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By T. Rosenqvist

From the chemical, metallurgical, and mineralogical points of view, the importance of thermodynamic data for metal-sulphides and sulphur dissolved in molten metal has long been realized. Such data will give a basis for thermo-dynamic calculations of processes such as roasting and the distribution of sulphur between molten metal and slags. Furthermore, it will help us understand the chemical forces which tie sulphur to the metal and to the melt. Thermodynamic studies of solid sulphides and the equilibria between solid sulphides and metals have been carried out in a rather large number of cases by several investigators. An excellent review of this work is given by Kelley.1 On the other hand, very little is known about the thermodynamic properties of molten sulphides and of sulphur dissolved in molten metal. The only system which previously has been investigated in this respect is the iron/sulphur system. The purpose of the present investigation was primarily to obtain further data for metalisulphur melts and the system silver/sulphur was chosen, not because this system was expected to be of special interest in itself, but because the silver/sulphur system is a typical example of a metal/sulphur system. Because of the low melting temperatures, the work could be carried out without appreciable furnace and refractory difficulties. The sulphur in this system possesses a rather high escaping tendency compared to most other metal/sulphur systems. By the method employed (reaction with hydrogen to form hydrogen sulphide) this gives ratios Ph2s/Ph2 up to 0.30, which may be determined accurately. 'rhermodynamic investigations of the heterogeneous reaction Ag2S +H2 —+ 2Ag + H2S have previously been carried out by Pelabon,2 Keyes and Felsing,3 Jellineb and Zakowski,4 Wat-anabe,6 and Britzke and Kapustinsky.6 Their results are in rather poor agreement. Experimental Part PRINCIPLE In the present invehgation the escaping tendency of sulphur from the condensed phase was determined by the reaction: S + H2 = H2S The ratio Ph2s/Ph2 is at constant temperature, directly proportional to the escaping tendency of sulphur and to its chemical activity in the condensed phase. (This ratio will subsequently be denoted by H2S/H2.) From this ratio and its variation with temperature and with change in the com- position of the condensed phase, thermodyrlamic quantities such as free energy and heat of reaction can be derived. The apparatus used is shown in Fig 1. The silver/sulphur alloy was placed in a crucible inside a refractory tube and mounted inside the furnace to the left. The tube was a part of a closed, gas-tight system in which the gas mixture could circulate until equilibrium was established. Circulation was maintained by the glass propeller to the right, driven by an external magnet, and promoted by the chimney action of the furnace. The gas passed up through the furnace, down into the crucible where it came in contact with the alloy, passed rapidly up through a narrow tube and out of the hot zone. After equilibrium was established between the gas and the condensed phase, the composition of the gas mixture was determined from its density. In its circulation, the gas mixture passed through a chamber (lower right on Fig 1) containing a buoyancy-balance, where the density of the gas was determined by magnetic balancing. From the measured density,

Jan 1, 1950

The Committee on Nominations begs to submit the following names as its nominees for the respective offices indicated: For President, SIDNEY J. JENNINGS, New York. For Vice-Presidents, WALTER H. ALDRIDGE, New York; MARK L. REQUA, San Francisco. For Directors, J. E. JOHNSON, JR., New York; ALLEN H. ROGERS, Boston; HOWARD N. EAVENSON, West Virginia; ROBERT M. RAYMOND New York; WILLET G. MILLER, Canada.

