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Jan 1, 1959

By Frederick Laist, H. J. Maguire

The ore from the Butte mines of the Anaconda company is quite siliceous; that is, it contains considerably less iron than is needed for the fluxing of the silica. The direct smelting of this ore, therefore, requires the addition of considerable fluxing material. The only flux available in sufficient quantity at Anaconda is limestone containing no metallic minerals. This necessarily makes the direct smelting of the ore so expensive that it is more profitable to subject the ore to a preliminary treatment by concentration. However, as the losses in the concentrator were very high, compared with the losses in the blast furnaccs, it was found, by calculation, more profitable to send ores containing more than a given percentage of copper to the blast furnaces, in spite of the higher costs of treatment. The dividing point was dependent on various factors, the chief of which was the prevailing market price of copper. It was customary, therefore, to segregate the ore as mined into two classes. Ore in the first class generally contained 5 per cent. or over of copper; this was sent directly to the blast-furnace department. Second-class ore contained less than 5 per cent. of copper, and averaged around 3 per cent.; it went to the concentrating department. With the introduction of the flotation process, it mas found possible to maintain an average recovery, as concentrates, of 96 per cent. At the same time, the cost of reverberatory smelting was very materially decreased by the use of pulverized coal. These two changes in practice made the blast furnaces unable to compete with the reverberatory furnaces on a cost basis. The distinction between first- and second-class ore was therefore abandoned, and the ore was treated by concentration. Obviously, on ores as high in iron as the Butte ores, the concentrator produces a product that is self-fluxing; in fact, it is possible to produce a concentrate containing more iron than is necessary to flux the silica. Under these conditions, the amount of basic fluxing materials required for the smelting operations became very srnall and the converter slag lost its former value as a blast-furnace flux. For this reason, a less expensive method of recovering the copper, silver, and gold contained in it than smelting in blast furnaces had to be found. It was not feasible

Jan 1, 1921

By George Norman

A NUMBER of methods have been developed for the determination of the dust concentration in air, some of which have been reported as very efficient and for research may be more satisfactory than the method about to be described. In practical mine use, however, the accurate research equipment is unwieldy and requires a high degree of technical skill to manipulate it. Also, it gives less general practical information to the operator in the same length of time than the method described here. Moreover, it is doubtful whether at the present stage of affairs the results obtained from the precise methods have any more practical significance than those obtained with simpler and more portable appara-tus, which can rapidly give a sufficiently reliable indication of the rela-tive dust hazard.

Jan 1, 1937

THOSE MARKED THUS * ARE MEMBERS, MARKED THUS ?ARE ASSOCIATES. THESE SIGNS DOUBLED INDICATE LIFE MEMBERS AND ASSOCIATES RESPECTIVELY. THE FIGURES AT THE END OF THE ADDRESS INDICATE THE YEAR OF ELECTION. HEAVY-FACED TYPE SIGNIFIES HONORARY MEMBERSHIP. *AARONS, J. BOYD, Vivian Gold Mining Co., Ltd., Harris, West. Australia. '05 *ABADIE, EMILE R., Cons. and Min. Engr., 214 Union Savings Bank Bldg., Oakland, Cal. '76 ?ABBÉ, MAX F., Prest., Abbé Engineering Co, 220 Broadway, New York, N.Y. '07 ? ABBÉ, PAULO., Secy.,Abbé Engineering Co., 220 Broadway, New York, N.Y. '07 *ABBOTT, CHARLES W., Min. Engr. Pioche, Nev. ?08 *ABBOTT, CLARENCE Chief EDgr., Iron Mines, Dic Tennessee Caol, Iron & R. R. Co., Bessemer, Ala. '04 *ABBOTT, JAMES W., Min. Engr: Ploche, Lincoln Co., Nev. '94 *ABE, MASAYOSHI, Prof. of Mining, Imperial University Kyoto, Japan. '05

