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By H. l. Burghoff, D. E. Lawson

The presence of tellurium in copper and, by inference, in copper alloys, has been considered seriously detrimental and has been avoided. In particular, very small amounts of tellurium have been found to produce red-shortness, although the effects on cold-working and ordinary physical and mechanical properties have not been known so definitely. References in the literature are few, but as long ago as 1881, Eglestonl reported that 0.083 per cent tellurium in fire-refined copper rendered the copper red-short and therefore worthless for hot-rolling. In hot-rolling copper cakes containing this amount of tellurium, he found that fine cracks appeared in the cakes on the first pass through the rolls, the cracks opening further in successive passes. When cold, the metal was said to be tough and malleable. A few years ago, during the course of an investigation in our laboratory on copper-base alloys, it was found that tellurium-bearing alloys could be machined much more freely than similar alloys not containing tellurium. The study was pursued further in this direction, and considerable data were obtained, which indicated that certain tellurium-bearing alloys might have properties of commercial interest. The work eventually led to patent protection,2 a wide range of tellurium-bearing copper-base alloys being covered. This article presents results obtained on the effect of tellurium on the mechanical properties of three copper-base alloys: commercial bronze (90 Cu, 10 Zn), 1.5 per cent tin bronze (98.5 Cu, 1.5 Sn), and silicon bronze (96 Cu, 3Si, 1 Zn). Several alloys were cast in each series, with tellurium content ranging from 0 up to about 1 per cent. The alloys were melted under charcoal in a clay-graphite crucible, using a high-frequency induction furnace, and were cast without undue difficulty in rod form, 15/8 in. in diameter. Charges for the zinc and tin series were made up from the following materials: cathode copper, electrolytic zinc, tin, and tellurium in slab

Jan 1, 1938

By T. S. Lundy, F. R. Winslow

DIFFUSION coefficients of Hf181 in the high-tem-perature bcc phase of reactor-grade hafnium were determined at temperatures of 1795° to 1995°C by standard lathe-sectioning techniques. The temperature dependence of the data may be described by an Arrhenius-type expression for this limited temperature interval. However, hafnium is classed with the "anomalous" bcc metals zirconium, titanium, and y uranium by the low values of Do and Q observed in this study. The hafnium metal was received as 1/2-in.-diameter crystal bar. Analyses by the Analytical Chemistry Division of Oak Ridge National Laboratory showed the major impurity to be zirconium— about 2.1 pct. The total interstitial content was about 225 ppm with 190 ppm of this oxygen. The Hf"' was supplied as HfC12 in HC1 solution by the Isotopes Division of Oak Ridge National Laboratory. The hafnium bar was cut into disk-shaped specimens 3/8 in. long. One of the flat faces of each specimen was metallographically treated and then the isotope was deposited by vacuum evaporation from a tungsten filament. A 3 by 3 in. NaI (Tl) crystal with a single-channel analyzer was used for counting y rays with energies of 0.3 to 0.7 Mev. The as-deposited layers of isotope had counting rates of about 200 counts per sec. Specimens were annealed in argon in a tantalum resistance furnace. Temperatures were measured with a microoptical pyrometer calibrated for the particular furnace sighting conditions. All sectioning was done by standard lathe techniques. Section weights were determined on a semimicrobalance. A density of 12.5 g per cu cm was used in determinations of section thicknesses. Activities associated with the various sections were measured and the penetration data were treated using the computer code by winslow.' In all cases, except for specimens annealed at temperatures below 1795°C, normal Gaussian penetration behavior resulted. At lower temperatures, plots of In A(x) vs x2 were nonlinear [~(x) = relative activity at a distance x from the

Jan 1, 1965

By H. l. Burghoff, D. E. Lawson

The presence of tellurium in copper and, by inference, in copper alloys, has been considered seriously detrimental and has been avoided. In particular, very small amounts of tellurium have been found to produce red-shortness, although the effects on cold-working and ordinary physical and mechanical properties have not been known so definitely. References in the literature are few, but as long ago as 1881, Eglestonl reported that 0.083 per cent tellurium in fire-refined copper rendered the copper red-short and therefore worthless for hot-rolling. In hot-rolling copper cakes containing this amount of tellurium, he found that fine cracks appeared in the cakes on the first pass through the rolls, the cracks opening further in successive passes. When cold, the metal was said to be tough and malleable. A few years ago, during the course of an investigation in our laboratory on copper-base alloys, it was found that tellurium-bearing alloys could be machined much more freely than similar alloys not containing tellurium. The study was pursued further in this direction, and considerable data were obtained, which indicated that certain tellurium-bearing alloys might have properties of commercial interest. The work eventually led to patent protection,2 a wide range of tellurium-bearing copper-base alloys being covered. This article presents results obtained on the effect of tellurium on the mechanical properties of three copper-base alloys: commercial bronze (90 Cu, 10 Zn), 1.5 per cent tin bronze (98.5 Cu, 1.5 Sn), and silicon bronze (96 Cu, 3Si, 1 Zn). Several alloys were cast in each series, with tellurium content ranging from 0 up to about 1 per cent. The alloys were melted under charcoal in a clay-graphite crucible, using a high-frequency induction furnace, and were cast without undue difficulty in rod form, 15/8 in. in diameter. Charges for the zinc and tin series were made up from the following materials: cathode copper, electrolytic zinc, tin, and tellurium in slab