Jan 12, 1916

By James Terry Duce

The gross production on the Island of Sahreirl during 1944 was approximately 6,700,000 U. S. bbl. No additional wells were drilled in the field during the year, but a number that were plugged off during the critical days of the war were brought back on production. This work is continuing. The construction of the extension of the refining plant was continued during the year and the new crude still was started in November. In Arabia, the production for the year 1940 was 5,074,838 U. S. bbl. Four wells were completed in Dammam field and all were commercial producers. Production for 1941 was 4,310,110 U. S. bbl. Seven more commercial producing wells were completed in Dammam field, and Well No. I at Abqaiq was complcted at 6180 ft. and was also a commercial producer. In 1942 production was 4,530,492 U. S. bbl. Abqaiq No. 2 was drilled to 5785 ft. but was left standing because of mechanical difficulty. The 1943 production was 4,868,- 184 with one well drilled, Abqaiq No. 3 completed at 6488 ft. and a commercial producer. Total production in Arabia for the year 1944 was around 7,800,000 U. S. bbl. and at the close of the year was running at approximately 40,000 bbl. per day. The small refinery, built in 1939, at Ras Tanura was in operation in the fall and a new refinery is being constructed. Only three wells were completed during the year—the El Jauf well in Northern Arabia (completed at 10,974 ft.) which did not bring in commercial production and Wells No. 4 (completed at 6270 ft.) and No. 5 at Abqaiq (completed at 6751 ft.), which were brought in as substantial commercial producers. Production for the year was entirely from the Dammam field. In this field, some of the wells that had been plugged off early in the war were brought back in production and this work is continuing. At the close of the year, one well was drilling in the Abqaiq field and an additional well was drilling at Qatif, the latter being a wildcat. Neither of the wells in question had reached producing horizons on the first of January.

Jan 1, 1945

By D. Turnbull, J. H. Hollomon, J. C. Fisher

The concepts of nucleation and of growth have adequately described the isothermal phase transformations to which they have been applied.ls2 However, these concepts have not yet been used successfully to describe the kinetics of a number of transformations that are not observed to take place isothermally. A typical reaction of this type is the austenite to martensite transformation in steels, for which the new phase appears only during cooling of the parent phase. If the cooling is interrupted, transformation ceases; yet had the cooling continued, transformation would also have continued. Nuclei of a new phase do not leap into existence all at once by the simultaneous cooperation of a large number of atoms or molecules of the parent phase; rather they are formed at finite rates by gaining or losing atoms one at a time from the surrounding materiaL3,4 Further thermo-dynamic considerations require a finite concentration of small transitory nuclei of all unstable phases to exist at equilibrium in a stable phase.= For steel in particular, nuclei of ferrite (a iron) exist at equilibrium in austenite (y iron) at temperatures where austenite is the stable phase. If a high-temperature phase a be cooled sufficiently rapidly from temperature TI above the a-ß equilibrium temperature To, to temperature T-1 below To where ß is the stable phase, the equilibrium distribution of ß nuclei corresponding to the high temperature will be retained. There are two limiting possibilities of particular interest: I. The steady state rate of nucleation of ß may be appreciable at T_1, and may require a concentration of sub-critical nuclei exceeding that retained from the high temperature. Time will be required then for the concentration of nuclei to build up to the steady state value, and an induction period will be observed during which the rate of nucleation will increase to the steady state value. 2. The steady state rate of nucleation of ß may be negligible at T-l, while the critical size for continuous growth of ß nuclei, which decreases with increased subcooling of the a phase, may reach a value so small that some. of the retained high-temperature nu-

Jan 1, 1949

By Rossiter W. Raymond

(Read at the Amenia Meeting, October, 1877.) IN the case of The Eureka Consolidated Mining Company v. The Richmond Mining Company of Nevada, recently tried at San Francisco, California, the real defendant was the Richmond Consolidated Mining Company, of London; but this being a foreign corporation, holds its mining property in Nevada through the Nevada corporation of similar name, in which the London Company owns all the stock, except the few shares necessary to "qualify" the American directors. The trial would naturally have taken place in the Circuit Court at Carson City, Nevada, and before a jury. But by stipulation of the parties, the case was tried in San Francisco, before Hon. Stephen J. Field, Justice of the Supreme Court of the United States, Hon. Lorenzo Sawyer, United States Circuit Judge of the Ninth Circuit, and Hon. E. W. Hillyer, United States District Judge, for the District of Nevada. The hearing began July 23d, 1877. The witnesses occupied two weeks, and the argument of. counsel three days. Very eminent lawyers were. engaged on both sides ; for the plaintiff, Messrs. Solomon Heydenfeldt, R. S. Mesick, John Garber, and H. J. Thornton ; for the defendant, Messrs. S. M. Wilson, Thomas Wren, and J. J. Williams. The court held the case under advisement until August 22d, when Mr. Justice Field delivered its unanimous opinion in favor of the plaintiff. The action was a complaint in ejectment, and an appeal was taken to the United States Supreme Court. The questions at issue between the Eureka and the Richmond Company in this suit, comprised several points in the construction of the mining law of the United States, and its relation to the customs and regulations of the mining districts, which possess an importance and an applicability far beyond the limits of the case in which they arose. It is my purpose to state these points, the arguments