Jan 1, 1910

By G. L. Oldright, F. W. Schroeder

Very great changes were made in the dimensions of the smelting hearths of the furnaces in the period from about 1800 to 1906, the length increasing from about 11 to 116 ft., and the width from 8 to 19 ft. During this time the tonnage smelted increased from about 9 to 250 tons per 24 hr., and the tons of charge smelted per ton of coal increased from 0.77 to 4.3. Dr. Mathewson3 noted no great difference in the "fuel ratio" (i. e., the amount of charge smelted per ton of coal) as the furnace at Anaconda was increased in length by stages from 85 to 116 ft. (The percentage of copper in the slag, however, was lowered from 0.42 to 0.36 per cent. The other components of the slag were not given.) Lump coal fired on grates was the fuel used during this period. The practice in operating the furnaces over such a length of time naturally varied considerably, and there were differences in composition and nature of the charge, yet it may he considered that the improvements made were due largely to increases in the size of the furnace used. Doubtless some credit should be given to improvements in operating technique, like changes in the methods of firing the lump coal. However, the greater part of the advance was probably due to factors influencing the

Jan 1, 1928

By E. M. Wise, T. E. Kihlgren, N. B. Pilling

SYSTEMATIC data are presented on the relation of composition of nickel silvers to color, tarnish resistance, hardness and liquidus temperatures, for alloys containing up to 30 per cent nickel and 50 per cent zinc, further modified at certain nickel and zinc contents by 0 to 8 per cent of tin and 0 to 10 per cent of lead. Attention has also been directed, using a still more limited range of alloys, toward a study of tensile properties and such casting properties and characteristics as fluidity, shrinkage and pressure tightness. In some of these, rather broad ranges of composition are dealt with; in others, it has been expedient to focus attention on the Federal Specification 20 per cent nickel silver casting alloy, WWP-541.

Jan 1, 1935

By J. W. Hickman

Most of the electron diffraction studies of oxide films which form on metals and alloys have been carried out by oxidizing the specimens in an auxiliary furnace, cooling down to room temperature and then inserting the sample in the camera and taking a diffraction photograph. Prior to the investigations at the Westinghouse Research Laboratories, no systematic study of the oxidation of any metal or alloy had been made over a wide temperature range with photographs taken at elevated temperatures except the investigation of iron by Jackson and Quarrell.' In order to interpret the electron diffraction patterns of the oxides which may form on alloys, it seemed advisable to make a comprehensive study of the oxidation of the purest metals available in the bulk form. Thus far studies have been completed on iron,2 cobalt,~ nickel,= chromium,= copper,z tungsten,s molybdenum,3 beryllium,' uranium,' thorium,' titanium6 and zirconium6 while investigations are in progress on tantalum and columbium. The next step in the study is concerned with the investigation of the oxides which form on binary alloys. Some of the alloys consist of a single phase while others contain more than one phase. The identification of the oxides on the surface of a binary alloy may be more difficult than on the metals since oxides containing both metals as well as those of each metal separately may form. Furthermore, it is possible that solid solutions of the various oxides may occur. In these cases the electron diffraction method may not be able to identify the oxidation products unequivocally. Examples of solid solutions which may present difficulties are MOO* and WOp, Fe304 and FeO.CrnOa since the diffraction patterns are so similar. Since electron diffraction can determine only the structure of the oxide, the chemical composition must be inferred from the diffraction data based upon X ray diffraction investigations of specimens of known composition. It is possible in some cases to decide whether a given solid phase reaction can occur on the surface of an alloy by a study of available thermodynamic data. Table I lists the equations for the formation of most of the oxides from the elements together with values of loglo Kg for the several temperatures. AF"B = -RT In KR AF°R and KR are the free energy and equilibrium constant of the reaction. Calculations may be made using the the given in I 1 to determine whether a given solid phase reaction is possible thermodynamically. For example, a solid phase reaction should occur between aluminum and chromium oxide to form

