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By W. A. Backofen, G. Mayer

Single crystals of iron, copper, and a Cu-7 wt pct A1 alloy were pulled through conical dies to simulate the constraint in a polycrystalline aggregate undergoing axisymmetric reduction. With Taylor-type hardening, dependence of the drawing stress, od, on the Taylor orientation factor, M, is predictable from the polycrystal stress-strain curve; in particular, for a power-law relationship, it should follow that d log od/d log M = (1 + n). A first-order agreement with analysis was found in the data from iron. For copper, the implied n from the observed d log od/d l°g M was -0, while for Cu-7Al it was negative. The trend was in the direction of random polycrystal behavior. Thus the idea of hardening only in response to the amount of prior slip loses validity as stacking fault energy (SFE) is lowered. Two possible explanations have been suggested: as stacking fault ribbons are widened, barriers from dislocation reactions become increasingly effective in dispersing slip and reducing the orientation dependence of the total glide strain dm that appears in alternatively, or conjointly, the polyslip shear stress, 7, acquires an orientation dependence of a kind which has the same leveling effect on M. The problem of relating the strain hardening of polycrystalline material to that of an isolated single crystal is still largely unsolved. In a new experimental approach from recent work, single crystals of different orientations have been deformed under the constraints found in an aggregate while measuring their deformation resistance. Procedures have involved drawing cylindrical crystals through conical dies1 and compressing slab-shaped crystals in plane strain.2'3 Predictions for the outcome of such experiments were made first by Taylor~ and later, in more general form, by Bishop and Hill.5'6 Taylor's example was the axisymmetric extension of an fcc crystal slipping on the usual {111}(110) systems or, equivalently, a bcc crystal undergoing 'kestricted" slip on {110}(111). In his solution, the deformation work supplied was equated to that dissipated internally in slip on all active systems. With o the single applied tensile stress, dc the resulting axial strain, and dyT the total glide strain on systems operating at resolved shear stress, 7: The orientation dependence of M was found by minimizing dyT for each orientation while activating five independent systems, Fig. l(a).? The Bishop and Hill analysis, based on a principle of maximum work, leads to essentially the same conclusion; the need for at least five active systems is recognized in the finding that either six or eight are actually brought into operation. The mean value from the entire stereo-graphic triangle in either case is M - 3.06. More recently, Hutchinson8 made a Taylor-type analysis for pencil glide in a bcc structure, from which piehlerg prepared Fig. l(b) as the counterpart in Fig. l(a); here M = 2.75. The obvious weakness in such analyses is the indifference to slip-system interactions. A condition of what might be termed "independent"

Jan 1, 1969

By H. D. Merchant

NUMEROUS publications have examined hot hardness of metals and alloys. Some have studied creep in long-time hardness tests, few of which, however, were tested under a spherical indentor. 1-3 The results of Mulhearn and Tabor' indicate a parabolic-type creep for indium and lead, whereas Moore and Tabor2 how a logarithmic-type creep for indium. Similar semilog relationships between hardness and time have been found by Goffard and wheeler3 for magnesium, aluminum, and their alloys. In this note, the elevated-temperature hardness of some complex alloys, shown in Table I, was examined to discover whether any basic information about the deformation behavior of the alloys could be obtained. One of the alloys, H-13 alloy steel, was tested for short-time creep tests to examine the hardness-time relationship at various temperatures. A standard Brinell Hardness Tester, mounted with an appropriate furnace and 99 pct A12O3 poly-crystalline indentor, was employed for the purpose. The alloys were tested at temperatures from room to 1400°F for 30 sec under 1500-kg load. The creep studies were conducted for about 8500 sec at 7l°, 500°, 1000°, and 1200°F. For constants A and B, a relationship of the type H = Aexp(-BT) [ll was obtained for all alloys between hardness, H, and temperature, T. In the semilogarithmic plot, the data points for each alloy were arranged into two groups, each group on a straight line with a specific set of A and B values. These results are in agreement with many such observations on hot hardness, notably those of Westbrook for pure metals,4 The thermal softening coefficient, B, and transition temperature, Tt, for various alloys are shown in Table I. The change in slope around the transition temperature suggests an apparent change in the mechanism of deformation, probably from the shear (below Tt) to the diffusion type of mechanism. At the temperatures above Tt, for constants A' and B, a relationship of the type was obtained between H and T, Fig. 1. The nature of the equation, where R is gas constant, suggests the possibility of a thermally activated mechanism of deformation above Tt. The constant B' may hence be defined as the apparent activation energy of indentation. The B' values of various alloys are shown in Table I. A plot of B vs B' gives a curvilinear relation shown in Fig. 2. The indentation-creep data for H-13 alloy steel is shown in Fig. 3. At 71" and 500°F, the creep initially follows the logarithmic time law. However, the indentation size stabilizes after 7 sec at 71°F, and after 10 sec at 500°F. Further increase in loading time has no effect on indentation size. The creep of 1000° and 1200°F follows the logarithmic time law for the first 1000 sec, after which the