Jan 1, 1878

By L. B. Slichter

It has been estimated that rock exposures in most mining districts aggregate less than 1 per cent. of the total surface area.1 Conclusions concerning the hidden 99 per cent. necessarily have been based on knowledge of only a small fraction of the surface, and from this limited information the geologist has been obliged to deduce the approximate and general nature of the underlying formations. In the search for ore it is necessary to supplement this general picture with greater detail. Fairly accurate knowledge of relatively small zones is required. This knowledge is carefully sought in many different ways—detailed interpretations of geological history, the tracing of float, the use of test pits, of trenching, of drilling, and of other methods. Practical ingenuity, scientific brilliance, great perseverance and patience, and the expenditure of large sums of money have all been a part of this search. The problem of exploring beneath cover with economy, and of obtaining essential information which this cover hides, is obviously a difficult one. It is also a very important one, for geologist's inform us that already the story of the 1 per cent. exposed outcrops has been largely read.V here remains the nearly virgin field comprised in the hidden 99 per cent.: and the importance of this zone is bound to increase continually. In recent years, the problems connected with the exploration of this "99 per cent. zone" have attracted a constantly enlarging group of investigators and at present greater efforts than ever before are being made to resolve them. This work, in it's various special aspects, has enlisted, beside geologists, the cooperative efforts of chemists, physicists, and mathematicians. The progress made in this development should be kept before those directing explorations in order that due advantage may be taken of a changing situation. My subject concerns certain aspects of one of the older physical methods of exploration, the magnetic method. This method is familiar in principle to most of us, arid because of its age., is especially suitable for

Jan 1, 1929

By Douglas Bunting

THE first presentation of this paper was before the Pennsylvania Anthracite Section of the Institute in May, 1914, after which a committee was selected to verify and add to the data contained in the original paper. The author is indebted to G. W. Engel, H. W. Montz, R. V. Norris, and H. H. Otto, of this committee, for additional information. I also wish to acknowledge the courtesies extended me by a number of the mining companies for information relative to accidents, systems of proving, and mining practice. The paper should bring forth additional criticism and recommendations, which will be of value in establishing future practice relative to this subject. Throughout the northern anthracite field of Pennsylvania glacial and alluvial deposits of sand, gravel, and clay exist in varying quantities. The extent and character of these deposits are described by N. H. Darton in Bulletin 45 of the U. S. Bureau of Mines, entitled, Sand Available for Filling Mine Workings in the Northern Anthracite Basin. It is estimated that the northern field contains 10,000,000,000 tons of these deposits, or a sufficient quantity to cover the 176 square miles of coal area to a depth of about 25 ft. These deposits of sand, etc., overlying the coal measures attain a maximum depth of more than 300 ft., and are usually saturated to such an extent as to render them semi-fluid. It is .this condition of fluidity that limits the mining of coal seams cropping in or in close proximity to these deposits, and it is in the interest of safer and more efficient mining methods under these conditions that the study of this -subject is here presented. The dangers incident to mining under deep deposits of sand have long been realized by operators in the northern anthracite field, and much has been done to prove the contour of the rock and vein croppings underlying these water-bearing deposits of sand and gravel.

