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By Lyden, Joseph P.

THE Picher Mining Field, fig. 1, which lies between Baxter Springs, Kansas, and Commerce, Okla., is the most intensely mineralized and the largest zinc-lead ore producing area in the Tri-State District of Missouri, Kansas, and Oklahoma. It has a vast lateral extent of underground workings that is unequaled for the observation of the geology of zinc-lead ore bodies in sedimentary horizons; and thousands of churn drill holes in the unmined areas supplement the underground observations with useful data for the interpretation of the geology. This paper is confined to the ore deposits of the Picher mining field. The reader is referred to the bibliography for the general geology of the Tri-State district which has been ably covered by many geologists. The writer was co-author of several publications on the Tri-State district.- This paper is necessarily a repetition of parts of those publications but contains a few changes and additions on the deposition of the minerals. The parts of this paper concerning mineralization maps and pipe slump-structures are not covered in the above publications.

Jan 1, 1950

By AIME AIME

DESTRUCTION of the plants, machines, utilities, tools, materials, and other essentials for peacetime living penalizes not only the owners of the materials destroyed, but the world as a whole. Specifically, the fundamental fallacy of any proposal for the in- discriminate destruction of the German industrial system is that it fails to differentiate between the wartime and the peacetime economy of the Reich. We are for one simple, clear objective-an effective industrial means to keep Germany from starting another war. This objective should not be con- fused, especially before the war is even won, with the appropriate punishment of Germany or with the international arrangements for the long future to be made around the peace table by the representatives of the Allied Nations after victory is achieved. This paper, therefore, does not deal with broad, complex postwar questions of diplomacy and international policy. "Unconditional surrender" implies disarmament of the German armies, the surrender of all arms, munitions, air- planes, and other ordnance material in stock piles or in process. It also should include the elimination of all German war production facilities, such as ordnance plants, munitions plants, and submarine works, and the control of raw materials required by war industries.

Jan 1, 1944

By Arno C. Fieldner

METALLURGICAL coke and the by-products of the carbonization of coal continue in strong demand. Nearly 500 new by-product ovens were constructed in 1943. Output of by-product coke in the first ten months of the year was about 2 1/2 percent higher than in the corresponding period of 1942, but beehive production remained on approximately the same level as last year and constituted about 11 per cent of the total coke output.

Jan 1, 1944

By Stanley C. Herold

TWENTY-FIVE years ago no distinction was made between water wells and oil wells except in the nature of the fluid produced. Water wells usually showed no decline in their rate of production; when oil wells showed decline something in the manner of handling them was considered wrong. Both water and oil were believed to be subject to the same physical laws in their underground movement toward the wells. Today a sharp distinction is made between them. Whereas water exists alone in the porous formations at depth, oil is usually accompanied by gas. This mixture does not behave as a liquid alone. It is a frothy, seething mass of foam which approaches and enters the wells. Different physical laws come into play. Twenty-five years ago attention was directed entirely to the well itself; today the well is accepted as a mere hole in the ground, a hole to be equipped properly for efficient service, yet without any value whatever unless it is backed up by a sufficiently prolific reservoir. Then, we were concerned with wells alone, 3000 ft. in depth; now commercial wells and their reservoirs are 10.000 ft. deep. Petroleum engineering concepts have necessarily therefore undergone a change in this last quarter century. What are they today?

Jan 1, 1937

By H. R. Barnhurst

It would be a difficult matter to trace from the beginning the very few improvements made in the burning of fuels prior to 1860. Donbtless the crossing of the sticks of wood in building a mood fire early appealed to our savage ancestry as a means of expediting its effectiveness for their crude culinary purposes. Stones and andirons came later in assisting the admission of air to the under part of the fuel bed, while beacons and cressets, utilized metal bars as supports for the same purpose. It is probable that Tuba1 Cain owed his success to the use of bellows making possible the use of mixed fuel and charge upon a hearth. With the development of working in cast iron, grate bars came in, and they are still with us doing duty in every household and almost every art where heat is a factor. Little was done beyond these crude methods prior to 1860. With the advancement of knowledge came the fuel-gas producer, a natural child of the retorts employed in supplying illuminating gas. It is only within the last 15 years that the conclusion became general that complicated systems for saving heat would not remedy deli-. ciencies in its primary development, and within that time there has been great advancement in the means of producing initially a fire of high effciency, so that to-day we are moving rapidly toward both high development and high absorption, with the resultant of high efficiencies. In studying the subject of the availability of pulverized coal as a fuel, it may occur to ask, why has this not come up earlier? This, question would be naturally prompted by recalling the fact that Thomas Crompton's English patents upon his methods were issued to him nearly 40 years ago. A conclusive answer to this, however, is that Crompton at that time had very crude facilities for making what was at best a very imperfect pulverization of the coal, arid the expense of preparation mas very great. He does not seem to have been aware of the advantage of a thorough drying of the coal in the