Jan 1, 1964

By J. B. Clemmer, F. D. DeVaney, H. A. Doerner

PRODUCTION of magnesium metal in the United States during the past decade has increased from less than 6oo,ooo lb. in 1928 to more than 4,800,000 lb. in 1938.1 The growing industry has stimulated interest in methods of production and in sources of raw material. All of the present domestic production is from brines. However, the availability of large tonnages of magnesite in the state of Washington, together with the possibility of cheap power, have created interest in the utilization of magnesite for the production of magnesium metal as well as for other purposes. Magnesite, the carbonate of magnesium (MgCO3), usually is associated with limestone (CaCO3) and dolomite (MgCO3CaCO3). It occurs in crystalline and microcrystalline (sometimes termed amorphous) forms.2 The more common crystalline mineral is found in various shades of white, gray, yellow and brown, the colors being due to impurities, chiefly iron. Magnesite has a hardness of 3.5 to 4.5 and a specific gravity of 3.0 to 3.1. It forms rhombohedral crystals in the hexagonal system, having a vitreous, pearly luster. The quarries and mines of the Northwest Magnesite Co. near Chewelah, Wash., are large producers of magnesite for refractories. The deposits are extensive, some veins being hundreds of feet wide. The boundaries of the veins are indefinite, and the magnesite is interfingered with dolomite. Calcite, talc, serpentine, quartz and shale are disseminated through the deposits. The quality of the ore cannot be determined by appearance or by simple tests; chemical analysis is required. These features make it difficult to determine the boundaries or total quantity of workable ore.3 Only the higher-grade ores are mined, and a considerable proportion of the magnesite content is discarded by hand-sorting and log-washing methods. After calcining, the sorted product meets the specifications for usual refractory material, as it contains approximately 81 per cent MgO, 7 per cent Si02, 6 per cent CaO and 6 per cent Fe203 + A1203. A sample of the reject material had the following analysis after calcining: 65.4 per cent MgO, 6.3 CaO, 21.1 Si02 and 6.5 R203. The percentage reported as R203 includes compounds whose chlorides are acid-soluble but give precipitates in ammoniacal solution that are ignited and weighed. The more common constituents are Fe203, A1203 and Ti02. The sorted magnesite product is not the best grade, even for refractory purposes, and leaves much to be desired for a reduction process. The rejected material contains a large proportion of magnesite. It is apparent that an effective concentration method would yield a higher recovery and a better product. In general, the refractory grade is not suitably pure for other uses. Recent developments in the production of

Jan 1, 1940

By J. Quigley

As the outcrop mines in the West developed into underground operations, systems of ground support were gradually evolved. In the early coal mines there was little need for support except near the dirt line in portals, where stone masonry was common. Where the top was shaley or broken, native pine props with light cross bars and legs furnished enough support even in Utah's 25-ft coal seams. As depth of workings increased. roofs and backs of the same general nature as those near the surface became more and more unstable and required more and more support. Some coal airways show this tendency very clearly. From the surface down the same type of roof shows deterioration which an experienced eye can translate into a measure of depth under surface rather than change in rock characteristics. Rock bolts, developed by various companies and by the U. S. Bureau of Mines, have become an effective substitute for timber in sections of some metal and nonmetal mines formerly requiring escessive timber support, and further use of war surplus landing mats, chain link fencing, and a new punched channel developed by one of the steel companies has enabled other mines to operate deposits where costs of timber and lack of clearance for timber support would have prohibited mining. The block caving mines have made extensive use of reinforced concrete underground to achieve similar ends under difficult conditions. Steel sets are standard in many Bureau of Reclamation projects, although these are usually covered in with concrete to make the permanent structures the Bureau's reclamation projects require. But the use of steel in mining operations is limited and has been confined principally to the iron ore mines of Michigan, Wisconsin, and Minnesota. Some mines have installed used rail as posts, caps, and crossbars, but a rail section is not suited for load carrying, and used rails are generally brittle. having a tendency to fail without warning when overloaded. European mines were the first to reach the size of worked out areas and depths of cover resulting in major roof problems. The Europeans resorted to pack walls and masonry walls, in conjunction with timber arched sets. rail arches, and combination timber and rail and steel arches. The give in these pack walls and wooden blocking was supplemented by a hinge in the center of the arch. This design is called an articulated arch Through various refinements of this principle of the support giving graduallv with the load. Toussaint-Heintzmann developed the yielding or sliding arches, in which yield is accomplished by friction in the overlapping joints of the arch. This type has gained widespread acceptance in the Ruhr and Lorraine Basin and is being manufactured by Bethlehem Steel for sale in this country. In North America the anthracite mines in Pennsylvania, followed by certain iron ore mines in upper Michigan and Canada, were the first to employ these arches to any extent. The practice was later adopted by Kennecott at Ruth, Nev., and by others. Despite high initial cost, the use of these arches is growing in many parts of the country because of their suitability in heavy ground. In its present form of manufacture the yield-able arch consists of open U-shaped rolled section with heavy beads on the edge. The open edge of the U is placed toward the wall. The section nests in another section of the same dimensions, and an arch can be built up from rolled radii and tangents of various weights and lengths. Sections are fastened together by U bolts and saddles. The lap on the joint varies from 12 to 24 in., and ordinarily the bolts are tightened with a 1-in. drive air wrench. The arches are spaced with channel struts held by J bolts and saddles. Sections can also be obtained that are composed of various combinations of radii and tangents and true circles. The joints can be placed to bear against anticipated loads and asymmetrical loads imposed by dipping strata. In the arches now being manufactured clearance widths up to 19 ft are obtainable in weights of sections from 9 to 30 lb per ft. The circular cross sections are available in the same weights ranging from 8 to 16 ft diam. At present most of the arches sold are supplied only in carload lots. It is hoped that demand will grow so that distributors can stock various weights and sections to give small operators a chance to try this new type of rock support under their own particular conditions. Several excellent papers have discussed the properties of various sections now manufactured, the dimensions of the sets obtainable, and their application under widely differing conditions. The present article will describe the methods and results of a special use of the arches at Kaiser Steel mine No. 3. Sunnyside, Utah. Problem at Mine No. 3 : In 1953 Kaiser Steel Corp. laid out Sunnyside mine No. 3 to recover coking coal left by the previous operator, Utah Fuel Co.. below workings that had been abandoned in 1928. Two seams had been worked, the upper and lower, separated by 30 to 42 ft of rock. Approximately 10 million tons of coal had been extracted from this area some 3000 ft down the itch from the outcrop to a 1500-ft depth of cover. The mine had been opened by slopes in both upper and lower seams. Sometime in the late 1920's the lower slope