Jan 1, 1915

By E. C. Rudolphy, M. E. Potter, J. R. Mitchell

The effects of 0.006 to 0.20 pet Sn ml the hot workability and the annealed mechanical properties were investigated for Types 302, 410, and 430 stainless steel. The hot workability of these steels was not significantly affected by their tin content within the range studied, although some effects on mechanical properties were noted. Apart from the effect of tin, optimum hot-working temperatures and V-notch Charpy impact transition temperatures for these grades were determined. HIGH tin residuals in some heats of stainless steel have been blamed for the poor hot workability, particularly during secondary mill rolling. However, very little quantitative information has been available. Previous work1"6 with carbon steels indicates that tin increases tensile strength and hardness but de- creases tensile and impact ductility. Halley,7 in reviewing the sources and effects of residual elements in carbon and alloy steels, concluded that much of the surface checking (hot shortness) encountered in rolling was caused by copper, and that tin, arsenic, and antimony combined with copper to form low-melting constituents which further increase the steel's sensitivity to hot shortness. These elements had little effect in the absence of copper. A more recent paper by Langenberg and Johnson8 concluded that tin reduces hot workability but that researchers disagree concerning the amounts which will cause trouble. They state that laboratory investigations with small ingots seem to indicate a higher tolerable level of tin than do statistical studies of mill data, and also that statistical analysis of mill data indicate that small amounts of residual tin are detrimental to the surface quality of stainless sheet. The accumulative increase in the general level of tin and other tramp elements in steelmaking materials will present greater problems to steelmakers in the future. The purpose of the present study was to obtain quantitative information on the specific effects of tin on the hot workability and mechanical properties of such common stainless steels as Types 302, 410, and 430.

Jan 1, 1962

By H. W. Highriter

THE method developed and used in this laboratory for the production of metallic uranium of such purity that it is ductile and can be cold-worked to fine wire or thin sheet by rolling has already been described1. It consists, briefly, in the electrolysis of potassium uranous fluoride (KUF5) in a molten bath composed of equal parts of sodium and calcium chlorides. The bath is contained in a graphite crucible, electrically heated to about 775° C., the crucible serving as the anode for electrolysis. The uranium deposits in finely divided form mixed with salts upon a molybdenum cathode suspended axially in the crucible. Upon com-pletion of the electrolysis the cathode is removed and cooled, the deposit broken and leached to remove salts. The metal powder is washed with water and dilute acetic acid and dried in vacuo to reduce oxidation. Suitable amounts are then pressed into pellets and heated in vacuo by high-frequency induction, using a thoria crucible. The uranium melts and flows away from the pellet, leaving a shell, which is largely oxide. In general, this method produced a satisfactory metal, although at times the uranium was not ductile. The investigations recorded here were made to find the cause of this embrittlement. It was known that the metal generally contained carbon, derived from disintegration of the graphite crucible in which electrolysis is conducted, in amounts dependent upon the thoroughness of washing the metal powder. Accordingly, analyses of several samples, both ductile and brittle, were made by combustion and absorption of C02 in Ascarite, using air instead of oxygen to reduce the temperature and rate of oxida-tion. Several of these metals were made with special precautions to reduce carbon content. The results show no relationship between ductility and carbon content in the range investigated (Table 1).

