement plants controlled by the Lehigh Portland Cement Co., of Allentown, Pa. Work on this plant was commenced in June, 1910, and was completed in April, 1911, but on account of some delays in 'the construction of the power plant, the works were not put into operation until August, 1911. Since then it has been in continuous operation and has furnished the Inland Empire with a high grade of cement. Fig. I is a view and Fig. 2 is a plan of the works. Water Power Development.-The source of the water supply for the hydro-electric plant of the Inland Portland Cement Co. is Sullivan lake, a body of water approximately 5.5 miles long and 0.5 mile wide, situated in the Kaniksu Forest Reserve. A wooden crib dam was installed so as to raise the elevation of the lake 25 ft., and the additional storage capacity was taken up by the diversion of Sullivan creek into the lake by means of a wooden flume, 0.25 mile long, 6 by S ft. in cross-section, and a ditch 1,200 ft. long. The water from the lake follows the natural water course to an intermediate storage reservoir, which was created by the construction of an earthen dam. This pond wits used in connection with the saw mill which was installed at this point. Besides the earth dam, there was also built a crib, at the point shown in the sketch map, Fig. 3. This crib dam is 35 ft. high. From this point the excess water follows the natural course of Sullivan creek to the Pend Oreille river.

Jan 7, 1913

By R. Grierson, L. J. Bonis

The high-temperature Strength oF TD nickel has been observed to be dependent upon the previons thermal and mechanical history of the material. Variations in both the level and the anisotropy of strength have been observed. 01 this paper- these variations are correlated with the storing of annealing resistant elastic strain energy in the matrix of the TD nickel. An x-vay line -broadening tecknique is used to measure the maLrTis elastie strain. THE inclusion of a finely dispersed second phase into a ductile matrix has long been recognized as an extremely effective method of strengthening the matrix both at high and at low homologous temperatures. It has been found, however, that the factors which determine the high-temperature strength are not the same as those which are important at low temperatures. Below 0.5 Tm the size and distribution of the second phase particles are of prime importance in determining the strength,')' while above this temperature the strength is mainly dependent upon the previous thermal and mechanical history of the alloy,3-7 This paper is primarily concerned with explaining the response of the high-temperature mechanical strength of one of these alloys (DuPont's TD nickel) to various thermo-mechanical treatments. It will be shown that this response is not associated with the occurrence of any form of dislocation substructure within the matrix of the alloy. It has been found, however, that a correlation does exist between the elastic strain level in the matrix and the previous thermomechanical history of the alloy and that the observed changes in elastic strain level parallel the measured changes in high-temperature strength. It therefore must be concluded that variations in high-temperature strength are a direct result of the variations in elastic strain level. MATERIAL TD nickel contains approximately 2 vol pct of Tho2 in an unalloyed nickel matrix. It is formed, as a powder, by a chemical technique and this powder is compacted to form ingots which are then extruded to give 21/2-in.-diam rod. Rod of smaller diameter is prepared from the as-extruded rod by swaging. In the studies reported in this paper, 1/2-in.-diam rod was used. This rod received an anneal of 1 hr at 1100°C prior to being used in any of these studies. EXPERIMENTAL TECHNIQUES Two methods were used to examine the structure of the nickel matrix of the TD nickel. These were: 1) transmission electron microscopy; 2) the analysis of the position and profile of X-ray diffraction lines obtained using the nickel matrix as the diffracting media. To prepare thin foils for electron-microscopical examination, slices of TD nickel approximately 0.050 in. thick were cut from the as-received 1/2-in.-diam rod. These were then chemically polished down to 0.045 in., rolled to 0.009 in., given a predetermined heat treatment, and thinned, using a modified Bollman technique, to provide the foils for observation. All observations were carried out at 100 kv, using a Hitachi HU-11 electron microscope. Specimens of the undeformed rod were prepared by grinding down the 0.050-in.-thick slices to approximately 0.015 in. and then thinning chemically and electrolytically to give the thin foils. The X-ray specimens were prepared by rolling 0.375-in.-thick rectangular blocks down to 0.075 in. The surfaces of the rolled material were ground flat, chemically polished to remove the layer disturbed by the grinding, and given a predetermined anneal in an inert atmosphere. They were then ground lightly to check their flatness and given a final chemical polish prior to being examined. The X-ray diffraction line profiles were measured using an automated Picker biplane diffractometer. A special specimen holder was built to allow a more accurate and reproducible positioning of the specimen. The line profiles were determined by carrying out intensity measurements at intervals of either 1/30 deg or 1/60 deg over a range of 3 deg on either side of the nickel peaks of interest. A piece of pure nickel which had been recrystallized to give a large grain size was used as a standard to give the X-ray line profile generated by a strain-free matrix. The analysis of the X-ray diffraction line profiles is a modification of that due initially to Warren and Aver-bach8and has been described elsewhere.3 This analysis gives a measurement of two parameters associated with the structure of the nickel matrix. These parameters are: 1) the size of the coherently diffracting domains within the nickel matrix; 2) the magnitude of the elastic strains in these domains. Both of these parameters are first determined in terms of a Fourier series. These series are obtained from other Fourier series which describe the measured profile of the X-ray diffraction lines. Thus, for both the coherently diffracting domain size and the elastic strain level, it is possible to plot Ft (the Fourier coefficient) against t (the term in the Fourier series), where t can be expressed in terms of a distance L and the Fourier coefficient Ft(S) (associated with elastic strain level) can be expressed in terms of the root mean square strain (e2)1/2. Thus a plot of (F 2)1/2 vs L can be obtained. Plots of this type are shown graphically in Figs. 6 and 8. Interpretation