Jan 1, 1949

By G. W. Tower

THE YEAR 1931 was for most American copper producers one of restricted output but extremely low production cost.. When compared with 1929, the marked reductions in costs achieved in 1931, operating at rates in many instances a third to a half of capacity, can only be regarded as remarkable. In fact, the recent shut-down of several large operations suggests the probability that 1931 costs represent a bare minimum for many properties. Before discussing the 1931 results a few remarks on cost data are appropriate. The type of cost tabulation here presented was first published in 1929, (A. B. Parsons. E. & M. I. June 8, 1929), and has appeared each, succeeding year following in general the calculation method and company set-up of the original article. (. G. W. Tower, E. & III. L, July 8. 1930; S. D. Strauss, E. & M. J.; July 27, 1931). As far as possible the leading American copper companies are included. In considering these cost tabulations it must be borne in mind that the information from which they have been prepared is entirely contained in the annual report of each company; and that a multiplicity of interests and a condensed income statement for some of the larger companies, such as Cerro de Pasco and Kennecott, make the cost figure an arbitrary one depending upon sundry metal credits, metal products, miscellaneous income, etc. For Granby, Howe Sound. Magma, and Noranda, sundry metal credits are important. Furthermore Andes, Chile and Greene Cananea give costs only against copper sold. Although the individual costs here figured are by no means absolute they are computed by the same method each year and offer a basis of annual comparison; and with attention to footnotes the premises on which the costs are based may be easily followed.

Jan 1, 1932

By A. F. Colombo, R. T. Sorensen, D. W. Frommer

An analytical method has been developed and used in batch and continuous tests to provide initial insights into the effect of soluble calcium ion in anionic flotation of silica from iron ores. A deficiency or excess of calcium ion in pulps subjected to this type of flotation produces an impairment in flotation efficiency. Data developed in the investigation are from a single ore, but show that total calcium requirement is met from water, ore and reagent sources. In batch studies, starch additions were shown to exert no influence on the calcium level, but fatty acid and sodium hydroxide had subtractive effects. The investigation was next extended to continuous flotation testing where the general observations from batch testing were confirmed. Factorially designed experiments were performed showing that the relationship of calcium additions to flotation response was not a simple one, but tended to shift to higher additions with increased fatty acid. Nevertheless, the range of soluble calcium levels measured remained fairly constant in areas of good flotation response. It is concluded that techniques developed should be useful in removing empiricism from flotation operations in this and other systems requiring activation for success. Further development should aid in process control both through methods outlined and through investigations aimed at studying the effects of other soluble reagents. Of the major mineral commodities, iron ore was one of the last to succumb to flotation processing. Commenting on this fact, one of the speakers 1 at the convention celebrating the 50th Anniversary of flotation in the U.S.A., said ". . . in 1951 froth flotation as a means of beneficiating nonferrous minerals was a might giant and could be characterized by 'you name it, we float' - but not iron ore". This tardiness in applying flotation to iron ores was the result of a number of factors, including economics and ready availability of direct shipping ores. Even now, when the need for beneficiation can no longer be denied, proposals for flotation of iron ores are apt to be viewed with some misgivings. This disquiet results from knowledge that wide variability, which would necessitate corresponding adjustments in reagents, often exist within even a single ore deposit. Coupled with ore variability is the fact that, at present, there is no way of quickly and precisely anticipating the direction and magnitude of reagent changes required for uninterrupted production of acceptable concentrates. Despite the long delay, iron ore flotation is now practiced commercially, although the chief applications2-4 are to specular hematites having relatively coarse liberation and low slime content. In addition, the application of flotation in upgrading magnetic concentrates seems assured. However, these flotation methods do not appear applicable to substantial tonnages of fine grained, earthy, and frequently more complex semitaconites and nonmagnetic taconites. The U.S. Bureau of Mines, in devoting its attention to the semitaconite and nonmagnetic taconite class of materials, has demonstrated that anionic flotation of calcium-activated silica can be utilized with an expected high frequency of success.' Even so, it has been recognized that the flotation method is a complex one, and that the reagent suite must be carefully tailored to the feed. These conditions would be expected to offer difficulties in treating ores with the wide range of variability previously discussed. Accordingly, research was initiated to develop methods to remove much of the empiricism from the flotation operation by measuring the reagent variables within the pulp for a correlation with flotation response. A simple illustration of the technique sought would be in the well established use of pH meters to provide feedback control to reagent feeders and thereby limit acidity or alkalinity to a range producing optimum results. The first efforts in this area have been concerned with measurements of soluble calcium ion. Bureau experience in both laboratory and pilot plant over the past five years has proved that the amount of calcium