Jan 1, 1935

By G. M. Schwartz, G. A. Thiel

THE first record of the quarrying of dimension stone in Minnesota dates back to 1820 when limestone was quarried locally for part of old Fort Snelling. Limestone quarries were operated at Stillwater, Mankato, and Winona as early as 1854. Granite was quarried first at St. Cloud in 1868, and within a few years thousands of tons were shipped to widespread points. Rough dimension stone for large buildings furnished the first important market, but beginning in 1886 paving blocks were in demand. The largest shipment was in 1888, when 1925 cars were shipped from the St. Cloud area. Quartzite was quarried first at New Ulm in 1859 and somewhat later at Pipestone and elsewhere in southwestern Minnesota: The productive dolomite quarries at Kasota were opened first in 1868 and have continued as large producers of a variety of stone to the present time. At present, the industry is controlled by relatively few operators, and for that reason detailed figures on dimension stone are not released for publication. A general idea may be obtained from the data in the Minerals Yearbook for 1948. The figures for total stone produced in Minnesota are 1,804,000 tons valued at $5,090,652. Probably the largest item in the latter figure is received from dimension stone. A better idea of the situation, in relation to the country as a whole may be gained by using the data for 1930 when more companies were operating in Minnesota, and complete figures were published. In that year Minnesota produced granite valued at $2,668,119 and ranked third among the states in value. Minnesota's production of granite was almost exclusively for dimension stone. In the same year Minnesota produced 300,000 tons of limestone (dolomite) valued at $840,860, and this likewise was mainly dimension stone. In finished limestone Minnesota ranked second among the states in 1930. Sandstone and minor amounts of quartzite are the only other dimension stones that have been produced in Minnesota, but the quarries are now inactive. The commercial stones of Minnesota have been described in two reports by Bowled and by Thiel and Dutton.2 The early history of quarrying in Minnesota and extensive notes on the various rocks are given by N. H. Winchell.3 Small limestone and dolomite quarries were numerous throughout the area of Paleozoic rocks in southeastern Minnesota. Early production was largely dimension stone. With the increased use of Portland cement, most of these ceased production, and today only those at Kasota and Winona remain in operation. In recent years many quarries have reopened and new ones started, but these are devoted to the production of crushed rock and agricultural lime. As the application of modern quarrying and finishing methods increased, small companies in the granite business have dropped out, and the remaining companies have modernized their plants, purchased old quarries, and opened up new ones, thus furnishing a wide variety of granites suitable for most of the customary uses. It is the purpose of this review to present notes on' the geology and operations of each of the quarries now operating within the state. Granites and Related Igneous Rocks The term granite as used in this report includes granites, gneisses, diorites, gabbros, and other igneous rocks. The granites of greatest economic importance are found in three widely separated regions, see Fig. 1. 1-Central Minnesota in the region of the city of St. Cloud, 2-the upper Minnesota River valley region, 3-the northeastern portion of the state, commonly referred to as the Arrowhead region. The St. Cloud Region: The rocks of the St. Cloud region are mainly granites and related rock types such as monzonites and quartz diorites. The stones may be grouped into three major types, namely, pink granite, red granite and gray granite. Most of the pink granite occurs in the area to the southwest of St. Cloud. The rock is best described as stone with large pink crystals set in a finer grained black and white background. The minerals of the matrix occur in remarkably uniform sizes, and the pink crystals are sufficiently uniform in. their dis-

Jan 1, 1952

By M. H. Sommer

MANY attempts have been made to develop a relation between the tensile properties and the deep-stamping qualities of metals com-monly used in deep drawing. These operations are generally performed cold and the metal is always stressed beyond the elastic limit. However, the problem cannot be readily solved without a proper investigation of (1) the relation between actual stress and actual strain in the plastic range and (2) the stresses that are set up in the metal during the process of deep stamping. Much work has been done in recent years to add to our knowledge on plastic deformation of metals and the shortcomings of the ordinary tensile test, particularly in the plastic range, have been sufficiently recognized. It has been widely acknowledged that the local contraction, which appears in a tensile test after the maximum load is reached, is not a general characteristic of the material but is peculiar to this form of testing. The plastic deformation of materials is explained by the slip of their crystals along certain planes and this rearrangement should be similar whether observed in a tensile, compression or torsion test, and if the results of any of these forms of testing show deviations, it must be due to other influences, as for example the local contraction in a tensile test. For this reason the tensile-test curve as obtained from the measurements taken on a tensile-test machine or registered by an autographic device has been supplemented by the so-called "actual stress-strain curve," which is constructed from the observed tensile-test data by eliminating the effect of local contraction and is in complete alignment with the stress-strain values obtained in a compression or torsion test. The actual stress-strain curve shows the increase of actual unit stress in relation to unit elongation beyond the yield point and

Jan 1, 1934

By Hannon, J. W. G.

Silicosis is today's most important industrial disease and probably dates back to the Stone Age. Since the industrial revolution, increasing attention has been paid to those occupations where mineral dust is present in the air breathed by the workers. For many years it was assumed that the inhalation of all mineral dusts was hazardous. but investigations conducted in several countries pointed the statistical finger of guilt at free silica in any of its numerous physical forms as a dust of outstanding toxicity. Recognition of silica as the chief hazard has resulted in widespread use of the term "silicosis." Depending upon the concentration of finely divided silica dust to which the individual is exposed and the duration of exposure, silicosis may become a disabling condition in from one to thirty years. The structure of the lung and respiratory passages is such that only minute particles of silica can gain entry to the air cells in the lung (5 microns or under are most toxic). When these minute particles gain entry to the lung tissues they stimulate certain protective cells in the lung to multiply at an excessive rate. The cell's undergo inflammatory changes which result in nodular scars and a low-grade inflammation of the lung tissue. These progressive changes in the lung structure gradually encroach