Jan 1, 1938

By E. E. Malouf

With the continued development of low-grade porphyry copper deposits by open pit mining, substantial amounts of copper-bearing strip material have been accumulated in waste dumps adjacent to the many large mines. Since the end of World War II, the production of copper from leaching these copper-bearing wastes increased from approximately 4% of the total copper production to 10% by the early 1960's. Projected increases will probably raise this figure to 20 to 30% by the early 1970's. Furthermore, a gradual recognition of the economic feasibility of leaching mined-out areas is evident and will undoubtedly contribute additional production. Waste dumps in canyons and gulches on the periphery of open pit mines, mine stopes, caved areas, and abandoned open pits often contain substantial quantities of leachable rock ranging in concentration from 0.1 to 0.4% copper. Recent developments in the leaching of copper, mainly the recognition of bacterial oxidation of sulfide minerals combined with better under- standing of the control of the salt content of the leach solutions, both by adjusting the pH and/or by hydrolysis, are resulting in a greatly expanded recovery of copper from these hitherto uneconomic mine rejects. 11.5-1. Mechanism of Leaching. Leaching processes for the extraction of metal values from mine ore or waste may be classified for convenience as either chemical leaching or bacterial leaching. Chemical leaching is considered to be the extraction of soluble salts by metathesis in acidic, basic, or neutral water solutions. The reactions involved may be evaluated by chemical thermodynamics. Bacterial leaching, although a chemical process, is dependent on biological catalysis and this is generally a much more complex process. This justifies its separate treatment in the application to leaching. Acid ferric sulfate solutions are commonly employed in the mining industry to leach valuable metals from metal sulfide ores. The leaching mechanism is a reduction-oxidation reaction in which minerals are oxidized at the expense of ferric sulfate. Such chemical leaching is profitable when

Jan 1, 1968

By W. P. Frey

THE briquet plant of the Lehigh Coal and Navigation Co., at Lansford, Pa., has previously been referred to.1 It has passed. the stage of experiment and now rests,, on a foundation practically and financially sound. The purpose of this paper is to explain how success has been attained, and to set standards for the development of hard-coal briquetting which may eliminate future failures. All the conclusions are based on actual results, avoiding speculation and theory. Up to three years ago, the L. C. & N. Co. used coal-tar pitch as a binder in making hard-coal briquets. The plant operated with a monthly output of 300 to 600 tons and was unable to meet its own expenses. Naturally, no one was satisfied, especially as the ideals of a smokeless briquet were still unrealized. Then came the Dutch oil process, introduced in this country by the General Briquetting Co. of New York. This process uses as binder a small percentage of heavy residue of petroleum, which, being liquid, permits great economy of handling; it also did away with the most objectionable fumes of the former briquets. This oil2 is not absolutely smokeless; heating the fresh fuel to red heat liberates some low-volatile hydrocarbons, yielding a white smoke which is not objectionable. On the other hand, this oil adds to the briquet about 7 per cent. of volatile matter, giving the product a heating capacity equal to that of the best free-burning anthracite coal. The average silt used in the manufacture of these boulets averages 16.5 per cent. chemical ash, corresponding to 12,000 B.t.u. per pound of coal. The Hydrolene used as binder runs about 17,500 B.t.u. per pound, and approximately 7 per cent. of it enters into the mixture, hence 12,000 X 0.93 11,160 B.t.u. 17,500 X 0.07 1,125 B.t.u. Total 12,355 B.t.u. per pound of briquets

Jan 1, 1918

By Peter G. Groer

Several methods1-3 are being used to determine the WL and individual Rn-daughter concentrations in uranium mine atmospheres. The best of these methods is the one given in Ref. 3. According to this method, the WL and the Rn-daughter concentrations are determined from the total a-counts observed during three consecutive time intervals. Its only disadvantage lies in the fact that rather involved calculations are necessary to convert the observed counts into WL or pCi/l (picocuries per liter). There are, however, counting intervals that give simple weighting coefficients for the observed counts. This fact makes it possible to convert from a-counts to WL or pCi/l with the aid of a graph. After some trial runs on a computer the following equations emerged as the basis for the most practical procedure: [ ] NA, N.., and & stand for the number of RaA, RaB, and RaC atoms per liter of air. C(t1,t2) denotes the counts observed from time t. to time t2 (in minutes) after the end of the 5-min sampling period. E is the detector efficiency and V is the flow rate in liters per minute. With an accuracy loss of less than -5% one finds from [Eq. 1] by adding the corresponding terms: If the WL would have been calculated according to [Eq. 2] instead of using the graph, the result would have been 0.31. Since the values used for C's under [Eq. 3] represent the exact number of counts from a Rn-daughter mixture in equilibrium with 100/3 pCi of Rn the exact WL of this mixture can be calculated easily. The exact value is: [ ] This shows that the method is quite accurate for the 0.3 WL domain. The precision of the method excluding errors made in reading the graph can be estimated with the help of the following formula: [ ]