Jan 1, 1965

By Royal Jackman

Two comprehensive papers have appeared regarding the forms of copper that occur in smelter slags, one by Frank E. Lathe1 and the other by C. G. Maier and G. D. Van Arsdale.2 These authors comment on other published results and draw conclusions from their own investiga-tions. The development of X-ray examination of minerals and improve-ment in high-power microscopic methods make it possible today to get additional evidence by means that were not available to earlier investi-gators. The present work was confined to reverberatory slags obtained from five different plants. Some definite conclusions were reached regarding the forms of copper present in these slags. In most cases these agree with some of the findings of Maier and Van Arsdale but new methods of attack were used in the investigation.

Jan 1, 1933

By Martial P. Corriveau

Almost everyone agrees that coal and oil shale are the only fossil fuel resources in which the United States is self-sufficient. Of the two, only coal has a technology sufficiently developed to be of intermediate term benefit. Since it takes at least 20 years to bring advanced technology into practice, it seems logical that the major focus on energy developments should be aimed at coal. Meanwhile, we need to trade-off between actions to meet our immediate needs and the various political regulations and social demands that are disrupting the coal industry and the industries dependent upon it. The largest single user of coal is the electric power generation industry. Over 300 million tons of coal are presently being consumed each year. In view of the 5-to 7-years lead time to bring in a base-load fossil-fuel fired generating station, our requirements for double this tonnage in 1980 are already well forecast; that is, if the coal companies are allowed to mine and the utilities are allowed to burn the coal.

Jan 2, 1974

By A. M. Gaudin

CHANGES in industrial practice, in plant design, and in research methods which are so clearly to be seen on every hand, have affected the mineral industry as well as others. In particular, ore dressing has passed through a revolution in practice brought about by the introduction of flotation and other quasi-chemical methods, until it has ceased to be solely the mechanical preparation of ores. In fact, the term "ore dressing" itself is obsolescent, and "mineral dressing" has been growing in popularity. This assures adequate recognition of the fact that mineral substances other than ores, e.g. coals, clays, and cement rock, are treated by the same general methods. As a result of these industrial changes it was felt that a complete rearrangement of the curriculum and laboratories at the Massachusetts Institute of Technology would be ad-vantageous. Such a rearrangement would allow instruction and research to proceed in wider accord with industrial evolution and the needs of our times.

Jan 1, 1942

By Kefton H. Teague

Attempts to locate domestic supplies of sillimanite have been unsuccessful until recently. This paper describes recent discoveries of sillimanite-bearing schists in the Southeastern States, with emphasis on geology of the deposits, mineral composition, origin, and reserves. Statements concerning possible methods of mining, milling, and utilization of sillimanite are given. Results from refractory tests on a laboratory scale are summarized.