Jan 1, 1949

By Jose J. Alvarez

INTRODUCTION Three major plant processes control the operation of an uranium in-situ mining plant. The three pro- cesses can be categorized under the headings termed - loading, elution, and precipitation. All other plant processes can be subcategorized under the three. In summary, the major plant processes in an in- situ mining plant are: 1. Loading - The pregnant lixiviant from the production wells flows through anion exchange resin. The loading of the uranium on the resin is controlled by various factors, such as ionic strength, valence, functional groups, etc. 2. Elution - The uranium-loaded resin is eluted or regenerated by a high ionic strength solution. The effluent from this process is de- fined as the pregnant eluate. 3 . Precipitation - The pregnant eluate is chemically treated to attain the ideal conditions for the selective precipitation of uranium. Hydrogen peroxide is an ideal precipitating agent under URI conditions. This paper will focus on two of the major processes: Elution and Precipitation. For the most part this relatively young industry has grasped the theory of liquids in continuous flow for the operation of the plant processes. Likewise, URI initially operated the two processes of interest with the continuous flow concept. Through laboratory experiments, URI has abandoned the flow concept and operates the eluting and precipitating stages with the concept of "batch" processes, whereby only one container, filled to a specified liquid level, is chemically processed. In the proceeding sections, each of the two pro- cesses will be discussed in detail, from their original concept to the present operation. Only minor modifications were made to the existing circuits for the conversion with results revealing a greater level of efficiency. ELUTION The elution of the loaded anion exchange resin can be achieved by different high ionic strength solutions. The selection of constituents is dependent on both chemical and economic considerations (i .e., efficiency and operating/restoration factors). The regenerant presently used is a pH 9.5 solution containing 7.5% NaCl and a mixture of Na2C03/NaHC03. expressed as 2.5% NaHC03.

Jan 1, 1980

For the year ending February, 1917 PRESIDENT L. D. RICKETTS,1 NEW YORK, N. Y PAST PRESIDENTS BENJAMIN B. THAYER 1 NEW YORK, N. Y. WILLIAM L. SAUNDERS,2 . NEW YORK, N. Y. FIRST VICE-PRESIDENT SIDNEY J. JENNINGS,1 NEW YORK, N. Y. TREASURER GEORGE C. STONE,1 NEW YORK, N. Y. SECRETARY EMERITUS ROSSITER W. RAYMOND, NEW YORK, N. Y SECRETARY BRADLEY STOUGHTON NEW YORK, N. Y.

Jan 10, 1916

For the year ending February, 1917 PRESIDENT L. D. RICKETTS,1 NEW YORK, N. Y. PAST PRESIDENTS BENJAMIN B. THAYER,1 NEW YORK, N. Y. WILLIAM L. SAUNDERS,2 NEW YORK, N. Y. FIRST VICE-PRESIDENT SIDNEY J. JENNINGS 1 NEW YORK, N. Y. TREASURER GEORGE C. STONE,1 NEW YORK, N. Y. SECRETARY EMERITUS ROSSITER W. RAYMOND, NEW YORK, N. Y. SECRETARY BRADLEY STOUGHTON NEW YORK, N. Y.

Jan 3, 1916

For the year ending February, 1917 PRESIDENT L. D. RICKETTS,1 NEW YORK, N. Y. PAST PRESIDENTS BENJAMIN B. THAYER,1 NEW YORK, N. Y. WILLIAM L. SAUNDERS,2 NEW YORK, N. Y. FIRST VICE-PRESIDENT SIDNEY J. JENNINGS,1 NEW YORK, N. Y. TREASURER GEORGE C. STONE,1 NEW YORK, N. Y. SECRETARY EMERITUS ROSSITER W. RAYMOND, NEW YORK, N. Y. SECRETARY BRADLEY STOUGHTON, NEW, YORK, N. Y.