Jan 1, 1914

By Robert Linton

M ETHODS by which Americanization is developed among the foreign workers at the mines in the United States, with particular reference to mines of the Pennsylvania coal region, were discussed in a most constructive way at the Wilkes-Barre Meeting of the Institute. Arthur Notman, of the Phelps Dodge Corpn., as chairman, guided the discussion. Americanization was defined by E. E. Bach, !chairman of the Institute's Sub-committee on Americanization, who said: "Americanization applies either to the native-born or foreign-born and is that process of assimilation which guarantees the full functioning of American citizenship. Naturalization papers merely entitle one to the privileges of citizenship."

Jan 1, 1921

By Robert Kinzie

WHEN Mr. Cameron, the President of the Santa Cruz Portland Cement Co., returned from Europe in 1929, he brought first-hand infor-mation about a very versatile type of hydraulic cement. It was not a new cement, many articles having been written about it in foreign journals, but in this country the record of this type of cement had been either neglected or minimized. Using local materials, and applying the information brought back by Mr. Cameron together with many data in numerous publications, the Santa Cruz Portland Cement Co. developed the Santa Cruz high-silica cement. This cement is manufactured by grinding with portland cement clinker a properly calcined mixture of siliceous material and lime. It has all the utility of portland cement, together with an increased resistance to the destructive action of many aggressive solutions. To explain the necessity for the development of a cement having these characteristics, the history of hydraulic binding materials may be reviewed briefly. The materials used as binding media by primitive people were mud, lime, gypsum and bitumin. Due to its utility, ease of preparation, and its common occurrence, lime was the most widely used. Fat lime, when used by itself or with an inert sand, hardened only on the outside surface, where the carbonate was formed by absorption of carbon dioxide from the air, while, the interior of the mortar remained soft. It was quite early discovered that the incorporation of proper siliceous material with the lime increased its ability to harden, and for this purpose various natural siliceous powders were used, such as puzzo-lana in Italy, trass in what is now Germany, and santorin in Greece. These powders reacted with the lime forming a permanent cement and rendered unnecessary the access of carbon dioxide to the mortar.

Jan 1, 1934

By O. H. Banes

The electrolytic zinc plant of the American Zinc Company located at Sauget, Illinois started operations in April 1941. The plant had a designed capacity of 45(T) per day. The original flow sheet was quite simple, incorporating the low density process. Through the years the capacity of the plant has been increased to the current design of 214(T) cathodes per day. This paper describes the current operation along with typical metallurgical data.

Jan 1, 1970

By David J. Mack

A survey and critical appraisal of published information about Young's modulus was originally made by the writer because of a complete lack of information about this very important quantity in works on. mechanics, physical metallurgy, physics, and other sciences. It was felt that a comprehensive summary of such information about Young's modulus might be of general interest and may suggest new problems or lines of attack on other problems that involve E. Hence this paper has been prepared even though it is only a review, with no new ideas or experimental data. The references are only those used in assembling the paper. No attempt was made to compile a complete bibliography on the subject of Young's modulus. CalculatioX oP YouNg's Modulus from Theoretical or Empirical CoNsidera-tions Many attempts have been made to compute E from theoretical considerations. The earliest calculations were probably those of Tomlenson (1883) and Souther-land (1891), but Fess'enden4',~ made extensive calculations a few years later and arrived at the relationship: £ = 78.TOw(i)* where V is the atomic volume. In 1923, Peczalski, working from the same standpoint but with more information available on atomic structure, arrived at an identical relationship, which he expressed as: where B is a constant of value about 8 . 107, p is density and mis atomic weight; the atomic volume, of course, being ml p. Portevind4 immediately pointcd out that while the equations of Fessenden and Peczalski were true of the common metals, they gave low values for the refractory metals with high moduli (Fig. I). He showed (Fig. 2) that much better concordance was obtained by means of an empirical equation of the form: F- KT" where K is a constant; T the absolute melting point; V, atomic volume, and a and b constants of value approximately I and 2 respectively. This constant K in the Portevin equation is not necessarily the same for all elements, as shown by Thompson. Other equations for E based upon theoretical considerations have been derived by Honda and Yamada49 and Lasareff.50 The most recent calculations of elastic moduli based upon quantum mechanics are probably those of Fuchs He extended the method of Wigner and Seitz for calculating the lattice energy and compressibility of monovalent metals and computed the elastic constants of lithium, 18