Jan 1, 1950

By Frank J. Markewicz, William Lodding

Greensand, greensand marl, and green earth are names given to sediments rich in the bluish green to greenish black mineral known as glauconite by the mineralogist. The word glauconite is from the Greek word glaukos, meaning bluish green. The term "greensand" as a rock name for a glauconite-bearing sediment is more appropriate than "greensand marl," a term that has been doggedly perpetuated in the literature. Because of its potash and phosphate content, greensand was dug and marketed as a fertilizer and soil conditioner for more than 100 years. The advent of prepared fertilizers with adjustable nutrient ratios led to the decline of green- sand for agricultural application. The material has since been recognized for use in water treatment. Unfortunately, in spite of large reserves and worldwide distribution, the mineral has not been utilized to any significant commercial extent because no major application has been found for a substance with its chemical composition and properties. This lack is probably due to a paucity of research on its potential commercial application. Extraction of potash received considerable attention during and just after World War I. Because of relatively high extraction costs and generally low potash content (up to 8%), glauconite lost its appeal as a source of this commodity. Historical Background Greensand was used as a fertilizer in New Jersey in the latter part of the 1700s. During the early 1800s its use became more common; applications of up to 100 tons per acre were sometimes made, although recommendations for agricultural use suggested 20 to 50 tons per acre (Tedrow, 1957). Many crops, especially the forage type, were said to improve with greensand application; however, because of slow release of potash, large quantities were required. Certain greensands that contain sulfur and sulfide minerals are harmful to plant growth, and these were classified as "poison," "burning," or "black marls." The availability of higher-grade potash salts from other mineral sources, and the manufacture of prepared fertilizers, displaced the agricultural use of green- sand during the later 1800s. During the mid-1800s the domestic greensand industry, centered in a small section of the eastern United States, grossed more than $500,000 per year. Toward the end of the century, annual production had dwindled to less than $100,000. By 1910 there were only six or eight greensand producers, grossing less than $5000 (Tyler, 1934). There was a small revival in the industry during World War I because of the curtailment of foreign potash, especially from Germany. During the later 1940s and early 1950s greensand was again recommended as a food nutrient for plants and farm crops. Agronomic studies discussed its potential as a soil additive that gradually releases potash and many trace- element nutrients essential for plant growth (Tedrow, 1957). Greensand was sold with the idea that it would condition soil and absorb and hold water while its base-exchange properties would release trace elements. For a short time glauconite was utilized in certain parts of New Jersey as a binding additive in the brick industry, and in the 1800s for making green glass (Cook, 1868). In the early 1900s the base-exchange property of glauconite was recognized for water treatment, and the mineral gained acceptance as a water softener. Mansfield ( 1922) does not mention base-exchange; however, the base ex-

Jan 1, 1975

By C. W. Goodale

I. INTRODUCTION. In the summer of 1909 the Boston & Montana reduction department of the Anaconda Copper Mining Co. completed a new flue system, at a cost of about $1,100,000, and -is this includes the largest and highest chimney in the world, and some new features of flue construction, a description will be of interest. At the Spokane meeting of the Institute in September, 1909, a brief mention was made of this flue system, in discussing Mr. Brunton's presidential paper on the Progress of Metallurgy in the West, and a promise was given that when a long enough time had elapsed, so that operating results could be given, a paper would be offered. The smelting plant includes blast furnaces, MacDougall roasters, gas-fired reverberatories, and converters.