Jan 1, 1974

By M. B. Bever, A. K. Jena

In the investigation reported here, calorimetric measurements have been made to determine the heat of formation of the compound AuSb2 and the partial gram-atomic enthalpies of antimony and gold in dilute solution in liquid tin and their enthalpy interaction coefficients. In order to interpret the behavior of antimony and gold in dilute solution in tin, nonzero values are assigned to the energies of bonds between like solute atoms relative to the pure solute state. Sa.mples of the compound AuSb2 were prepared by melting stoichiometric amounts of antimony and gold (99.999 pct pure) in evacuated and sealed Vycor tubes, which were shaken vigorously and quenched in water. The ingots were annealed in evacuated and sealed tubes at approximately 700°K for 2 weeks. Metallo-graphic and X-ray examinations gave no indication of second phases or microsegregation. The samples were added from 273°K to tin-rich solutions in a solution calorimeter1 maintained at 623°K. The calorimeter was calibrated with tin; the heat content of tin, H623°K- H273°K, was taken as 4.08 kcal per g-atom.2 In each calorimetric run at least four additions were made. The total concentration of solutes in the bath at the end of any run did not exceed 1 at. pct. The measured heat effect of an addition was plotted against the average of the atom fractions x of Sb + Au in solution before and after that addition. From this plot the heat effect at infinite dilution h,,, and the composition dependence of the heat effect dh/dx in the composition range 0 < x < 0.01 were obtained. The results for the additions of antimony, mixtures of antimony and gold, and the compound AuSb2 are listed in Table I. The heat effect h on addition of a sample of the compound AuSb2 or a mechanical mixture of antimony and gold at 273°K to a tin-rich solution at 623°K can be expressed as:

Jan 1, 1969

By D. T. MacRoberts

A simple disturbance in a gas reservoir travels with a finite velocity which is nearly independent of the amplitude of the disturbance. As a result very complex transients may be set up which seriously affect observation at a well. The time of transient is much longer than commonly supposed. INTRODUCTION A change in pressure at a gas well is not propagated through the reservoir instantaneously but with a definite fin- ite velocity. Knowledge of the period ! of this transient is of value because: 1. Observations of pressure and flow-rate during the transient may affect interpretation of back-pressure tests. 2. Interference effects between wells may be used to determine continuity of formation. 3. Additional information concerning the physical characteris- tics may possibly be deduced from the behavior of a well during the transient. MATHEMATICAL DEVELOPMENT It will be assumed that the well is initially closed in and that the pressure is constant throlughout the reservoir. As the initial disturbance passes outward from the well it is further assumed that a logarithmic pressure distribution is established between the most distant point reached and the well, so that: <l> = ((/)r-<t>w) I ------------ + (/) . (1) Manuscript received at office of the Branch September 15. 1948. Paper presented at Branch Fall Meeting, Dallas. Texas. Oct. 4-6, 1948. r. = distance to any point between r and rw r = radius of drainge iw= radius of well (/) = potential (P for incompressible fluids, P2 for perfect gases) Up to the time the effect reaches the point r the production from the well will be: W= (Pr-P,,,) . (2) i b W = volume produced t = sand thickness F = fractional porosity Pr = reservoir pressure Pm = average pressure between r and rw Pb = atmospheric Pressure All pressures will subsequently be stated in atmospheres and the constant Pb will be omitted. This will be produced at a rate: dw t k (Pr³-PW2) do d 0 - . (3) log — Pw = pressure at the well k = permeability 0 = time = viscosity

Jan 1, 1949

By D. T. MacRoberts

A simple disturbance in a gas reservoir travels with a finite velocity which is nearly independent of the amplitude of the disturbance. As a result very complex transients may be set up which seriously affect observation at a well. The time of transient is much longer than commonly supposed. INTRODUCTION A change in pressure at a gas well is not propagated through the reservoir instantaneously but with a definite fin- ite velocity. Knowledge of the period ! of this transient is of value because: 1. Observations of pressure and flow-rate during the transient may affect interpretation of back-pressure tests. 2. Interference effects between wells may be used to determine continuity of formation. 3. Additional information concerning the physical characteris- tics may possibly be deduced from the behavior of a well during the transient. MATHEMATICAL DEVELOPMENT It will be assumed that the well is initially closed in and that the pressure is constant throlughout the reservoir. As the initial disturbance passes outward from the well it is further assumed that a logarithmic pressure distribution is established between the most distant point reached and the well, so that: <l> = ((/)r-<t>w) I ------------ + (/) . (1) Manuscript received at office of the Branch September 15. 1948. Paper presented at Branch Fall Meeting, Dallas. Texas. Oct. 4-6, 1948. r. = distance to any point between r and rw r = radius of drainge iw= radius of well (/) = potential (P for incompressible fluids, P2 for perfect gases) Up to the time the effect reaches the point r the production from the well will be: W= (Pr-P,,,) . (2) i b W = volume produced t = sand thickness F = fractional porosity Pr = reservoir pressure Pm = average pressure between r and rw Pb = atmospheric Pressure All pressures will subsequently be stated in atmospheres and the constant Pb will be omitted. This will be produced at a rate: dw t k (Pr³-PW2) do d 0 - . (3) log — Pw = pressure at the well k = permeability 0 = time = viscosity