Jan 1, 1946

By David R. Mitchell

THIS paper is limited primarily to a description of dry coal-cleaning processes in which air currents are used to effectuate a separation between coal and refuse. Processes depending mainly on differences in the coefficient of friction, resilience and shape are not described unless the use of air is necessary for the proper functioning of the process. The air cleaning of coal is of primary importance to the coal industry of the United States. From figures presented in the 1941 edition Mechannual,1 it is estimated that at least 12 million tons of bituminous coal was cleaned in the United States during 1940 by machines using air as the separating medium. One of the current problems confronting the coal-preparation engineer is the dry cleaning of small sizes and slacks. Progress in machine development for the cleaning of small sizes has been slow in recent years in the United States of America; it has been much more rapid in Britain and on the European continent. This paper does not attempt an exhaustive survey of all these developments, and only machines and processes that have found considerable commercial application are cited. Further, no critical analysis has been made of the theory involved in the separation of coal from refuse by processes using air as the separating medium other than that necessary for an understanding of particular machine designs and applications. HISTORICAL SUMMARY The possibility of using air for the separation of coal from refuse was recognized early by mining men and many attempts were made to develop commercial machines. The ingenuity of the early experimenters is to be marveled at in view of their lack of knowledge of the theoretical principles involved. As in other arts, practice has largely preceded theory. Yet, science and practice play a game of leap frog, now one ahead, then the other; the careful experimenter governs his efforts along practical lines by adapting his experiments to the limits prescribed by scientific laws. By first studying developments and the theory involved, it is not only possible to adapt processes to new uses but also to reduce materially operating cost and to build larger units without costly failures. Although many inventors have applied for patents for separating minerals by the use of air currents, the literature in regard to coal is meager. Berrisford2 describes briefly some of the early attempts to clean coal without the use of water. Several of the examples cited by him are reproduced herein. Fig. I shows a machine used for grinding and sizing, in which rollers running in a pan with a perforated bottom and fan opening on the side crushed the coal, which was then carried by the air currents to a settling chamber. The heaviest particles dropped out first and the light ones farthest away, as shown. In the year 1864, a machine was made that could be used as a sizer or to separate dirt from coal with a sized feed (Fig. 2).

Jan 1, 1942

By C. V. Millikan

New developments in air-gas lift practices in the Mid-Continent area since our Pall meeting in Fort Worth have done much to increase the efficiency of installations, and thus bring within economic limit of air-gas lift many wells which could not have been flowed profitably before. After the gas-lift had so thoroughly demonstrated its value in the Seminole field, its use spread to other areas and many installations were made of which the economy could be questioned. In the Seminole area, when production began to decline it was necessary either to increase the efficiency of the air or gas-lift or to put the wells on the pump, and pumping was not a process of lifting oil to which any operator looked forward with confidence. These conditions have resulted in the development of many practices which increase the efficiency and permit wells to be flowed with air or gas which earlier could not have been flowed economically, and wells which have been flowing to continue to a lower rate of production. The practices which have come into more common usage in the Mid-Continent area recently are mostly revivals of and improvements on practices which have been known in air-lift work for several years. Many arc peculiar to the individual well on which they are used. Intermittent Flowing Some interesting results are being obtained in Seminole and other districts by intermittent injection of gas. Gas is introduced during per-iods iods of 3 to 5 min. at a rate considerably over that necessary to acquire the production at a steady rate of injection, and is then cut off for a period of 3 to 15 min. Two to five wells are run from the same group of conlpressors. The total volume of gas required is sometimes reduced as much as one-third of that required when it is introduced at a constant rate, without changing the amount of oil production. The maximum pressure required is usually higher, but the average equal to or lower than that required for constant rate of flow. The effect on the wells is usually an irregular rate of flowing which may cause inconvenience where recycling is practiced. It would seem that this increase in efficiency is due to less slippage when the gas is introduced intermittently than when it is intro-