Jan 1, 1960

By F. M. d’Heurle

Films of molybdenum have been prepared by sputtering onto oxidized silicon substrates. The resistivity. lattice parameter, orientation, and grain size were studied as a function of substrate temperature and substrate bias. Under normal sputtering conditions, the resistivity of the films was found to be quite high (600 x 10 ohm-crn). However, with the use of the negative substrate bias of 100 v and a substrate temperature of 350°C, films weve produced with a resistivity of ahout twice that of bulk molybdenum. The lattice parameters measured in a direction nornzal to the surface of the films weve found to be gveatev than the bulk value. This was interpreted as being at least partly due to the presence of compressive stresses. The effects of annealing in an Ar-H atmosphere were studied in terms of diffraction line width, lattice parameter, and resistivity. BECAUSE of its relatively low bulk resistivity (5.6 x 106 ohm-cm)' molybdenum is potentially interesting as a thin-film conductor in integrated circuits. An additional feature which makes it attractive for this purpose is its low coefficient of expansion (5.6 x KT6 per "c),' which is fairly well matched to that of silicon (3.2 x 10 per c). It is possible to deposit molybdenum films by evaporation but generally films produced in this manner have a high resistivity. In order to achieve resistivities close to bulk value, Holmwood and Glang found it necessary to operate in a vacuum of about 107 Torr and to maintain the substrates at 600 C during film deposition. Sputtered molybdenum films have been examined by Belser et a1.7 and, recently, by Glang et al.' This paper describes the results of an attempt to extend some of that work and examine the effects of annealing and getter sputtering on the physical and structural properties of the films produced. SPUTTERING APPARATUS AND PROCEDURE The apparatus used for most of the film sputtering work described here consisted of two "fingers" serving as anode and cathode, respectively, which were mounted within an 18-in.-diam glass chamber. A liquid nitrogen-trapped 6-in. diffusion-pump system was used to achieve a vacuum of about 1 x 107 Torr within the chamber prior to sputtering. The essential features of the equipment are shown in Fig. 1. Cathode and anode fingers are stainless-steel tubes isolated from the top and bottom plates by Teflon collars. In order to limit the discharge to the space between anode and cathode, each finger is surrounded by an aluminum hield, at ground potential, having an internal diameter 18 in. larger than the outside diameter of the finger. The cathode and anode fingers are 6 and 4 in. in diam, respectively. A 116-in.-thick sheet of molybdenum is brazed with a 10 pct Pd, 58 pct Ag, 32 pct Cu alloy to a copper disc which is mounted by means of screws and a large 0 ring onto the lower end of the cathode finger. The disc is cooled during sputtering by water circulation inside the finger. The use of several feet of plastic tubing for the water input and outputg reduces leakage to ground to less than 1 ma when the cathode potential is raised to 5 kv. The upper end of the anode finger is terminated by a brazed-on copper block. A variety of specimen holders can be easily mounted on the upper face of this block. Substrate heating or cooling is achieved by use of an appropriate unit attached to the lower face of the same block. Heating is achieved by means of cartridge-type heaters and cooling by copper coils fed with forming gas under pressure. The inner chamber of the specimen finger constitutes a small vacuum chamber of its own which is evacuated by an auxiliary mechanical pump in order to limit heating element oxidation and heat transfer by convection currents. An advantage of the finger arrangement is the absence of cooling and heating coils and wires within the main chamber. The stain less-steel shutter is useful to establish a discharge for cleaning the cathode at the beginning of each sputtering run. Water cooling of the shutter reduces heating and the out-gassing of impurities which might condense on the nearby substrates. Unless otherwise specified, the substrates used in these experiments were 1-in.-diam oxidized silicon wafe:s, 0.007 in. thick, having an oxide thickness of 6000A. The substrate holders were large copper discs onto the surface of which a number of molybdenum discs, 116 in. thick and 78 in. in diam, were brazed. The wafers were clamped to the molybdenum discs

Jan 1, 1967

By G. H. Turner, R. C. Bell, E. Peters

Zinc oxide activities in a typical lead blast furnace slag have been calculated from plant operating data. These activities were used to assess the probable effect of fuel composition, oxygen enrichment, and air preheating on the efficiency and capacity of the slag-fuming operation. THE physical chemistry of zinc fuming has been examined with three objectives in mind: 1—to predict conditions favorable to increasing furnace capacity, 2—to predict the changes required to fume zinc more economically, and 3—to explain reported differences in the efficiencies of various slag-fuming plants. This study, made at ail in the plants and laboratories of The Consolidated Mining and Smelting Co. of Canada Ltd., developed from a program undertaken some three years ago on behalf of the AIME Extractive Metallurgy Div. subcommittee on slag fuming. Lead metallurgists first became interested in the recovery of zinc from lead blast furnace slags in 1905 and 1906. An excellent review of the early experimental work has been made by Courtney,' who described blast furnace, reverberatory furnace, and converter methods of fuming zinc from slag. Some of the investigators did not appreciate the importance of reducing the zinc oxide content of the slag to metal in order to fume it, since they tried compressed air blast without fuel in their earliest attempts. However, by 1908, the importance of reducing the zinc was established.' In 1925, the Waelz process for the recovery of zinc oxide from oxidized zinc ores was developed in Germany.' This process was not readily adaptable to lead blast furnace slags because of the difficulty in handling fusible charges in a kiln. What appears to have been the first slag-fuming operation as it is known was commenced by the Anaconda Copper Mining Co. at East Helena, Mont. in 1927." The first Trail furnace was completed in 1930, and this was followed by the construction of several other slag-fuming plants. During the period in which slag fuming has been extensively employed, little development of the chemistry of this process as a whole has taken place. Several good papers on the petrography of lead blast furnace slags have been published,""= but these studies could do little more than establish the forms in which lead and zinc occur in the initial charge and final products of the slag-fuming operation. In recent years, zinc-smelting problems have been ap- proached from a thermodynamic point of view. Maier has published an excellent thermodynamic treatment of zinc smelting." The important thermodynamic properties of zinc and its compounds have been determined and checked by other investigators.' However, to the best of the authors' knowledge, no thermodynamic treatment of the fuming of zinc from slag has been published. A thermodynamic study of any process requires that the essential chemistry of that process be known. In slag fuming there appear to be some differences of opinion as to whether the active reducing agent is elemental carbon or carbon monoxide. Furthermore, some observers have noted that high volatile coals appear to be more efficient than low volatile coals, indicating that hydrogen is also an important factor in the reducing efficiency of a fuel. That both hydrogen and carbon monoxide are effective reducing agents for the zinc oxide content of lead blast furnace slags can be demonstrated readily by introducing these gases into a slag bath held in a neutral vessel at 2100°F (1150°C). Elemental carbon also will reduce zinc oxide, but it is improbable that much free carbon is available for reduction of zinc, as the reaction between the finely powdered coal and air should be largely completed before the solid coal particles reach the slag. Some large-scale fuming experiments using gaseous hydrocarbons have been carried out by other investigators, but, as far as is known, these have not been developed yet into operating processes. The thermodynamic treatment in this paper is based on the following reactions: 1—to supply the thermal requirements C+V2O2- CO [1] C + 0,-CO, [2] H2+ ~z0,-H,O 131 and 2—to reduce ZnO ZnO + CO + Zn + CO, c41 ZnO + H, e Zn + H,O. [51 The furnace-gas composition also is controlled by the equilibrium constant of the familiar water-gas reaction H,O + CO + CO, + H2. C6l In order for the thermodynamic calculations to be quantitatively applicable, it is necessary that the chemical reactions to which they are being applied