Jan 1, 1968

By Charles Clayton

CAST-STEEL runners, while not interesting from a commercial standpoint, furnish valuable material for microscopic study. Foley1 found not only the usual ingot structure, but zones of Widmannstattian structure, which he explains as due to differential crystallization. The writer, in examining nickel-steel runners, found a type of pro-eutectoid ferrite that is unusual and most probably new. The runner in question was 8.75 cm. (3.5 in.) in diameter and analyzed at its center 2.69 per cent, nickel and 0.350 per cent. carbon and at its edge 2.62 per cent. nickel and 0.359 per cent. carbon. The macrostructure, which is the usual type, is shown in Figs. 1 and 2, which are a cross-section and the longitudinal surface, respectively. Slight segregation of ferrite can be seen near the center of the segment and at other points near the edges of polyhedral grains. Stead's reagent brings out the dendritic structure within the grains as shown in Figs. 3 and 4. This texture is what would be expected of such a steel. Figs. 5 to 10 show the peculiar swirls of pro-eutectoid ferrite, the finding of which prompted this paper. These swirls, or eddies, if such a term can be applied, occur in all parts of- the runner and in all parts of the individual grains. I he tipper left-hand figure shows this ferrite at a grain boundary; the middle left-hand figure shows the inner portion of a grain; and the lower left-hand figure shows these swirls at the edge of a grain which is also the outer edge of the runner. Straight-lined ferrite associated with swirls is found in the areas of Figs. 11 and 12. The texture of the carbon-bearing constituent of the runner is shown to- some extent in Fig. 12, the pearlite being very fine or sorbitic. Higher magnification does not bring out any new features either in the peculiar ferrite or in the pearlite. Figs. 13 and 14, at 240 diameters, show the curved and straight-lined ferrite.