Jan 1, 1928

By G. K. Burgess

J. W. RICHARDS, South Bethlehem, Pa.-I think my affections are still rather with the radiation pyrometer than the optical pyrometer, for practical use, and I wish that Prof. Burgess would use the two together, under the same conditions, using the optical as his standard, if he prefers. Then, assuming the optical emissivity which he feels is correct for the optical pyrometer, he could calculate the thermal emissivity for use with .the radiation pyrometer. If we could thus get reliable values for the thermal emissivity, we could then use the radiation pyrometer, and would avoid the use of the standard lamp, which has to be frequently calibrated for use in the optical pyrometer. It is very advisable to distinguish carefully between the terms optical emissivity and thermal emissivity. There -is considerable confusion caused by the bare statement that molten iron has an emissivity of so much, meaning by that its optical emissivity, for a light wave of a certain length; whereas what we want in the radiation pyrometer is its total ther-

Jan 4, 1917

By Howard Willey

MINING operations of the Charcas unit at present are limited to the Tiro General mine at Charcas, in the State of San Luis Potosi, Mexico. The Tiro General mine was first operated during the Spanish occupation of Mexico for rich silver ores in an oxidized zone along the outcrop of the principal vein. In depth the ore is a complex sulfide with widely varying proportions of sphalerite, argentiferous galena and chalcopyrite; and until recent years, it was economically impossible to carry on mining otherwise than irregularly in sections of the veins richest in galena and chalcopyrite. The advent of selective flotation brought the orebody as a whole within the field of economic interest, and a flotation mill of 650 metric tons daily capacity was constructed in the year 1925. The mining of partly worked-out sections of the mine, as well as the very heavy ground in most of the stopes opened in virgin ore, presented an unusually difficult problem. This -paper describes the so-called "filled top slice" stoping method finally adopted as the standard system.

Jan 1, 1930

By G. V. Jere, V. Krishnan, C. C. Patel

Standard free energy and standard enthalpy changes as a function of temperature have been calculated for the chlorination reactions of different oxides constituting columbite and tantalite. The tallies of standard lee-energy change (F) indicate the possibility of pvefeential chlorination of different oxides but the ease 0.f chlorination of columbium pentoxide at about 250°C and the chlorinating tendency of columbium pentachloride in promoting the chlorination of tantalum and other metal oxides, p7-evetzt the separation of columbiu?n and tantalum from other oxides and pom each othel.. It is likely that low temperatuves of chlorination and continuous 1err2oval of columbium pentachloride from the ..eaction zone may help partial separation of columbium from tantalum as well as from titanium. The standavd enthaply change (AH?) values shotr that 1ou.-temperature chlorination around 300" to 500°C is likely to sustain the chlorination , without external heating. COLUMBIUM (niobium) and tantalum metals, their alloys and interstitial compounds are finding extensive uses in nuclear reactors and high-temperature equipment.la-3 These metals also find uses in chemical process plants, electrical rectifiers and capacitors and as "getters" in electronic tubes.la With the development of Kroll process of reduction of volatilized titanium tetrachloride by magnesium for the production of titanium metal, chlorine metallurgy is receiving greater attention. Chlorine metallurgy has several advantages, the foremost amongst them are: the ease of chloride formation, separation of the different constituents of minerals by selective chlorination, and the reduction of the chlorides in vapor phase to the respective metals. Recently, Si-bert, Kolk, and Steinberg4 have considered a number of methods for the preparation of columbium metal and the most promising is found to be the halide reduction. Since the minerals columbite and tantalite are comparatively abundant in nature, the future of the metallurgical processes depends on the utilization of these minerals for the production of columbium and tantalum chlorides by chlorination. In this paper, an attempt has been made to interpret thermodynamically the chlorination of individual oxides constituting columbite and tantalite, with the help of the recent thermodynamic data.5-8 For this purpose, standard free energy and standard enthalpy changes of the chlorination reactions of the oxides with chlorine, both in absence and presence of carbon as the reductant, have been calculated as a function of temperature and represented graphically. Similar calculations for the reactions employing carbon tetrachloride and carbonyl chloride as chlorinating agents have also been incorporated in this paper. REPORTED WORK ON CHLORINATION Cuvelliezg has patented a process for the separation of columbium and tantalum from their concentrate, wherein 75 pct Cb05 is claimed to be chlorinated at 1050°C in the course of 7 hr using chlorine or chlorine containing nonreducing gases, the products of reaction being CbC1, or CbOC1,. At this temperature, Ta,05 is claimed to remain unaffected. It is further claimed1° that at higher temperatures, the proportion of Ta205 chlorinated increases while that of Cb205 diminishes. During the studies on the action of chlorine on individual metal oxides, Kangro and Jahn" have observed that Ta,05 is not chlorinated even at 1200" in the stream of chlorine, while 75 pct of Cb,05 is converted into CbOC1, around 900 to 1100°C. The chlorination of Cb205 by chlorine in the presence of carbon, investigated by Lind and Ingle,' and