Jan 1, 1956

I have the honor to submit herewith the report of the Secretary for the year 1915 showing the principal activities of the Institute: Meetings.-The 110th Meeting, including the Annual Business Meeting, was held in New York City, Feb. 15 to 17, 1915. The full report of this meeting is given in Volume LI of the Transactions. The number of papers presented was 53, and the attendance was 357 members and guests. The 111th Meeting was held in San Francisco, Cal., Sept. 16 to 19, 1915. Sixty-eight technical papers were presented, and the attendance was over 400 members and guests. The full report of this meeting is given in the Bulletin for December, 1915. Local Section.-A new, strong Local Section of the Institute, with head-quarters in Arizona and known as the Arizona Section, was formed during 1915. Affiliated Student Societies.-Three new Affiliated ,Student Societies were recognized in 1915 consisting of the Pick and. Hammer Club of the University of Oklahoma, Mining and Metallurgical Club of the Univer-

Jan 2, 1916

* Kennecott Copper Corp. gets Charles R. Cox as president on Jan. 1. Mr. Cox is resigning his position as president of Carnegie-Illinois to take the new post with Kennecott, left vacant by the death of Mr. Stannard in September. •The ECA signed a contract in December to advance X3,600,000 to Newmont Mining Corp. to aid development of lead and zinc mines in French Morocco. The funds are to be repaid in lead and zinc for the United States' stockpile over a period of seven years. The mines are owned by the Societe des Mines de Zellidja, with which organization Newmont is associated. • Under the direction of John M. Brooks, Jr., general manager, the Matahambra mine in Cuba, will probably produce sufficient tonnage to make 4 million lb of copper per month during 1950. The grade is presently running between 7 and 10 pet. •S. H. Ash reports that the fatality rate per million-man-hr for the anthracite industry for 1949, through November, is 0.78. This is 15 pct better than that achieved during 1948, which was the lowest fatal injury rate in coal mining history. The first full year on record without a major disaster was recorded in 1949 (p. 34). •The Atomic Energy Commission has authorized the production of 200 lb of uranium metal for use under AEC license in non-Commission research projects. •A national survey of projected 1950 purchases of new machine tools, machine tool accessories, materials handling equipment, etc., just completed by the American Society of Tool Engineers reveals that, of the companies reporting, 80 pct state that they plan to buy either more equipment or the same amount as in 1948. • Armour Research Foundation is conducting investigations for the use of clay and shale deposits to make lightweight aggregates. The material is heated until it expands and forms material suitable for mixing with cement which it is hoped will be lighter, stronger, have better insulating qualities and will lower the cost of concrete. •In the first six months of 1949 the bituminous coal miners' average hourly earnings were $1.94 -as compared with X1.392_ national average for all manufacturing. Average annual earnings of full-time employees in the bituminous coal mines in 1948 were $3387 as compared with $2809 for all industry. •LaSalle Business Bulletin reports: "year ends on a rising trend in industry and trade ... nearly record-breaking demand from almost all sources keeps business high... most indicators but little below postwar peak... forces keeping activity high arestill powerful--changes in general business conditions likely to be slow and moderate." •Office of Internal Trade of the Commerce Department requests that technical data significant to the national security which is to be sent outside of the United States be submitted to it for an official opinion on the desirability of transmitting such information. This voluntary compliance program is part of our national security control. • Blast furnace slag reduced to 12 to 16 mesh is being used for sanding track at the Mont Coal mines of Armco. The slag replaces silica sand which caused silicosis. It has proved so effective and cheap that tests are being made to use the slag for rock dusting.

Jan 1, 1950

Not many accounts of mining methods or labor conditions in the mines in early days can be found; all that have seemed to be authentic have been included in the preceding chapters. In practically every field opened before 18.10 the first coal was recovered by quarrying, or strip mining, the operations, of course, being by hand and on a very small scale; new places were opened as soon as mining became difficult or expensive. Where it became necessary to drift into the hillsides, the first coal was taken out by sleds, and later by small wagons, the power being supplied by the miner, often assisted by dogs. Wooden rails then came into use with small cars running on them. These cars were very small, usually holding only a few bushels; in the Belleville, Illinois field as late as 1863 cars having capacities of 10, 12, 14 and some as large as 30 bushels were in use. It was not until late in the 1830's that horses or mules came into use for haulage purposes in the Pittsburgh region, although some had been used in the Richmond, Virginia field at an earlier date. Coal was usually undercut by hand and wedged down, until explosives came into general use, and in nearly every field the coal was forked into the cars, the fine coal, or slack, being left in the mine. Hours worked were very long, but few records remain to show what they were at different places and times; there was undoubtedly a great variation between districts and mines. Roy stated a miner could often produce 5 or 6 tons in a day of 8 or 9 hours in a 5 or 6 foot seam, but in another seam possibly could mine only 3 1/2 to 4 tons. He estimated an average day's work in a four foot seam at about 3 1/2 tons.1 In a strike in the Belleville field in 1863 it was found that an average skilled miner in the field could probably produce 4 to 5 tons a day.2 This was only the coarse coal loaded and did not include slack. In 1873, a coal undercutting machine was tried at a mine about two miles from Brazil, Indiana, said to be the first coal machine ever invented in the United States. It was run by a 5 H.P. steam engine (later to be changed to compressed air), and consisted of an iron rim, four feet in diameter with movable steel teeth placed about one foot apart. The rim