Jan 3, 1920

By R. W. Stormont, F. Wald

The phase diagram of the Pseudobinary section PbTe-Fe was determined. It was found to contain a monotectic and a eutectic reaction, the latter one taking place at 14 at. pct Fe and 875° * 5°C. The solid solubility of iron in PbTe was found to be 0.3 at. pct by electronmicroProbe analysis. No solubility of PbTe was detected in iron. Slight deviations from true pseudobinary behavior were found to occur in the range of - 5 to 10 at. pct Fe. In the course of a general investigation of reactions of various metals with lead and tin telluride,' the lead telluride-iron system was reinvestigated. It had been established much earlier than iron does not chemically react with lead telluride but forms a eutectic with a melting point of 879" The eutectic composition or other related information has never been reported, but for a number of years iron has been in general use for contacting of lead telluride and lead telluride alloys for thermoelectric applications. It seems therefore desirable to clarify the exact constitution of the system to furnish a base for the long-term evaluation of bonds made between lead telluride and iron either by pressure contacting or by brazing methods. I) EXPERIMENTAL METHODS Lead telluride-iron alloys were prepared in 10-g charges, using premelted lead telluride. This material was prepared from high-purity, semiconductor-grade lead and tellurium obtained from the American Smelting and Refining Co. and described as 99.999 pct pure. The iron used was "Armco" iron; the major impurities found here were 0.02 pct C, 0.018 pct Si, and 0.015 pct Cr. All remaining impurities were less than 0.01, the total of all impurities not exceeding 0.15 pct. Charges were prepared in closed quartz arnpoules which were evacuated and in some cases backfilled with high-purity argon to retard excessive lead telluride evaporation and deposition in slightly cooler parts of the ampoule. For high iron concentrations, this can lead to total separation of the constituents, since the vapor pressure and the sublimation rate of PbTe are quite high.4 Nevertheless, since the ampoules are closed, no change in overall composition was expected and the nominal composition of all alloys was assumed to be retained. X-ray diffraction analysis, thermal analysis, and microsections were used in the evaluation of the alloys. The nature of the system was such that X-ray diffraction was not particularly helpful. It merely served to establish that at all concentrations PbTe and a! iron were in equilibrium at room temperature. Thermal analysis was carried out by taking direct temperature vs time curves on a Sargent recorder where a width of 10 in. was kept as 1 or 0.5 mv by use of an automatic bucking voltage network. Quartz ampoules with minimized dead space, coated with boron nitride and fitted with a thermocouple reentrant, were used as containers for the charge. At high temperatures and over long periods of time, boron nitride reacts with iron. For the thermal analysis runs, however, this was not significant. More significant was the fact that the vapor pressure of PbTe at some of the meas -uring temperatures apparently exceeded I atrn quite considerably. This, in some cases, caused the slightly softened quartz tubes to blow out if great care was not taken to contain them and minimize time and temperatures used. As containers pure nickel tubes were used which also served to avoid temperature gradients in the quartz ampoule. Nevertheless, the experimental difficulties at high temperatures were severe and the monotectic temperature could therefore not be determined accurately. In general, the accuracy reached by the thermal analysis setup in this case is *4"C as determined with gold, silver, and tin, under the conditions of analysis here. Inherently, the apparatus is capable of reaching accuracies better than i 1°C. Also, difficulties were encountered in microsection-ing. They were related to polishing, since it is rather difficult to avoid pulling the iron out of the weak and brittle lead telluride matrix. It proved best to follow a procedure where, after grinding to 600 grit on carborundum paper, a polish with 6 p diamond was used on nylon cloth. Finally, #3 "Buehler" alumina and an automatic polisher were used for -5 min only, to avoid relief. The best etching results were achieved with

Jan 1, 1969

By C. S. Cole

CO-CHAIRMAN CARTER S. Cole l-The stimulus of war definitely increases interest in the subject we are discussing at this Symposium. There have been, in the past, other symposia on this subject and there probably will be still others in the future, but I feel sure that this one will go down as one of the most important that have ever been held on the subject. In 1918 A.S.T.M. held a Symposium on Stress- Corrosion Cracking that was confined entirely to brass, because at that time few people were interested in the phenomenon as it applied to other metals. Again under the stimulus of war, we are gathered to discuss the subject, but this time brass alone is but part of our interest. It is interesting to note more papers on brass will be presented than there were in the 1918 session, but these brass papers, you will also note, comprise less than half our program. Aluminum, magnesium and

Jan 1, 1945

By C. E. Birchenall, J. R. Stubbles

ThE equilibrium between lead, lead sulfide (PbS), and atmospheres of H2 and H2S has been determined previously by Jellinek and Deubel,' and SudO.' Blbem and Kroger3,4 used Jellinek's data to calculate the sulfur dissociation pressures of PbS crystals (of

Jan 1, 1960