Jan 1, 1962

By H. D. Outmans

The mechanics of filtration are described by a theoretical-empirical nonlinear diffusion equation which, under certain circumstances, may,be linearized and then solved explicitly. For filtration under static conditions linearization leads to a boundary value problem analogous to a heat flow problem with a known explicit solution. The corresponding solution for static filtration is compared with published experimental data. Under dynamic conditions filtration takes place in three successive stages. During each of these the rate of filtration and/or the thickness of the filter cake are different functions of the filtration time. The proposed mechanism explains the observed high resistance of dynamically deposited filter cakes against erosion and also the connection between filtration rate and viscosity of the drilling fluid. Several of the quantities governing dynamic filtration have no counterpart in the static filtration mechanism. The static filtration rate is, therefore, not a reliable measure for the dynamic rate and vice versa. INTRODUCTION Filtration under simulated borehole conditions, i.e.. either from a static suspension or from a suspension flowing parallel to the filter cake (dynamic filtration), has been the subject of several laboratory studies.1-7 This experimental and theoretical work showed that many aspects of the filtration mechanism cannot be explained by an elementary filtration theory based on the assumption that the filter cake is incompressible. For a more satisfactory theory compressibility should be taken into account. This has been done. at least to some extent, in the filtration theory developed for the chemical industry. Surveying the literature (see Ref. 8 for a bibliography) it becomes apparent that, although several properties of filter cakes deposited from many different suspensions have been measured, including compressibility, the filtration equations are essentially empirical in nature. No attempt has been made, for instance, to develop filtration theory along the lines of consolidation theory.12 This theory, upon which a highly successful development in soil mechanics rests, would appear to be an excellent starting point for a filtration theory since the compressibility concept is an essential part of it. As we will use this theory in the following development it is well to state the four assumptions on which it is based: 1. The fluid flow through a compressible porous medium is governed by Darcy's law. 2. The rate of change in fluid content of an element of the porous medium is proportional to the rate of change of solid pressure between the particles. 3. The solid particles are incompressible within the range of pressures considered. 4. The total pressure on a surface normal to the line of flow is equal to the sum of the fluid pressure and the pressure between the particles (solid pressure) at that surface. To calculate the rate of filtration and other quantities of interest it is necessary to know the filter cake compressibility and the permeability as a function of the solid pressure. It has not been possible to calculate these functions from theoretical considerations and they will therefore be introduced in this paper as empirical expressions. Both are determined in a compression cell where the cake is subjected to a mechanical load. Permeability and compressibility are measured after the solid pressure has stabilized, i.e., after the excess fluid pressure has been dissipated and the uniform pressure is transmitted entirely by the solids. The permeability and compressibility thus determined are not the same as during filtration in the borehole, under either static or dynamic conditions, because then, due to frictional drag, the solid pressure and hence also the permeability and compressibility vary along a line normal to the direction of the mean flow and can only be defined locally. DERIVATION OF THE FILTRATION EQUATION FOR COMPRESSIBLE FILTER CAKES As the filter cake in the borehole is thin compared to the radius of the hole the filtration may be considered as linear. Taking the x-axis normal to the wall, with its origin at the formation, we have, according to Darcy's law,