Jan 1, 1949

By L. W. Bahney

The photograph, Fig. 1, shows the apparatus a little less than half size, consisting of a filtering-flask fitted with rubber stopper through which passes a bent glass tube, and an extraction-thimble fitted with rubber stopper through which passes a glass tube of 0.25-inch bore. Both tubes are connected by a short piece of rubber tubing. A section of a thimble is shown in the photograph ; the tube extends to within & in. of the tapered end. The object of using the thimble is to remove the acid from the beaker after all the copper has been precipitated. Time is saved, the copper is not exposed to the acid alone, and there are none of the losses attending ordinary filtration. I have accomplished these results by means of a piece of perforated platinum fastened in the end of a (0.25-in. bore glass tube and a filter-mat of asbestos, but after my supply of proper length fiber became exhausted I could not replenish it even after purchasing 14 lots from four different dealers. The above apparatus may be used to remove at least seven-eighths of a supernatant liquid from a settled precipitate without disturbing the latter. The application of the thimble is best shown by partly outlining the assay for copper, as follows: Dilute the acid solution of copper and other sulphates to 150 cc. in a 200-cc. Jena beaker, place on a hot plate, add 2 drops of concentrated HCl, then place a strip of aluminum in the beaker (this may be bent or straight, as desired). Connect the apparatus, as shown in Pig. 1, with a filter-pump having a strong suction. When the copper is precipitated, remove the beaker from the hot plate and insert the extraction-thimble alongside the strip of aluminum. The acid solution will be drawn through the porous tube. Wash the upper end of the aluminum strip with a jet of hot water, wash down the sides of

Jan 1, 1913

By L. W. Bahney

(Cleveland Meeting, October, 1912.) THE photograph, Fig. 1, shows the apparatus a little less than half size, consisting of a filtering-flask fitted with rubber stopper, through which passes a bent glass tube, and an extraction-thimble fitted with rubber stopper through which passes a glass tube of 0.2-5-inch bore. Both tubes are connected by a short piece of rubber tubing. A section of a thimble is shown in the photograph; the tube extends to within in. of the tapered end. The object of using the thimble is to remove the acid from the beaker after all the copper has been precipitated. Time is saved, the copper is not exposed to the acid alone, and there are none of the losses attending ordinary filtration. I have accomplished these results by means of a piece of perforated platinum fastened in the end of a 0.25-in. bore glass tube and a filter-mat of asbestos, but after my supply of proper length fiber became exhausted I could not replenish it even after purchasing 14 lots from four different dealers. The above apparatus may be used to remove at least seven-eighths of a supernatant liquid from a settled precipitate without disturbing the latter. The application of the thimble is best shown by partly out-lining the assay for copper, as follows: Dilute the acid solution of copper and other sulphates to 150 cc. in a 200-cc. Jena beaker, place on a hot plate, add 2 drops of concentrated HC1, then place a strip of aluminum in the beaker (this may be bent or straight, as desired). Connect the apparatus, as shown in Fig. 1, with a filter-pump having a, strong suction. When the copper is precipitated, remove the beaker from tine hot plate and insert the extraction-thimble alongside the strip of aluminum. The acid solution will be drawn through the porous tube. Wish the upper end of the aluminum strip with a jet of hot water, wash down the sides of

Nov 1, 1912

By H. Foster Bain

FROM time to time geologists and mining engineers, impressed by the heavy demands made on our mineral reserves&apos; by modern industry, and particularly by the steadily mounting rate of production necessary to meet that demand, have issued warnings as to the danger of exhaustion. There can be no dispute as to the fact that mineral deposits are exhaustible. New mineral, is not created to replace that taken from the earth and when a crop of mineral is once harvested another cannot be grown in the same area. The evidence of exhaustion &apos;of particular oreshoots, deposits, or even of whole districts is familiar to all who have mined. If one were to judge solely from the abandoned mills and prospect holes he would rightly conclude that mining is but a short-lived industry. If one were, furthermore, to assemble the data as to known reserves of almost any of the commonly used minerals, and divide them by the annual tonnage mined, he would come to the same conclusion. If, again, one were to consider the most carefully made estimates of competent men seeking to measure the earth&apos;s reserves of minerals and plot against them a projection of the curve of past consumption, he would be justified in viewing the situation with alarm.