Jan 8, 1913

Jan 2, 1953

By R. D. Pehlke, P. D. Goodell, R. W. Dunlap

The rate of dissolution of steel bars in molten pig iron has been measured experimentally in the temperature range 2300° to 2650° F. The rate of solution is shown to be a .function of bath composition, temperature, and stirring. A kinetic model based on carbon diffusion in the liquid phase has been derived to fit the experimental results. THE rate of scrap melting has long been an important variable in steelmaking operations. With the advent of the oxygen steelmaking process and the accompanying shorter heat times, the rate of scrap melting has now become one of the rate-limiting factors in steel production. As observed in commercial practice, the solution rate is influenced by the compositions of liquid and solid, the temperature, agitation, and time. However, no definitive work has been done on the Fe-C system, and there is very little information in the literature regarding the relative effects of these variables in steelmaking systems. A number of questions have been raised in regard to scrap utilization in basic oxygen steelmaking operations. Consideration has been given to the optimum size and shape of scrap, and to the use of preheated scrap as a means for decreasing the pig-iron requirement in oxygen blowing. The determination of an optimum scrap practice for a specific installation depends to a large extent upon the economics of the scrap market and also upon the behavior of scrap in the vessel. The present research was undertaken as a preliminary study in evaluating the behavior of steel in a pig-iron bath under various conditions of temperature, composition, and agitation, as might be encountered in oxygen converter operations or in any steelmaking operation where scrap behavior is an important process variable. Related studies have been carried out on non-ferrous systems. The solution rate of solid aluminum in a molten A1-Si alloy has been studied.' Furthermore, the increasing use of liquid metals has created considerable interest in studies related to dissolution of a solid in a liquid, or mass transfer taking place between a solid interface and a liquid metallic phase.2-10 In an effort to clarify the relative importance of factors influencing the dissolution of scrap in Fe-C alloys, this paper presents the results of a study of the rate of dissolution of a low-carbon steel cylinder in a molten Fe-C bath at various bath compositions, temperatures, and conditions of agitation. An attempt has been made to determine the mechanism of solution, and a model has been derived to fit the experimental results. The rate of heat transfer between the molten pig-iron bath and the solid-steel cylinder has also been studied. EXPERIMENTAL PROCEDURE A molten bath of pig iron (nominal composition 4.2 pct C, 0.5 pct Mn, 0.8 pct Si)* was held in a 200- *In view of the fact that the composition of the pig-iron bath was slowly changing with time because of steel dissolution and reaction with the surrounding atmosphere, intermittent samples of the liquid bath were taken throughout each experiment, Table 1. lb induction melting unit. The internal diameter of the furnace was 8-1/2 in. and the bath depth approximately 14 in. Cold-finished 1020 steel cylinders of 1/2-, 3/4-, 1-, 1-1/2-, and 2-in. diameters were cut into 1 -ft lengths for use as test specimens. One end of each bar was machined to fit a hand-driven, mechanical stirring device which rested on top of the furnace. This fixture permitted 7 to 8 in. of the bar to be immersed in the melt. The steel cylinders were cleaned to free the surface of grease and oxide. The rods, at ambient temperature, were immersed into the molten pig-iron bath. The melt temperatures studied in this investigation were 2300°, 2500°, and 2650°F. Different agitation conditions were achieved by operating with a) the power to the furnace, giving induction stirring; b) induction stirring plus mechanical stirring, using hand rotation with a chain and sprocket assembly at approximately 200 rpm; c) mechanical stirring alone with the power off; and d) the power off and no mechanical stirring resulting in minimum agitation, i.e., only that caused by natural convection currents in the bath. The samples were immersed in the melt for prescribed times ranging from 30 sec up to 6 min. Immersion times were measured with a stopwatch and temperature control of the melt was achieved by power adjustment following temperature measurement with an optical pyrometer. The measurements with the calibrated pyrometer were checked out to within less than 10°F with simultaneous thermocouple measurements. Following immersion, the bars were water-quenched and the diameters were measured with a micrometer at several positions on the reduced area, and by volumetric displacement. The dissolution rates calculated from the