By Ian Wark

IT has been shown1 that in the absence of heavy metal salts, the nature of the alkali used to promote differential flotation-whether caustic soda, lime or sodium carbonate-is unimportant. The hydroxyl ion is the active depressant upon which differentiation depends, and the pH value determines whether a film of collector forms on any given mineral surface. Even when sodium cyanide is used in conjunction with alkalies, it is the pH value and not the nature of the alkali or its concentration that is important, for upon the pH value alone depends the fraction of the added sodium cyanide that is present as cyanide ion, which is the true depressant. When heavy metal salts become dissolved from partly oxidized ores, or are added intentionally as activators, conditions are different, and metallurgists have found that lime and sodium carbonate do not give identical results, even when added in amounts sufficient to produce the same pH value. In the few instances in which we had attempted to confirm this view, we had failed to do so, for, with nothing to guide us, we had inadvertently chosen solutions that gave contact curves of a "stand-ard type," which correspond to conditions of ready floatability. Now, however, we find that, in the presence of copper salts, and within a restricted range of reagent concentrations, the nature of the anions present is important, and that sodium carbonate does influence the results, apart from the usual effect due to its influence on pH value. With the recognition of this anion effect, and with the control of temperature already introduced,' it appears that the factors of major importance in connection with this set of reagents have been taken into consideration, and that the results obtained and the conclusions drawn from contact tests will be of more immediate value to the operator.

Jan 1, 1939

By Morris A. Steinberg

Because of the broad scope of my topic I will discuss my subject from the point of view of a present status of the metallic materials that are used in structures and will dwell primarily on those structures related to high- performance aerospace systems. Thus, I can best portray the status of these structural materials as related to existing transportation systems, delineating some of the highlights of alloy development, fabrication, and properties obtained. I shall point out what are, in my opinion, the needed solutions to pressing unsolved metallurgical problems connected with certain selected metals: aluminum alloys, beryllium, titanium, steels, superalloys, refractory metals and some metal-matrix composites. Aluminum Alloys For a number of years a series of strong aluminum alloys used for airframes has had an important bearing on the development of minimum- weight, highly efficient structures. Among these alloys are such familiar ones as 2024-T3, 2014-T6, 7075-T6, 7079-T6 and 7178-T6. A review of the development and use of strong aluminum alloys in aircraft structures indicates that before about 25 years ago there was very little application of products other than forgings in the high-strength tempers produced by precipitation heat treating to T6- or T8-type tempers. 1 As stated by Dix in 1944, "There has been a gradual evolution in engineering viewpoint regarding the mechanical characteristics which are required in a structural material suitable for aircraft. Formerly, emphasis was placed on a generous spread between yield and tensile strengths, on elongation, on impact strength and on resistance to corrosion. Aircraft structural engineers still differ widely as to the importance which they attach to these proper tie.” 2 It is fair to say that this evolution is still taking place, that the problem is much the same in 1970 as in 1944 - except that strength levels have advanced some - and the question remains as to how far we can go in that direction. In the meantime, a new group of alloys has received acceptance and widespread use. The first alloy of this group, 7075-T6, was formally introduced by Dix's 1944 paper. The drastic changes that have taken place in the size and configuration of components employed in air-

Jan 1, 1971

By Joseph C. Buchen

IN principle, production of salt from sea water is a simple operation. Sea water is trapped in ponds, the sun and wind cause evaporation of the water, and what is left is principally salt. Commercial production of solar salt, however, requires a careful consideration of many factors. Obviously, sufficient evaporation must take place throughout the making season to produce an economically adequate crop. Other factors are density of soil, contour of ground, height of ground above sea level, minimum dilution from fresh-water streams, and distance from market. Unfortunately, in the United States the localities of greatest evaporation, allowing for the other factors, are not the most suitable for the manufacture of sea salt by solar evaporation. The south end of San Francisco Bay most