Jan 1, 1942

By L. Leibowitz, M. G. Chasanov, L. W. Mishler

A drop calorimeter system is described for use in measuring enthalpies to 3600°K. Data are presented for tungsten between 2800" and 3600°K. The enthalpy of tungsten in cal per mole between 2000° and 3600°K can be represented by the equation HºT- Hº298 = - 1.7622 X 103 + 5.7772T + 8.9861 where T is in degrees Kelvin. A tabulation of com -puted values is presented for heat capacity, entropy, and free energy function. A drop calorimeter has been constructed to carry out enthalpy measurements at temperatures to 3600°K. Samples are heated by induction1 and dropped into a commercial adiabatic calorimeter, modified for this purpose. The experimental temperature is limited by the melting point of container materials and compatibility of the container and its contents. Several high-temperature drop calorimeters have been described in the literature1-5 but none has been used at temperatures as high as those in the present work; our measurements of the enthalpy of tungsten range from 2800" to 3600°K. DESCRIPTION OF EQUIPMENT An overall schematic view of the equipment is shown in Fig. 1. Power for the induction coil is supplied by a 25-kw 250 kHz Ther-Monic generator coupled to an iron core RF transformer. The Sample capsule is suspended in the work coil by 10-mil diam tungsten wires which are wrapped around a horizontal 5-mil diam tungsten wire. The horizontal suspension wire is clamped between two massive copper electrodes which are fixed in an x-y motion device that allows adjustment of the position of the heated capsule from outside the vacuum chamber. The copper electrodes are connected by flexible copper straps to a 1250-joule (5 kv, 100 pfarad) condenser bank. When it is desired to release the capsule, the condensers are discharged through the horizontal suspension wire causing it to vaporize rapidly. Very reliable and precise release of the capsule is achieved in this manner. Experiments have shown that no heat correction is required for this discharge energy. As part of the temperature measuring system, two prism holders have been incorporated in the apparatus. The upper prism holder is in the main vacuum chamber itself, whereas the lower one is in a side arm attached to the drop tube below the gate valve. The upper prism is mounted on a rotary vacuum feed-through, and may be moved under a protective shield when not in use. This prevents deposition of vapors on the prism surfaces when temperature measurements are not being made. Similarly, the lower prism is mounted on a push-pull vacuum feed-through, and when not in use may be pulled into its side tube. The prism mountings are fitted with guides and stops so that they may be moved precisely into the desired position. The aim throughout is to minimize the time the prisms are exposed to vapors from the hot samples. At the high temperatures reported in this paper, only the lower prism was used. The upper prism holder in these cases was fitted with an additional radiation shield. By using a prism and viewport, the lower surface of the samples can be observed by an optical pyrometer. The measurements discussed in this paper were obtained with a Leeds and Northrup 8622-C-S series manual pyrometer which is estimated to be accurate to 0.5 pct. Pyrometer calibrations and prism and window corrections were carried out in the conventional manner6 using tungsten strip lamps calibrated by the National Physical Laboratory, Teddington, England. Prism corrections were rechecked after each use. All work to date has been done in vacuum, and no measurable change has been observed in the prism correction below -2300°K for the upper prism and below -2800°K for the lower one. The total time of exposure of the prisms is about 50 sec per run. At high temperature, the final temperature reading is corrected by using the final A value for the prism; see Ref. 6 for details of this procedure. The calorimeter is a modified Parr Instrument Co. (Moline, lll.), Series 1230 adiabatic calorimeter with automatic jacket control. Other authors5 have used a similar calorimeter with good results. The calorimeter jacket cover and calorimeter cover are attached to the drop tube which contains a radiation shield. This shield is a gold-plated copper disc which can be operated manually from outside the calorimeter. The receiver is attached below the radiation shield and is lined with tungsten. In a typical experiment, the calorimeter and its jacket water temperatures were adjusted to 0.000°K temperature difference. The sample was allowed to equilibrate in the furnace at the desired temperature for about 20 min. The initial calorimeter temperature was then recorded, the sample dropped, and appropriate shutters closed. After about 3 min, the drop tube and receiver were filled with helium to 60 torr. The final calorimeter temperature was recorded after it had remained constant over a 5-min period. The equilibration time in the calorimeter was about 25 min. Thermistor probes are used to operate a hot and cold water supply system to maintain the jacket temperature equal to the calorimeter temperature. For actual measurements of the calorimeter temperatures, a quartz thermometer was used (Hewlett Packard Dymec Thermometer, Model #2801A). This thermome-