Jan 1, 1965

By J. Chipman, N. J. Grant, H. L. Bishop

Lime and dicalcium-silicate crucibles were equilibrated with molten iron and liquid slags containing iron oxide and small amounts of sulfur. The oxygen content of metal, iron oxide activities, and desulfurization values of the slags were determined in the temperature range 1530 to 1700°C. The influence of magnesia in the slag and the temperature dependence of the solubility of lime in liquid iron oxide and the ferric oxide content were established. The temperature contour of the liquidus surface of iron-silicate slags saturated with lime and dicalcium silicate was also established at 1600°C. THE importance of the role that slag composition plays in the refining of steel has been known for many years. Numerous studies have been made using actual plant data in order to establish the relationship between the composition of the slag and metal during the refining of a heat of liquid steel. These results rarely represent equilibrium conditions since completion of the various chemical reactions involved in steelmaking is seldom realized. In order to establish quantitatively the equilibrium conditions existing between the slag and metal, several laboratory studies have been conducted in the past 20 years to determine the reactions important in slag control. These investigations have included studies of simple liquid basic and acid slags as well as more complex slag systems which approach those commonly found during the refining of a heat of steel. Since most of the previous studies of simple basic iron-oxide slags equilibriated with molten iron were made in magnesia crucibles, it was not possible to establish the distribution of sulfur and oxygen between molten iron and slags consisting only of the three essential components, lime, silica, and iron oxide. This investigation was undertaken to establish the equilibrium conditions for simple lime-iron oxide and lime-silica-iron oxide slags. Accordingly, it was expedient to prepare crucibles both of lime and dicalcium silicate to establish the equilibrium conditions between molten iron and iron-oxide slags saturated with the refractory materials and free from other components. The only other studies of the equilibrium between molten iron and lime-saturated slags are those of Fischer and vom Ende, 1, 2 in which the solubility of oxygen was determined in an air atmosphere. The

Jan 1, 1959

By B. C. Allen

The solubility of chromium in liquid silver and that of molybdenum and tungsten in liquid tin have been determined by equilibrating Ike Liquid in a crucible of the solule metal. Generally the weight of solute in solulion was delermined both chemically and from crucible weight losses. The resulting weight percent solubilily of chromium in silver as a function of absolule temperature T is given by log w = -6660/T + 4.02 in the range 960° to 1445°C, and that of molybdenlttrl in tin by log w = —5050/T + 1. 79 in the range 1200° to 2200°C. The values appear unaffected by minor changes in solute composition. Calculations aye made of the parlial molar heal and excess entropy of mixing. The estimated solubility of tungsten in tin is 0.001 pct at 2000°C. Evidence is presented that molybdenwm dissolves in tin without compound for mation and that tungsten and tin form W10Sn. RECENT developments in coatings, heat transfer, and brazing require a knowledge of equilibrium solubilities in a variety of systems at elevated temperatures. Of particular interest are solid-liquid interactions in metal systems involving dilute solutions. This investigation was undertaken since little is known about the phase relations or solubility of chromium in liquid silver or of molybdenum and tungsten in liquid tin.1,2 EXPERIMENTAL WORK As indicated in Table I, high-purity metals or those of known impurity levels were used. Crucibles were machined from chromium, molybdenum, and tungsten bar stock 1.3 cm diam and 2.2 cm long. Chromium rod was prepared by arc melting and extruding iodide process crystals.3 The five chromium impurity alloys were in the form of 0.6-cm-diam swaged rod. A Cr-0.06N* alloy was prepared by exposure to NH3 at 1150°C in a closed quartz capsule for 24 hr. Because significant nitrogen was lost during annealing in argon at 1600°C,4 the estimated level was 0.01 pct N. Chromium and Mo,W crucibles were outgassed at 1200" and 1600°C, respectively, at 3 X 10-5 mm. The solvent was placed In crucibles of the solute metal- 6 g Ag in chromium, 0.4 g Ag in the five chromium impurity alloys, and 4 g Sn in Mo,W crucibles. The silver and tin series were outgassed at 900" and 110O°C, respectively, and held at the desired solution temperature in a tantalum resistance furnace under 1.05 atm 99.995 pct Ar. An equilibration time of 0.5 to 1 hr was chosen since 0.3-, I-, and 4-hr anneals at 1235°C for Cr-Ag yielded similar results. Temperatures were measured optically to +10°C under essentially black body conditions which were checked against the melting point of silver. The Cr-Ag and Mo-Sn,W-Sn series were respectively equilibrated at 990° to 1400°C and 1200" to 2000°C. Vaporization losses were generally held to <1 pct by the argon. In the 1800" and 2000°C anneals for 0.5 hr, the crucibles were placed in tightly sealed tantalum cans which kept tin losses to <5 pct. After the anneals, the specimens were furnace-cooled. One anneal was made on small Mo-0.02 C, Mo-0.5Ti-0.lZr, and tungsten crucibles containing tin at 2200°C. The metals were sealed in an electron-beam-welded tantalum can of minimum volume. After the anneal, tin was still present in each crucible, none of which was severely attacked. After equilibration, the saturated solvent metal was selectively removed from the crucible by acid leaching. Weight losses sustained by the crucibles were determined from the initial weight minus the final blank-corrected weight after acid leaching. Chemical analyses were performed on some of the samples. Hot 1:l HNO3-H2O removed silver from chromium with the blank running <0.1 mg or <0.002 pct on measured solubility. Tin was removed from molybdenum and tungsten by hot concentrated HC1 with the respective blanks amounting to -0.004 and -0.0004 pct in the presence of tin. The insoluble residues were weighed and checked for composition. The leaching solutions contained traces of the solute metals which were analyzed by colorimetric methods, Diphenyl Carbazide for chromium, Thiocyanate for molybdenum, and Dithiol for tungsten. The total of the two percentages found from the residue and leaching solution minus the blank gave the desired solubility values. On the basis of annealing empty molybdenum and tungsten crucibles, weight losses due to MoO3 or WO3 volatilization were found to be generally 10.4 mg and affect measured solubilities by <0.01pct. RESULTS AND DISCUSSION Chromium-Silver . Since no intermediate compounds are reported to form in the Cr-An system,&apos; crucible weight losses and chemical analysis of the entire melt should provide reliable measures of the chromium in solution. Values obtained by the two methods are in agreement as shown by the results for unalloyed chromium in Table II and plotted in Fig. 1. Furthermore, the results are consistent with those previously determined by melting equilibrated silver out of the crucible and analyzing calorimetrically for chromium.&apos; On the basis of limited thermal analysis data, the solubility of chromium in silver has been quoted as 8 pct at the monotectic temperature of -1445°C.1 This investigation indicates an extrapolated solubility of 1.38 pct which is believed to be more reliable. At the eu-