Jan 1, 1937

By E. Miller, K. L. Komarek, M. Ettenberg

The activity of aluminum in solid Co-A1 alloys has been measured by an isopiestic technique between 850° and 1200°C from 45 to 80 at. pct Al. The activity shows a Precipitous decrease around the stoichzornetric composition of CoAl. Free energies of mixing have been calculated over a limited composition range. Considering an antistructure-vacancy defect mechanism, the degree of intrinsic disorder, a , in CoAl was related to the alunminum activity. Excellent agreement between the calculated and experimental activity curves was obtained for a = 1.25 x 10-4. ThERMODYNAMIC properties of solid aluminum-transition metal alloy are being studied in an investigation of disordering in ordered compounds. In a continuing series of investigations, activities of solid Fe-1,' Ni-A1, kd r-A13 alloys have been measured. From the results for Fe-A1 and Ni-A1, the degree of intrinsic disorder for the equiatomic compounds was calculated2 using equations derived by Wagner and chottk. From the results for Cr-A1 the degree of intrinsic disorder was calculated from equations derived by Orr.' In this paper, the results of the study of Co-A1 alloys are described. Published activity data in the Co-A1 system has been limited to liquid alloys at 1600°C.° A heat capacity study7 of stoichiometric CoAl indicated that a second-order phase transformation occurs at 790° C, attributed to an order-disorder reaction. Oelsen and Middel,' employing the calorimetric mixing of pure liquid metals, obtained heats of formation for compositions from 6 to 90 at. pct Co. Heats of formation for 50 and 78 at. pct Co alloys have also been measured by acid solution calrimetr. The Co-A1 phase diagram, as compiled by Hansen and Anderko,lo is in good agreement with more recent X-ray evidence. The method for measuring activities of aluminum in this study is essentially that employed in the studies of the Fe-1,' i-Al, and r-A13 systems. This isopiestic method entails placing cobalt specimens, in a temperature gradient, in a sealed alumina system containing a pure liquid aluminum source of fixed vapor pressure. The specimens are equilibrated, cooled to room temperature, and their final compositions determined. From the measured temperature of the specimens and the known vapor pressure of pure aluminum the activities of aluminum in the alloy can be calculated. EXPERIMENTAL PROCEDURE The cobalt was 3-mil-thick sheet of 99.9 pct purity (herritt Gordon Mines Ltd., anada). The major impurities were 0.1 pct Ni, 0.014 pct C, 0.018 pct Fe, 0.004 pct S, and 0.005 pct Cu. The aluminum metal had a purity of 99.99 pct (Aluminum Corp. of America) and all alumina parts were 99.7 pct A1,O3 (Triangle RR Grade, Morganite Refractories, Inc.) with major impurities 0.05 pct SiOz, 0.1 pct Fe203, 0.2 pct NazO, and 0.05 pCt K20. Runs 1 to 3 were made with annular cobalt specimens (12 mm ID by 21 mm OD) punched from the sheet. The specimens were deburred and degreased in carbon tetrachloride and in acetone. The samples, each weighing about 150 mg, were then positioned along an alumina rod, a in. OD by 14 in. long, separated by alumina spacers, i in. ID by | in. OD by & in. long. The lower end of the rod was placed in a hole drilled in the center of an 80-g aluminum cylinder. This assembly was put into an alumina crucible, 1+ in. ID by 13 in. OD by 3+ in. high, and the position of each sample was measured to within 50.5 mm relative to the bottom of the crucible. An alumina tube, 28.5 mm ID by 35.5 mm OD by 14 in. long, closed at the top, was slipped over the whole assembly, so that it fitted snugly into the bottom crucible. The entire reaction assembly was tied with molybdenum wire and lowered into a mullite tube, closed at the bottom. A quartz thermocouple tube, closed at one end, containing a t/Pt-10 pct Rh thermocouple, calibrated according to the specifications of the National Bureau of standards,'' was placed along the reaction assembly inside the mullite tube. The temperature of each specimen could be determined by gradually raising the thermocouple and measuring the temperature gradient along the reaction assembly. The combined error in temperature measurement and sample position resulted in a total error of Q°C in the recorded temperature of each sample. The mullite tube was sealed at the top by a water-cooled brass head, connected to a conventional glass vacuum system. The aluminum reservoir is heated to its melting point sealing the alumina system containing the samples. During this process the pressure is maintained below 0.01 li Hg. During subsequent heating to establish the proper temperature gradient and throughout the entire run the pressure is maintained below 2 1 Hg by means of a two-stage mechanical pump. Equilibration runs lasted from 4 to 6 weeks and were terminated by air cooling. The temperature of the liquid aluminum reservoir was brought below its melting point in less than 20 min. For runs 4 and 5, alloy buttons with 49 and 69 at. pct A1 were prepared from the initial high-purity metals by arc melting under purified argon. The alloy buttons were comminuted to powder with an alumina mortar and pestle until the powder passed through a 400-mesh screen, particle size 0.0014 in. Portions of this powder weighing between 50 and 200 mg were placed in small alumina trays, 25 by 15 by 5 mm, which were then