Jan 1, 1970

By Benjamin Petkof

The mineral mica, which has been known to man since ancient times, has played an impor¬tant role in the development of our modern industry. In the latter part of the 19th century sheet mica began finding use as a dielectric insulating material in the newly developing electrical industry. Later, when modern elec¬tronics began to develop, it became a vital insulating and dielectric material for use in electronic equipment. Both the electrical and electronic industries were greatly dependent on some form of natural mica. The manufacture of electric motors of varying sizes, electronic tubes, and other electronic items was dependent on an adequate supply of sheet mica. During World War II this material was so vital to national defense that special efforts were made to mine it in the United States as well as to obtain it from overseas mica-producing areas. However, advancing technology has successfully begun the progressive development of man-made mica-based and non-mica-based materials that can replace mica for many uses. In addition, developing technology has dictated changes that have made sheet mica unnecessary for some uses. As the demand for sheet mica declined, the demand for scrap and flake mica has continued to increase. In fact, today the domestic production and use of scrap and flake mica far outshadows the necessity for good¬quality sheet mica in this country. Historically the United States has always been dependent on foreign sources of material for good-quality sheet mica and imports practically its entire requirement. In the case of scrap and flake mica, the United States is the dominant world producer and consumer. End Uses Sheet mica (Chowdhury, 1941; Rajgarhia, 1951; Skow, 1962) is available in many com¬mercial forms, but these forms can be broadly classified into manufactured and unmanufac¬tured mica. Manufactured mica consists of mica that has been shaped, punched, or other¬wise processed into some form, suitable for a particular end use. Unmanufactured mica con¬sists of partially hand-trimmed or processed material that has not been prepared for any particular end use. Unmanufactured mica is broken into two commercial classes consisting of sheet mica and scrap and flake mica. These classes of mica differ greatly in their ultimate end uses and marketed forms. Sheet muscovite mica can be classified by color, degree of prep¬aration of the crude material, thickness, size, visual appearance, and electrical quality. In addition, phlogopite mica is also classified by its thermal stability. Scrap and flake mica consist of mine, trimming shop, and factory scrap that occurs as remnants from mining, processing, and manufacturing operations, and small particle size mica that is available from the beneficiation of pegmatites, clays, schists, or other mica-rich host rock. The end uses for sheet mica vary so greatly from those of scrap and flake mica that it is necessary to discuss them separately. Sheet Mica Sheet mica consists of relatively flat sheets of material which have been mined as naturally occurring books or runs of mica. These sheets are hand-trimmed to remove any imperfections and are punched or stamped into specified shapes for industrial use. Sheet mica can be further processed and is described or specified as block, film, or splittings based on thickness. Block mica is not less than 0.007 in. thick with a minimum usable cross-sectional area of 1 sq in. Film mica is split from the better quali¬ties of block mica to specified thickness groups ranging from 0.0012 to 0.004 in. Splittings are sheets of mica with a maximum thickness of 0.0012 in. and a minimum usable area of 0.75 in. Other small sized, lower quality block mica

Jan 1, 1975

By Byron W. Cheever

While engaged in experimenting with the usual methods for estimating phosphorus in iron and steel, it occurred to me that potassium chlorate might be used to oxidize the carbon, and thus avoid the tedious and vexatious evaporations necessary for successfully carrying out the usual methods. After many trials, the following plan was adopted : Take, for analysis, of Bessemer or other low-carbon steels, from 3 to 5 grammes; of crucible steel, 10 grammes; of pig-iron, 1 to 5 grammes, according to the percentage of phosphorus supposed to be present. Of iron, high in phosphorus (1 per cent.), take 1 gramme. Place in a No. 4 evaporating dish the amount of iron or steel decided upon, cover with a funnel which will just fit inside the dish, and then add gradually HNO3, (1.20 specific gravity), using 12 C.C. of acid for each gramme of steel or iron taken. (A larger quantity of acid will be required for small samples.) When the full amount of acid has been added, and the violent action has ceased, place the evaporating dish on a sand-bath, add 10 C.C. HNO3, (1.40 specific gravity), and boil till the bulk of the solution is reduced about onehalf. Then add 10 C.C. HNO3, (1.40 specific gravity), continue the boiling, and add from time to time, during the next 15 minutes, small portions of pulverized KCIO3, till about 2 grammes have been added. (If the solution shows signs of going dry, more strong acid must be added.) This will precipitate the manganese, with some iron. Sometimes it happens that the manganese does not come down readily, and more KCIO3, or further concentration, or both, will be required. The process is not complete till the manganese is precipitated, which may be known by the appearance of a dark, mirror-like deposit on the dish, at the edge of the solution. Boil the solution 5 minutes after the last addition of KCIO3, and then add cautiously (to prevent sudden explosions) 5 C.C. strong HCl. This will dissolve the precipitated manganese and iron. Continue the boiling till the chlorine is all expelled, adding from

Jan 1, 1885

AVING started to tell you of working potter's clay for making crucibles and shells, the wish came to me to tell you of the practice of this art also. Although it may seem at first glance to be outside the order and purpose of my writing, he who considers well will see that it is not unrelated to it but proper, since it is wholly dependent on the agency and power of fire if it is to be brought to its perfection. Moreover, the potter's glazes and colors are all substances of various metals or impure minerals and therefore belong to fire. Since it is my intention to treat of fire, minerals, and metals for you, I surely should not have omitted this, particularly because it is a necessary art which enriches and is greatly praised both for its ingenuity and its beauty. The art of the potter has two sources as its principal basis. One comes from the art of design, the other from various alchemical secrets and elemental mixtures. In regard to these, I find that, in my opinion, all this art depends in the last analysis on four things: on good judgment in general, and on the art of design so as to be able to make the vessels beautiful and of good shape, as well as to ornament them with painting; after baking them well the first and second times, the next thing is to know how to make and apply the glaze well and to paint them with varied and appropriate colors. The fourth is to see that you have good, fine clay without small stones or lumps-indeed this is to be considered as the first thing. Now this that I have called clay is what many call cretaceous earth and some call argil. It is found and dug up when the masters wish to make use of it and is put in a container to be moistened. When it is moistened, it is beaten on a bench with an iron rod and very well prepared. Mixing it carefully, every small stone, lump, or other hardness that it contains is removed and cleaned away. Then a shaft [145V] of iron is fitted as the journal in a large wheel. On the other end of the journal a small wheel is made which forms an instrument for working that is called a lathe. Having put some clay on this, it is made to rotate by pushing with one foot, and, by rotating it, vessels are worked into a pleasing shape and size. Then they are taken off and put on a board to dry. After drying artificially or naturally they are painted red,