Jan 7, 1916

For the year ending February, 1917 PRESIDENT L. D. RICKETTS,1 NEW YORK, N. Y. PAST PRESIDENTS BENJAMIN B. THAYER,1 NEW YORK, N. Y. WILLIAM L. SAUNDERS,2 NEW YORK, N. Y FIRST VICE-PRESIDENT SIDNEY J. JENNINGS,1 NEW YORK, N. Y. TREASURER GEORGE C. STONE,1 NEW YORK, N. Y. SECRETARY EMERITUS ROSSITER W. RAYMOND, NEW YORK, N. Y SECRETARY BRADLEY STOUGHTON, NEW YORK, N. Y.

Jan 12, 1916

By O. D. Sherby, J. E. Dorn

For elevated temperature-constant load creep tests of a solid solution alloys, the creep strain is a function of a temperature-compensated time parameter 0 = je H/RT dt. The activation energy H is equal to o constant of about 36,000 cal per mol. The substructures resulting from a given creep stress condition are functions of the creep strain independent of temperature. Each new creep stress gives a new unique set of grain substructures; this is one of the factors responsible for the failure of the mechanical equation of state for creep. IN this report an attempt is made to correlate the creep properties of dilute a: solid solutions in aluminum with the subgrain structures that are developed during creep. The possibilities of such correlations have already been suggested by Wood et al. and others1-" who demonstrated that the subgrain structures are functions of the creep stress, creep strain, rate of creep, and temperature. Investigations by Sherby and Dorn' have shown that the creep strain, E, at constant load for dilute a solid solutions of aluminum is given by the functional relationship: e = f(8,u,) [1] where: 0 equals te-AH/RT = temperature-compensated time; t, time; AH, activation energy, - 35,800 cal per mol; R, gas constant; T, absolute temperature, above 400°K; and u,, initial creep stress. Consequently, it was anticipated that the subgrain structure that develops during a constant load creep test should also correlate with any two of the three significant variables C, 8, and Another possible correlation between the subgrain structure and the creep variables is obtained by differentiating Eq. 1 with respect to time, whence the creep rate, 2, becomes: = (2L) (2) =f (, u,) e-AHRT [2] or: e = F (c e H/RT, 0) [3] For the minimum creep rate, ;,, 8 is solely a function of U, as revealed by Eq. 1. Consequently, at the minimum creep rate Eq. 3 reduces to: = F (eAH/RT) [41 Correlations between U, and i, eAH/RT were found valid for solid solution alloys of aluminum where AH was a constant of about 35,800 cal per mol. The parameter ;, eH/RT is identical to the Zener-Hollo-mon parameter8," used by them in evaluating the tensile properties of copper and other metals. Eq. 4 suggests that the subgrain structure developed during secondary creep might be correlatable with either of the two variables 2, e H/RT or u,. Some of the solid solution aluminum alloys which were discussed in an earlier report' were also used in the present investigation. Sheets of these alloys were homogenized, cold rolled from 0.100 to 0.070 in. in thickness and then recrystallized to about the same grain size. Their chemical composition and grain size are recorded in Table I. Creep specimens were selected with their tensile axes in the rolling direction. The details for creep testing have been described10 and will not be repeated here. All creep tests were performed under constant load conditions. Experimental Results and Discussion Metallographic Structure of Creep Specimens: In order to obtain a preliminary concept of creep on the metallographic structure of high purity aluminum, the various ruptured specimens previously used to obtain the creep data for pure aluminum were polished and etched electrolytically in a dilute solution of fluoroboric acid. Oblique illumination was used to reveal the substructures which, for convenience, are shown in correlation with the vs. ;, eH/RT curve in Fig. 1. It is necessary to emphasize that the data for the curve refer to the various secondary stages of creep whereas the micrographs refer to the fractured creep specimens. Nevertheless a regular and systematic correlation is observed between E, eAH/RT (or the creep stress) and the micro-structure at fracture. For In (e, eAH/RT) = 42.3, which refers to creep at a high creep rate and a low creep temperature, the fractured aluminum specimen, as shown by the micrograph in the upper right-hand corner of Fig. 1, exhibited extensive deforma-