Jan 1, 1930

THE man who forgot to mail the letters his wife gave him was for once justified at Tulsa, for envelopes, scratch paper and tablecloths were all in demand and through the two days of the meeting of the Petroleum Division, pencils were busy everywhere sketching out diagrams, drawing curves, figuring, or just taking notes. Those attending took the serious papers seriously, and discussion was wide-ranging but pointed. Despite the highly technical character of the papers presented, the chairmen had never to call for discussion; it was only necessary to say the paper was open for it. Both days the meetings lasted until after five in the afternoon, and it was enthusiastically voted to advance the meeting hour on Friday, in order to give more time. In all, ten papers, abstracts of which appeared in MINING AND METALLURGY for October, and copies of all but two of which were available in print, were presented in the two days, and no more could have been handled to advantage in that time. All but one of these dealt with problems of production engineering. That, the opening paper, was a general review of demand, supply and price in 1928, by Campbell Osborn, in which he argued for the price control of production and showed how the economic conditions determined development. J. Elmer Thomas presented a carefully prepared review of the same data, but came to somewhat different conclusions as to trend, and J. E. Pogue pointed out that in recent years it has been the manufacturing rather than the producing industries that have been notably profitable. These and other discussions were too long to be reported here, but will be printed in full later.

Jan 1, 1928

By J. K. Elliott, P. H. Kelly

Many engineering functions such as surface metering work and laboratory compressibility check points involve the use of liquid densities of light hydrocarbon mixtures at various pressures and temperatures. However, at the present time, no simple reliable method exists for determining density variation, particularly if the composition of the liquid is unknown. Consequently, a study was undertaken to develop and present a simple and accurate method of predicting density variation of a light hydrocarbon liquid with pressure and temperature, knowing only the density of the liquid at some condition. The experimental liquid compressibility data from API Project 37 by Sage and Lacey&apos; have been considered to be accurate within 0.5 per cent and cover a wide range of pressure (14.7 to 10,000 psia), temperature (100" to 400°F) and molecular weight (up to 150). From these data, a set of liquid density curves, which relate density to pressure, temperature and molecular weight, was developed. These curves make it possible to predict density variation with pressure and temperature. Compared to extensive laboratory compressibility data on a complex, light hydrocarbon liquid, the use of the liquid density curves resulted in an average error of less than 0.5 per cent. Based on the results of this analysis, it is concluded that the set of liquid density curves developed from the data of Sage and Lacey provides an accurate and simple method for predicting the density variation of light hydrocarbon liquids when the density at some condition is known. These curves should be very helpful in many engineering calculations, particularly in the surface metering of light hydrocarbon liquids. INTRODUCTION Many situations arise in field and engineering laboratory work, such as reservoir engineering studies, check of experimentally determined laboratory data and orifice flow-meter formulas, where liquid density factors at various pressure-temperature conditions are required. Also, the need for accurate light hydrocarbon liquid information has become more important with the advent of miscible-type displacements for secondary recovery purposes in oilfield operations. Several reliable methods are available1 - "or determining the density of liquid hydrocarbons if the composition of the liquid is known. However, there is a definite lack of methods for accurately determining the variation of density when the composition of the liquid is unknown. The purpose of this study is to review the various methods for determining hydrocarbon liquid densities and to develop a simple and reliable method of determining variation in density of light hydrocarbon liquids with pressure and temperature when the compositio~n of the liquid is unknown. METHODS FOR DETERMINING DENSITY OF LIQUIDS OF KNOWN COMPOSITION Sage, Lacey and Hicks&apos; have proposed a method to predict the density of light liquid hydrocarbons by using partial molal volumes. Data are available on experimentally developed partial liquid volumes of hydrocarbons over a rather limited range of temperature, pressure and composition. The partial mold volume method has proved satisfactory for determining the density of some hydrocarbon liquids when the composition is known. Within the range covered in the Sage, Lacey and Hicks1 data, the results agree within about 3 per cent of the experimental values. Hanson mentions the limitation of this method to a composition range of approximately 10 per cent by weight of methane, which will not allow this correction to cover most low molecular weight-light hydrocarbon liquids. Standing and Katz2 studied data on light hydrocarbon-liquid systems containing methane and ethane at high temperature and pressure and have presented a method for determining liquid densities, assuming additive volumes for all components less volatile than ethane and using apparent densities for methane and ethane. The compressibility and thermal-expansion curves used by Standing are based on assumptions that compressibility of a hydrocarbon liquid at temperatures below 300°F is a function of the liquid density at 60°F and that thermal expansion of the liquid is affected little by pressure. The information required to use this technique with an example problem is furnished by Standing.&apos; Hanson eports an average error of - 0.5 per cent using the method of apparent densities in calculating liquid densities of several volatile hydrocarbon mixtures. However, as implied, the apparent density method is not applicable for liquid density calculations when the composition of the liquid is unknown. Watson- as presented a method