Jan 1, 1942

By J. J. Fischer

COMPOSITES containing cold-drawn, high-strength steel wires have shown promise for normal and slightly elevated temperature applications, particularly where strength-to-weight ratios or corrosion resistance are important.'-3 Although tensile strengths up to 500,000 psi may be obtained by cold drawing these wires, processing the composite at elevated temperatures will result in a rapid decrease of the wires' strength. In wrought maraging steels, high-strength levels can be obtained by aging at 900' . Because these alloys do not rely on heavy cold working to achieve their strength, and because they do not overage readily, they are of potential interest for use in composites. In view of this, the tensile strengths of composites containing The total heat effect thus represents the heat of formation, AHf of the compound at 273' . Since the heat of solution of tin in the tin solvent bath is zero, AHz = 3( - H273)Sn and Hf is given by: For LaSn3, AH3 had a measured value of 11,285 i 380 cal per g-atom while for La2Sn, the corresponding value was 33,658 870 cal per g-atom. Using the measured data for the compounds and pure lanthanum, a value of -15,150 200 cal per g-atom was calculated for the heat of formation of LaSn, at 273°K, while Hf for La2Sn3 was found to be -28,090 400 cal per g-i&om. The authors would like to acknowledge the financial support of the Army Research Office, Durham, North Carolina. under contract No. DA-31-124-ARO-D-384.

Jan 1, 1969

By J. B. Conway

RECENT studies of first-stage creep data have led to a special least-squares procedure for use in calculating the Andrade creep-equation constants. This procedure is easy to apply, uses only experimental data, and yields results which do not vary with the individual making the analysis. Taking logarithms of the Andrade equation I = lo(1 +ßl1/3)ekt leads to In l = In lo + In(1 + ßl1/3) + kt A residual can then be defined as the difference between the logarithm of an experimental length value and the logarithm of a calculated length value. Following the usual least-squares approach differentiation with respect to 10 and k of the expression for the sum of the squares of the residuals leads to two equations which cannot be solved directly for the three constants involved. However, values of ß can be assumed and corresponding values of lo and k can then be calculated. Then the sum of the squares of the residuals can be calculated. For a certain value of ß this sum will exhibit a minimum value to identify the least-squares values for ß, lo, and k. An illustration of the application of the above least-squares approach is obtained by employing the creep data for lead originally presented by Andrade' in the development of the one-third creep law. A plot of the sum of the squares of the residuals as a function of ß is shown in Fig. 1 along with the corresponding lo and k values. The minimum is seen to occur at ß = 0.0143 from which lo = 39.149 and k = 7.27 x 10-5. Based on these results the Andrade equation for these lead data is 1 = 39.149(1 + 0.0143 t1/3)e7.27 x 10-5t compared to the equation I = 39.13(1 + 0.01457/l/3)e6.95 X 10-5t developed by Andrade (calculation procedure not given but was probably a graphical solution). Calculating length values using the above equations and comparing with the experimental length values, residuals corresponding to the difference between experimental and calculated length values can be obtained. The sum of the squares of the residuals can then be calculated. For the case of the least-squares approach a value for this sum was found to be 2.37 x 10-3 compared to a value of 3.47 x 10" for the equation originally proposed by Andrade. In other words, while the constants proposed by Andrade provide an excellent fit for the lead data, a still better representation is afforded by applying the least-squares approach discussed above. A similar result was obtained for the lead data at 162oc.l The least-squares approach led to 1 = 9.866(1 + 0.0497 t1/3)el.011 x 10-2t compared to the equation I = 9.94(1 + 0.0433 l1/3)e1.06 X 10-2t given by Andrade. In this case, too, the sum of the squares of the residuals is slightly smaller for the equation based on the least-squares approach. It should be pointed out that a double trial and er-

Jan 1, 1965

By Robert D. Pehlke, Robert G. Blossey

The solubility of nitrogen in liquid iron alloys containing chromium and nickel has been measured in the temperature range 1550° to 1700°C at nitrogen pressures to 1 ah. The solubility surface has been determined for the iron corner of the liquid metallic ternary to 21 pct Cr and 11 pct Ni. The nitrogen solubility increases markedly with increasing chromium concentration. The effect of nickel and the bilinear effect of chromium and nickel are less pronounced. The solubility data are presented, and interaction coefficients are determined from them. THE solubility of nitrogen has been determined in liquid Fe-Cr-Ni binary and ternary alloys. The work in this laboratory has been directed toward a relatively limited composition range, that is to 20 pct Cr and 10 pct Ni. Humbert and Elliott1 studied the entire ternary; but their investigation was, understandably, limited in this region. The region considered here is of the greatest commercial interest. Knowledge of the solubility in these alloys is important for accurate control of the nitrogen levels in various stainless alloys. Also, the solution behavior is of theoretical interest because of its deviations from ideal dilute solution rules at moderate chromium levels. The nitrogen solubility in the iron binaries has been reviewed extensively by Pehlke and Elliott,2 particularly with respect to the dilute solution interaction parameters. More recently, there has been some interest in accurate descriptions of solute interactions in non-dilute solutions. Most of the investigators have adopted a power series fit to accommodate any non-linearity of the data. The Taylor series expansion is adopted here, using Scimar's notation3 for the interaction coefficients. An alternate method, instead of requiring higher-order expansions, is to restrict the range of the composition variables. A planar solubility surface may be fitted to the data and its range of validity determined. If the axes of this region are displaced from the usual origin—the solvent pure iron—a change in standard state is required for the solution reaction. The standard state for nitrogen in iron is commonly taken as the hypothetical 1 wt pct solution of nitrogen in pure iron. However, for an alloy of appreciable solute concentration, e.g., 13 pct Cr or 18 pct Cr-8 pct Ni, it would be convenient to use that base composition as the solvent and redefine the solution reaction in terms of that particular solvent. A brief derivation follows, defining the free energy of solution in an alloy solvent. Following the treatment by Darken and Gurry,4 for a nitrogen pressure of 1 atm: N (pure component) = N (1 wt pct in solvent) [l] AG=RT ln100/ wt pct N in solvent Taking this reaction for an alloy solvent less the same reaction for a pure iron solvent the relation between nitrogen in pure iron and an alloy is: N (1 wt pct in Fe) = N (1 wt pct in alloy) [2] AG = RT[ln(wt pct N in Fe) - ln(wt pct N in alloy)] Adding ½ N2(g) to each side and subtracting N (1 wt pct in Fe) = ½N2(g), the total free energy for solution of nitrogen in an alloy, referred to nitrogen at infinite dilution, is given by: ½N2 (g) = N (wt pct in alloy) L3] AG°3 = -RT ln(wt pct N in alloy )PN =1 atm Interaction parameters have their usual meaning when ?G°/RT is differentiated with respect to the proper composition coordinate. If desired, the dilute alloy treatment may be utilized with the new reference composition as the solvent. This has. indeed, been done by Small and pehlke5 in their analysis of nitrogen solution in liquid 18-8 alloys. The Sieverts' technique was used for this investigation on an apparatus previously described.6 The materials used in this program were: Ferrovac-E iron, 99.95 pct, Crucible Steel Co.: chromium, 99.95 pct, Union Carbide Metals Co.; nickel, 99.9 pct, International Nickel Co. Recrystallized alumina crucibles were used with no evidence of crucible-melt reaction. RESULTS The locations of the ternary compositions investigated are shown in Fig. 1. The data of Turnock7 and small8 have been alluded to in other papers.5'6 There were no departures from Sieverts' law observed for