Jan 1, 1969

By R. J. Towner

Tensile properties of Aluminum Powder Metallurgy (APM) products at 600°, 800°, and 1000°F were lowered by cold reductions of as little as 10 or 20 pct. The detrimental effect of cold work on yield strength at elevated temperatures increased with temperature. Heating cold-worked products at 850° to 1150°F removed the structural effects of cold work through the process of recovery and restored, at least partially, the strength at 600°F to the level of hot-worked material. Material containing 5 pct A1203 was recrystallized by cold reductions of 97 pct or more followed by annealing at 1100°F. Recrystallization lowered sharply the strength at room temperature, but raised the strength at 600°and 800°F relative to that of the cold-worked state The high strength of Aluminum Powder Metallurgy (APM) products at elevated temperatures'-4 is well-known. In this paper, some conditions of processing that can affect this important characteristic are presented. The following nomenclature will be used to identify different alloys: All of the above alloys are of the aluminum-aluminum oxide type made from milled powders of commercially pure aluminum with the exception of M486, which is fabricated from atomized A1-Fe alloy powder. The products made from milled powders are hardened by a dispersion of aluminum oxide par- ticles in the aluminum matrix, while the intermetal-lic compound FeAL is the dispersion hardening agent in M 486.' The process used for making all APM products involves the application of heat and pressure to form a compact from powder which is fabricated into an extrusion, sheet, strip, or wire by standard techniques. Probably the most common cold-worked APM product is sheet. Cremens, Bryan, and rant' determined the room-temperature tensile properties and the 600°F stress-rupture properties of XAPOOl and XAPOO3 sheet and reported that there was little difference between the as-extruded, cold-worked, and annealed at 1200°F conditions. On the other hand, Emmons6" found that the tensile and stress-rupture properties of XAPOOl and XAPOO3 sheet at 600" and 800°F were lower than those of extrusions. The tensile properties of XAPOO3 sheet were also determined at elevated temperatures by Doyle' and ~ayward.' According to Friske" and Kendal et a1.," cold working by swaging, rolling, and tube drawing reduced the tensile and creep-rupture strength of XAP 001 Recrystallized aluminum powder metallurgy products are rare because the dispersion in the aluminum matrix is usually too fine, uniform, and concentrated to permit recrystallization. However, Lenel12 was able to recrystallize wires made from aluminum powders containing about 1.75 and 3.0 pct oxide and found that the tensile properties at room temperature remained higher than those of annealed commercially pure aluminum because of the dispersed oxide particles. Westerman and Lenel13 found the kinetics of recrystallization of the powder products were very different from those of cold-drawn commercially pure aluminum wire. The alloy containing 3.0 pct oxide recrystallized to a very coarse grain size was more creep-resistant at 400" to 600°C (752" to 1112°F) than in the as-extruded, fine-grained condition, according to Ansell and weertman.14 Ansell and aenel" further studied creep at 500" to 620°C (932" to 1148°F) of recrystallized 1.75 pct oxide wire and confirmed the creep model of Ansell and Weertman. The present work is being reported for the fulfillment of the following objectives: 1) to show the effect of cold work on tensile properties at elevated temperatures;

Jan 1, 1964