By R. W. Cahn, C. D. Graham

The rate of growth of a single grain growing into a strained aluminum single crystal, measured by the conventional heat-cool-etch technique, is shown to decrease with time at temperature. The growth rate measured by means of X-rays, with the sample continuously at temperature, is found to be linear. Evidence is presented to show that the decreasing growth rate obtained by the conventional technique is due to abnormal recovery in the strained grain, and that the recovery in turn results from the heating and cooling cycles, rather than from the effects of etching. The experimental apparatus is described in an appendix. FREQUENTLY, the rate of grain boundary motion during recrystallization is determined by heating a sample to a known temperature for a given time, cooling to room temperature, and etching to reveal the boundary position. The cycle of operations is repeated as many times as necessary to establish the rate of boundary motion. Although this heat-cool-etch technique has been used by a number of workers over a period of many years,&apos;-!&apos; other investigators have encountered difficulty with the method."&apos;. " They have attributed the erratic results to the effects of repeated heating and cooling, or of etching, or both, and have adopted an alternative experimental procedure in which a number of identical samples are employed, each sample being cooled and etched only once. This alternative method ove1.comes some difficulties, but introduces others. In particular, the incubation periods of the observed grains are unknown: any effect of crystal orientation on growth rate cannot be determined easily. A preferable method would be to measure the motion of a recrystallizing grain boundary with the sample at temperature without etching," but such measurements have in the past been restricted to nonmetals. This paper describes the construction and operation of a device, the goniometer furnace, with which the position of a moving grain boundary between a recrystallizing grain and the strained single crystal into which it grows can be measured by means of X-rays, with the sample maintained continuously at temperature. Goniometer Furnace The operating principle of the goniometer furnace is shown in Fig. 1. The sample, in the form of a bicrystal strip, is surrounded by a furnace, not shown in the sketch, and can be rotated about the two axes A and B which intersect at the point where the X-ray beam strikes the strip. The strip is oriented so that one of the two grains gives a strong Bragg reflection, which is detected by a suitably placed Geiger-Miiller counter coupled to a counting-rate meter When the strip is moved parallel to its own length in the furnace, arrow C, so that the X-ray beam strikes the second grain, there is in general no strong reflection. By noting the position of the strip at which the drop in Geiger counter reading occurs, it is possible to determine the position of the boundary. Measuring the change in boundary position with time at temperature gives the rate of growth of the recrystallizing grain. Details of the construction and operation of the goniometer furnace are given in the Appendix. Measurements showed that the temperature in the furnace was uniform within ±10°C over its working length of about 28 cm. The temperature at the measuring position, i.e., at the point where the X-ray beam struck the sample, was estimated to be constant within ±2oC. Using the goniometer furnace, the position of a stationary boundary could be measured with a reproducibility of ±0.3 mm. At elevated temperatures, 500" to 625"C, with the boundary in motion and the X-ray reflection less sharp, the estimated accuracy of each measured boundary position dropped to about ±1 mm. Experimental Results The test pieces were single crystals of 99.6 pet A1 —principal impurities 0.19 pet Fe and 0.12 pet Si— 1 mm by 1 cm in cross section and 6 to 10 cm in length, grown by the strain-anneal method. This relatively low purity material was used because of the difficulty encountered in producing strain-anneal single crystals of very high purity—99.996 pet—

Jan 1, 1957

By S. G. Cupschalk, J. J. Wert, R. A. Buchanan

The uniaxial deformation of thermally ordered and disordered polycrystalline Cu3Pt was studied by means of the X-ray line - broadening analysis according to Warren and Averbach and the extension of this analysis to ordered fcc materials by Mikkola and Cohen. Because of the heat treatment history, extinction had a pronounced effect on the X-ray spectra of ordered and disordered C%Pt at small plastic strains. After an appropriate correction for extinction, the long-range order in thermally ordered ChPt was found to decrease at a slow constant rate with plastic strain. Furthermore, the antiphase domain probability increased at a constant rate to 17.5 pct strain. The effective particle size behavior indicated that the stacking fault energy is lower in ordered than in disordered Cu3Pt. Analysis of the stress-strain curves shouled that ordered Cuzt has a slightly lower yield Point but a much higher work-hardening rate than disordered Cu3Pt. THE presence of long-range order in a solid-solution alloy has a marked effect on its mechanical properties. While this effect has been known qualitatively for many years, it was not until recently that detailed investigations have been performed to determine the exact role long-range order plays in this strengthening mechanism. The development of an advanced, quantitative. X-ray diffraction analysis by Warren and Averbachl and the extension of this analysis to the L1, type super lattice by Mikkola and cohen2 have greatly accelerated research in this field. The research reported in this paper consisted of two primary phases. The first phase was to determine the effect of long-range order on the tensile properties of polycrystalline Cu3Pt. This objective was accomplished by comparing the stress-strain behavior of thermally ordered CusPt to that of thermally disordered CusPt. The second phase of the research was to determine the difference between the atomic arrangements in thermally ordered and thermally disordered Cu3Pt as a function of uniaxial deformation and thereby gain a deeper insight into the mechanism by which long-range order affects the tensile properties. This second objective was accomplished by applying the Warren-Averbach method of peak profile analysis to the X-ray diffraction patterns obtained from ordered and disordered Cu3Pt after given amounts of uniaxial deformation. EXPERIMENTAL PROCEDURE The Cu3Pt was prepared by vacuum melting and casting. After a homogenization anneal, the ingot was cold-rolled to sheet form. Two tensile specimens with gage sections of 2.50 by 0.500 by 0.115 in. were carefully machined from the sheet. The specimens were polished with a final step of 600-grit paper to insure smooth diffracting surfaces. Finally, one specimen was heat-treated to yield an average grain diameter of 0.016 mm and an initial degree of long-range order, S, of 0.825. The other specimen was water-quenched from above the critical temperature, 645"C, to yield an average grain diameter of 0.017 mm and zero long-range order. The heat treatment history of each specimen is shown in Table I. The tensile tests were performed utilizing a Research Incorporated Model 900.95 Materials Testing System. This unit employs a closed-loop feedback system which maintains a constant strain rate through an extensometer clipped to the gage section of the tensile specimen. A strain rate of 1.32 i0.02 x 10"4 sec-&apos; was employed in testing both specimens. In the X-ray diffraction analysis, a General Electric XRD-5 diffractometer equipped with a pulse-height analyzer set for 90 pct efficiency was employed. The goniometer speed selected was 0.2 deg, 20, per min. Filtered Cu radiation was used for all peaks and all peaks were chart-recorded. Because of nonuni-form grain size. it was necessary to spin the specimens during X-ray analysis in order to obtain reproducible integrated intensities. The spinning rate was 2000 i100 rpm. The application of the Warren-Averbach method of peak broadening analysis to a diffraction pattern is very time consuming if done manually. In this research, the calculations involved were performed with the aid of a computer program by wagner.3 As reported by Wagner, the program is written in Fortran TV computer language. It was modified to Fortran I1 so as to be handled by the IBM 7072 computer at Van-derbilt University. In the X-ray diffraction analysis of uniaxially deformed Cu3Pt, the 100, 200. 400. 111, and 222 reflections were recorded from the initially ordered sample after &apos;plastic strains of 3.0, 6.0, 9.0, 12.0,