Jan 1, 1968

By G. B. Craig, B. Ramaswami

The temperature and strain rate dependence of the flow stress ratio and the stvain rate dependence qi the flow stress of annealed polycrystalline a zirconiur were determined over the temperature range 30 0" to 1000°K. Some evidence was found for strain aging and discontinuous flow in the temperature ranges 520" to 650°Kand650" to 760°K, respectively. The Cottvell-Stokes relationship was obtained when deformation occurred by twinning as well as slip. The flow stress ratio showed a strong dependence on temperature and strain rate above 800°K. The expevirnental evidence indicated that the rate-controllitzg mechanism for the deformation of a zirconium above 800°K was dislocation climb, and that the deformation was not thermally activated in the range 520" to 800°K. The stacking-fault energy of a zirconium was estimated to be about 250 ergs per sq cm. A knowledge of the temperature and strain rate dependence of the applied stress necessary to deform a crystalline solid is essential for understanding the thermally activated processes occurring during deformation.&apos; Several experimental techniques have been developed for studying these processes.273 One of the techniques is the deter mi nation of the strain rate dependence of the flow stress at constant temperature. In close-packed crystals, it has often been observed that the change in stress due to a change in the strain rate varies linearly with the flow stress, (~1,&apos; This relationship, known as the Cottre ll-Stokes law, is obeyed when deformation occurs by glide alone. However, when deformation occurs by twinning as well as glide, there is disagreement among different investigators on whether the Cottrell-Stokes law is observed. Whereas Thornton et ~1.~find departures from Cottrell-Stokes law when twinning occurs in copper, ~avis~ and sasinski? find that Cottrell-Stokes law is obeyed when deformation occurs by twinning as well as slip in cadmium and magnesium, respectively. One of the main objectives of this study is to determine whether the Cottrell-Stokes law is obeyed when deformation occurs by twinning as well as slip. The second technique that has been used extensively to study the thermally activated deformation of crystals is the determination of the ratio of the flow stresses, at identical dislocation structures and con-

Jan 1, 1968