Jan 1, 1969

PRESIDENT AND DIRECTOR D.C. JACKLING SAN FRANCISCO, CALIF. PAST PRESIDENTS AND DIRECTORS NEW YORK, N. Y. R. C. ALLEN- CLEVELAND, OHIO VICE-PRESIDENT, TREASURER AND DIRECTOR KARL EILERS-* NEW YORK, N. Y. VICE-PRESIDENTS AND DIRECTORS HENRY KRUMB NEW YORK, N. Y. PAUL D. MERICA . NEW YORK, N. Y. H. G. MOULTON NEW YORK, N. Y. HARVEY S. MUDD Los ANGELES, CALIF. WILFRED SYKES CHICAGO, ILL.

Jan 1, 1938

By Gernot Kostorz

In a recent paper, Raffo and itcheell1 compared solid solution hardening of various bcc alloy single crystals at room temperature and concluded that the expression for localized elastic interaction between dislocations and solute atoms2 that gives the critical resolved shear stress (CRSS) 7,: to = Z . µE3/2 C1/2 where c = concentration, e = misfit parameter, (µ = shear modulus, Z = numerical constant Fig. 1—The slope dT0/dc1/2 for niobium alloy single crystals deformed at 570°K plotted against the misfit parameter € = In' I + 1616 I. from Ref. 6, •estimated from Ref. 7. Table I. Plateau Hardening and Alloy Parameters for Niobium Alloys dT0/dc1/2, kg/mm2 Solute Ref. 6 Tantalum 3.7 ± 0.3 1.9 0.73 + 0.06 9 0.0 ± 0.5 15 Vanadium 16.1 ±1.4 - 0.69 i 0.01 9 -7.4 ± 0.5 16 Tungsten 12.5 ? 1.5 20.9 0.92 i 0.05 10 -5.0 t 0.4 17 Rhenium - 25.9 1.24 11.12 -8.5 ± 0.4 I5 Molybdenum - 14.6 1.04 13,14 -4.6 s†±?˜µ?fF?? 0.5 17 Hafnium - 13.9 0.37 12 4.8 ± 0.5 17 Table 11. Solid Solution Hardening and Alloy Parameters for Tantalum Alloys i)' dTo/dc1/2 kg/mm2, dTp/dc1/2 kg/mm2, Ref. 22 1006 Solute ˜570°K Ref. 7 See Text Ref. 25 Rhenium 44.3 32.5 0.65 -8.5 Tungsten 32.1 24.3 0.34 -4.6 Molybdenum 29.3 19.1 -0.19 -5.9 Niobium 5.8 5.5 -0.43 0.I

Jan 1, 1970

By George B. Lee

DURING The Two Years In Which The New Reduction-Works Of The Copper Queen Consolidated Mining Co. Have Been In Operation At Douglas, Ariz., There Has Developed A Remarkable Condition In Regard To The Corrosive Action Of The Water Used To Cool The Jackets Of The Blast-Furnaces. Were It Not For The Many Contradictory Features, It Might Pass As One Of The Unavoidable Troubles Due To The Composition Of The Water. This Water, Obtained From Wells 600 Ft. Deep, Is Also Used In The Steam-Boilers, And Its Composition, As Shown By The Following Analysis, Does Not Indicate The Presence Of Any Ingredient Which Would Explain The Corrosion Grains Per U. S. Gal. Silica, 0.861 Iron Oxide And Alumina, 0.223 Calcium Carbonate, 0.2111 Calcium Sulphate, Magnesium Carbonate, Sodium And Potassium Sulphates, . 14.850 Sodium And Potassium Chlorides, 9.732 Sodium And Potassium Carbonate, 6.452 32.409 The Jackets Are Made Of Inner Plates 0.5 In. Thick And An Outer Plate I In. Thick, With 3-In. Stiffeners Between The Inner And Outer Plates. In From 10 To 12 Months The Inner Plates Have Been Reduced By Corrosion To A Thickness Of From 1/8 To 1/16 In., While The Outer Plate In The Same Time Is Reduced By Less Than 1/16 In., And The Stiffeners Show Very Little Corrosion. The Plates Are Pitted And Eaten Away In Some Places More Than In Others. There Is Practically No Scale Found On The Jackets, But When Cleaned Considerable Iron Oxide Is Found In The Bottoms. With An Action So Marked, Serious Trouble Would Be Expected In The Boilers, But, On The Contrary, A Recent Inspection By a

Mar 1, 1908

For the benefit of those of our members who are considerable holder; of securities, but owing to their isolated situations are not in close touch with the metropolitan market and current quotations, we are publishing two very interesting graphs, showing the course of the bond and stock markets in New York over a long period. These graphs are-fui?riished through the courtesy of the financial department of the New York Tribune.

Jan 8, 1919