Jan 1, 1970

By W. Rostoker

Single isothermal sections were constructed for the titonium-rich corners of the systems Ti-Fe-O, Ti-Cr-O, and Ti-Ni-0 with a view to locating the shape and disposition of the ternary intermediate-phase fields for the compounds isomorphous with Fe3W3C. IN a previous note,&apos; it was reported that a group of ternary intermediate phases existed which occurred in the general composition range Ti,X,O-Ti&O where X was one of the following elements: copper, nickel, cobalt, iron, or manganese. In two instances, binary intermediate phases occurred (Ti²Cu and Ti²Ni) which appeared to be isomorphous. The X-ray diffraction patterns of the phases could be indexed on a cubic lattice whose cell edge was of the order of 11 kX. Karlsson2 stated that the line extinctions and line intensities indicated that these phases were isomorphous with Fe³W³C and therefore belonged to the space group Oh. This author also noted that no unique phase of this type occurred at the composition Ti,Cr,O. This latter statement was accepted as true at the time the previous technical note was written.&apos; However, work continued along these lines and that reported here has shown that a phase isomorphous with Fe³W³C does exist in the vicinity of the composition Ti³Cr³O but not at or near Ti4 Cr²O. The lattice parameter of this phase was found to be 13.01 kX. Metallographic examination of both as-cast and annealed specimens of these supposed ternary oxide phases disclosed structures which were far from single phase in many instances. It was considered a point of some interest to locate more positively the composition coordinates of the single-phase fields. To this end, single isothermal sections for the systems Ti-Fe-O (1000°C), Ti-Cr-0 (1000°C), and Ti-Ni-0 (900"C) were constructed. Phase relationships were studied by both X-ray diffraction and metallotrra~hic methods. Allovs were prepared as 10 g buttons by melting in a noncon-sumable electrode, water-cooled copper crucible arc-melting furnace using a helium atmosphere. Oxygen was introduced quantitatively by the use of weighed amounts of TiO² or TiO. Iodide titanium and the purest available alloying metals were used. All results are discussed in terms of the nominal composition of the melts. Previous experience with making oxygen-rich alloys had shown that oxygen losses were not significant if a homogeneous melt was produced. Weight-loss measurements were used to check loss in metallics during melting. Anneals were conducted in evacuated Vycor bulbs, and annealing times ranged from 24 hr at 1000 °C to 48 hr at 900°C. To achieve equilibrium in certain sluggish alloys, seven-day anneals were used. Debye-Scherrer powder patterns were taken in a 14 cm diam camera using filtered CuK radiation (K² = 1.541232 kX; K., = 1.53739 kX). Specimens were prepared by crushing and screening previously annealed buttons. In general, the X-ray diffraction results were used to identify the major phases, while the metallographic examinations were more useful in indicating the number of phases present. By the use of the combined results and general fundamental rules governing ternary equilibrium, it was possible to construct isothermal sections in good detail. In some instances where auxiliary lattice-parameter data were available, it was possible to lay down tie lines and to locate more positively corners of three-phase fields. Isothermal Section of the System Ti-Fe-O at 1000°C The binary systems Ti-O³ and Ti-Fe4 have been published. Binary phases, TiO, TiFe, and TiFe2, are likely to be encountered in the titanium-rich corner of the system. The structures are NaCl (Bl), CsCl (B2), and MgZn, (C14) types, respectively. Although preliminary X-ray diffraction studies indicated the presence of a ternary phase in the composition range Ti,Fe,O-TiJ?e,O, metallographic examination of two specimens at these compositions revealed the presence of other phases. Thirty-eight alloys were used to delineate the phase boundaries of the isothermal section illustrated in Fig. 1. The five almost single-phase ter-