Jan 1, 1954

By L. Delisle

This work represents the first step of an attempt to test the applicability of the electron microscope to the study of subgrain structures in copper. Observations on annealed and deformed single crystals and polycrystalline samples of copper are described. IN the course of study of the structure of fine tungsten wires and tungsten rods with the electron microscope, well defined subgrain structures were observed. The size, size distribution, and orientation uniformity of the etch figures varied widely in different samples. Figs. 1 and 2, electron micrographs of a tungsten wire and of a tungsten rod, respectively, are illustrations of the difference in size and size distribution of the etch figures in different samples of the same metal. The observed differences, as pointed out in a previous paper,' appeared to be related to the heat and mechanical treatments of the samples. They were also consistent with the results reported in the literature on the mosaic structure of metals.' For that reason a program of research was initiated in an effort to obtain more systematic evidence of the possible relation of heat and mechanical treatments to the subgrain structure of metals as observed in the electron microscope. The purpose of this paper is to present observations made on the effect of cold work on the subgrain structure of copper. Procedure Starting Materials: Copper was the metal studied because it can be obtained in a high degree of purity, much information is available in the literature on its properties and its response to cold work and heat treatment, it shows no allotropic change, and it is sufficiently hard to be handled without great difficulty. Two groups of specimens were used: 1—single crystals cast from spectroscopically pure copper and 2—polycrystalline samples of oxygen-free high conductivity copper. Single crystals were studied because it was hoped that the elimination of a number of variables, such as grain boundaries, orientation differences, degree of purity, would simplify the problem and perhaps permit a better understanding of the phenomena that would be observed. The polycrystalline samples were designed to give a general picture of the changes considered. The single crystals were made of copper which analyzed spectroscopically to better than 99.999 pct Cu. They were cast in vacuum, by the Bridgman method, in crucibles made of graphite with a maximum ash content of 0.06 pct. The mold design is shown in Fig. 3. It permitted casting crystals of the size and shape required for the experiments, so that the danger of introducing cold work in the original samples by cutting or other machining would be eliminated. The polycrystalline samples were pieces, 3/4 in. long, cut from a rod of oxygen-free high conductivity copper, % in. in diameter. A flat surface, 1/4 in. wide, was milled along the rods, polished, and etched. The samples were then annealed in vacuum at 850°C for 1 hr. Polishing and Etching: Work previously done on tungsten,' polished mechanically and etched chemically," had shown that: 1—the general appearance of the etch figures of a given sample was not altered by repeated polishings and etchings under similar conditions; 2—variations in the time of etching and the concentration of the etchant changed the definition of the etch figures, but did not alter their general size nor orientation distribution within the limits of observation. Further work confirmed the reproducibility of the subgrain structures observed in, 1—single crystals and polycrystalline samples of copper when polishing and etching were repeated under similar conditions, and 2—specimens of tungsten and polycrystalline copper when electrolytic polishing and etching were substituted for mechanical polishing and chemical etching, respectively. On the strength of these observations, it was felt that, if conditions of polishing and etching were kept constant, changes observed in the subgrain structure of a sample upon deformation and annealing would be attributable to such treatments. For that reason the conditions of polishing and etching were kept as constant as possible. The single crystals were polished electrolytically in a bath of orthophosphoric acid in water, in the ratio of 1000 g of acid of density 1.75 g per cc to 1000 cc of solution, under a potential drop of 1.6 to 1.8 V. Electrolytic polishing was selected to prevent the formation of distorted metal in polishing. The same samples were etched by immersion in a 10 pct aque-

Jan 1, 1954

For the year ending February, 1917 PRESIDENT L. D. RICKETTS,1 NEW YORK, N. Y PAST PRESIDENTS BENJAMIN B. THAYER 1 NEW YORK, N. Y. WILLIAM L. SAUNDERS,2 NEW YORK, N. Y. FIRST VICE-PRESIDENT SIDNEY J. JENNINGS,1 NEW YORK, N. Y. TREASURER GEORGE C. STONE,1 NEW YORK, N. Y. SECRETARY EMERITUS ROSSITER W. RAYMOND, NEW YORK, N. Y SECRETARY BRADLEY STOUGHTON NEW YORK, N. Y.

Jan 10, 1916