Jan 1, 1956

By F. V. Lenel, G. S. Ansell, J. A. Dromsky

The growth of aluminum oxide particles in a nickel matrix was studied eve?. the temperature vange of 2140° to 2470°F. The instability of the dispersed alumina was shown to be independent of the crystal structure of the alumina. The activation energy for the growth of the dispersed alumina was found to be 84.7 1 2.0 kcal. The particle radius increased as a function of time. These results indicate that the growth is not diffusion controlled. It is believed that the rate controlling mechanism is the dissolution of the aluminum and oxygen atoms into the nickel lattice. THE strength properties of alloys which consist of a finely dispersed second phase in a metallic matrix depend upon the spacing between the second phase particles. It is therefore desirable to achieve very fine dispersions in these alloys. Furthermore, to retain the properties these very fine dispersions must be stable during fabrication and service of the alloys. The best known of the dispersion strengthened materials, the SAP type alloys, which consist of a dispersion of aluminurn oxide in aluminum, have exceptionally good stability up to the melting point of aluminum. There is evidence, however, that other dispersion strengthened alloys, even those consisting of refractory oxides in a metal matrix, may be less stable. This investigation is concerned with the stability of Ni-Al2O3 alloys in the temperature range in which these alloys are usually fabricated. The mechanical properties of Ni-Al2O3 alloys at elevated temperatures have been previously investigated by Crelnens and rant,&apos; and Gregory and Goetzel.2 The behavior of these alloys in stress rupture tests appears to indicate that at temperatures below 1800°F they are highly stable. There is some doubt, however, as to their stability at the higher temperatures used during the conventional fabrication. Cremens and Grant, in preparing their test alloys, cousolidated, by powder metallurgical techniques, nickel powders as fine as 0.13 µ diam and alumina powders as fine as 0.018 µ. Metallo- graphic examination of the alloys following fabrication revealed that none had interparticle spacings of less than 2 µ. Considering the size of the original component powder particles, it is likely that the dispersions coarsened during fabrication. Gregory and Goetzel, in their studies of extruded alloys of 80 pct Ni—-20 pct Cr matrixes with nonmetallic dispersion, observed a definite coarsening of the alumina dispersions in alloys sintered at 2280°F as cantrasted to those sintered at 2000oF. Similar observations on the spheroidization and growth of thoria particles finely dispersed in a nickel matrix were made by D. K. Worn and S. F. Marton.3 As a result of such coarsening, much of the effort expended in the preparation of very fine powder mixtures would be lost. The mechanical properties of the alloys which had experienced coarsening would be expected to be poorer than if the original dispersions had been retained. EXPERIMENTAL PROCEDURE Ni-Al2O3 alloys were produced from powder prepared by a coprecipitation technique. Aluminum hydroxide and nickel hydroxide were coprecipitated from chloride solutions of the metals. The mixed hydroxides were calcined to form metal oxides and the nickel oxide in the mixture was selectively reduced to nickel by treating it in hydrogen. Specimens were compacted from the resultant powder which consisted of a fine, uniform mixture of aluminum oxide and nickel particles. The compacts were sintered by resistance hot pressing4, a densification technique which requires exposure times of the order of only a second or less at elevated temperatures. A conventional sintering process was not used, since the temperature required for densification would have to be in the region in which the stability of the dispersion was to be studied. A series of hot pressed specimens were treated in hydrogen at temperatures from 2140o to 2470°F (1171o to 1355oC, for times up to 120 hr. Changes in the microstructures were studied by electron microscopy using the two-stage preshadowed carbon replica method.5 In performing a lineal analysis on a series of micrographs from each specimen it was found more convenient to determine the mean free path between alumina particles rather than particle radii as the parameter of growth. Although these quantities are directly proportional for only spherical particles, the alumina particles in these alloys

Jan 1, 1962

By Donald B. Gillies

THE great source of iron ore for the furnaces of this country has been the Lake Superior district. Ore was first discovered there in 1844, and the first shipments made via the Great Lakes in 1852 to a furnace at New Castle, Pa. The stream of ore from that region increased slowly to exceed a million tons in 1873, and did not reach 10 million tons until 1895. By 1901 it exceeded 20 million tons, and in 1907 over 40 million tons. Total Lake Superior output through 1948 was about 2500 million long tons. Outside the Lake Superior district are the Southern district, including mainly Alabama, Georgia, Missouri, and Texas; the Eastern district of New York, New Jersey, and Pennsylvania; the Western district embracing Wyoming, Utah, and California.

Jan 1, 1949

For the year ending February, 1923 PRESIDENT ARTHUR S. DWIGHT, District 0 NEW YORK, N. Y. PAST PRESIDENTS HERBERT HOOVER, District 4 WASHINGTON, D. C. EDWIN LUDLOW, District 0 NEW YORK, N. Y. FIRST VICE-PRESIDENT J. V. W. REYNDERS NEW YORK, N. Y. TREASURER CHARLES F. RAND NEW YORK, N. Y. SECRETARY FREDERICK F. SHARPLESS,. . . . . NEW YORK, N. Y. ASSISTANT SECRETARY PERCY E. BARBOUR NEW YORK, N. Y.

Jan 7, 1922