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By E. A. Gulbransen, W. S. Wysong

THE behavior of tungsten and its surface oxides in oxidizing and reducing atmospheres and in high vacua at elevated temperatures is a question of considerable technical importance. The use of tungsten as a metal or as an important component in alloys in high temperature oxidizing atmospheres has been limited because of the unprotective nature of its oxide film and the volatility of its oxide. This paper will present results of a microbalance study1,2 of the following problems: (I) the oxidation behavior in the temperature range of 25 to 550°C (2) the reduction with pure hydrogen of thin oxide films formed on tungsten, and (3) the volatility of thin oxide films on tungsten. Tungsten is an interesting metal to study for the following reasons: (1) although the oxide to metal volume ratio is greater than one, the oxide is not considered protective, (2) the metal readily oxidizes at temperatures from 300° to 550°C (3) the oxides W02 and WO3 are reduced at temperatures as low as 500°C. by hydrogen, and (4) the oxide W02 is volatile at temperatures from 800 to 1100°C. LITERATURE The oxidation of tungsten in its thin film range has not been studied critically. In the thick film range Dunn3 has made the only systematic study. He found the oxidation rate to obey the parabolic rate law in the temperature range of 700 to 900°C. The temperature variation of the oxidation rate constant was found to follow an exponential law of the Arrhenius type. An inflection was noticed in the temperature plot of the rate law constant at 850 to 900°C. This was attributed to a phase change in the oxides. Scheil4 has studied the oxidation rate at 500 and 700°C over long periods of time and found a linear rate law. This result was interpreted as evidence for the presence of a nonprotective film. Pilling and Bedworth5 analyses of the oxide volume to metal volume ratio would indicate that a compact protective film should form. McAdam and Geil6 have studied the oxidation of tungsten in the thin film range using the interference color method. A parabolic rate law was found. Their curves showed that tungsten oxidizes faster than nickel but more slowly than iron. The lattice structures found in the oxidation of tungsten surfaces have been studied by Hickman and Gulbransen.7 They have reported that W03 is the stable oxide in contact with the metallic substrate up to approximately 600°C while W02 forms first at 700°C. Hägg and Magneli8 have recently reported a study of the lattice structures observed in the tungsten oxides using the X-ray diffraction method. In addition to an a-phase W03 and a d-phase W02, they reported the existence of two new phases. A ß' phase, homogeneous between

Jan 1, 1947

By R. E. Old

Through the use of pressure and production records, formation properties and bottom-hole sample data, the performance of an oil reservoir may be studied analytically to define and evaluate the natural forces acting on and within the reservoir. Use is made of material-halance methods and the equations for natural water encroachment. to estimate reserves. Methods for calculation of pressures are given. A study of the Jones sand, Schuler field, Arkansas, has been made and is given here to illustrate the value of the methods discussed. Introduction With the decreasing rate of discovery of new oil reserves, attention is necessarily focused on the efficient development, evaluation, and production of existing reserves. From the nation's viewpoint, the necessity of conserving resources is obvious. From the operator's viewpoint, the problem is to lengthen the period of profitable operation, in an attempt to increase the return on his investment. To do this the operator must take advantage of the natural forces acting on and within the reservoir. Natural water encroachment, the nemesis of profitable operation in the past, can be and is being harnessed to produce a greater oil recovery during the stage of flowing production. Proper evaluation of water encroachment rates and a fuller under- standing of reservoir behavior dictate the appropriate production procedures. Complacency in hit and miss production is obsolete. Oil production must and will approach the efficiency of other businesses, such as manufacturing. A manufacturer will not place an article on the market until he has fully investigated the processes involved, additional investment in equipment, costs of production, and expected profits. These may be modified by actual experience at a later date, but at least he begins with an idea of expected return. It is just as logical that an oil operator should investigate these same factors during the development and the early period of production of an oil reserve. The complexity of the problems existing in oil reservoirs should not be underestimated. Conversely, they should not be regarded as insoluble. Many completely defy solution, but there are others that can be solved completely or attacked intelligently to yield approximate results. The petroleum engineer has many tools, both figuratively and literally, at his disposal. Physical data such as core analyses, electrical logs, bottom-hole sample analyses, and bottom-hole pressures are accumulated extensively. Advances in the analytics of fluid flow have kept pace with the advances in measurement of physical data. It is the purpose of this paper to show how some of these records may be analyzed to define certain phases of reservoir behavior.

Jan 1, 1943

By R. E. Old

Through the use of pressure and production records, formation properties and bottom-hole sample data, the performance of an oil reservoir may be studied analytically to define and evaluate the natural forces acting on and within the reservoir. Use is made of material-halance methods and the equations for natural water encroachment. to estimate reserves. Methods for calculation of pressures are given. A study of the Jones sand, Schuler field, Arkansas, has been made and is given here to illustrate the value of the methods discussed. Introduction With the decreasing rate of discovery of new oil reserves, attention is necessarily focused on the efficient development, evaluation, and production of existing reserves. From the nation's viewpoint, the necessity of conserving resources is obvious. From the operator's viewpoint, the problem is to lengthen the period of profitable operation, in an attempt to increase the return on his investment. To do this the operator must take advantage of the natural forces acting on and within the reservoir. Natural water encroachment, the nemesis of profitable operation in the past, can be and is being harnessed to produce a greater oil recovery during the stage of flowing production. Proper evaluation of water encroachment rates and a fuller under- standing of reservoir behavior dictate the appropriate production procedures. Complacency in hit and miss production is obsolete. Oil production must and will approach the efficiency of other businesses, such as manufacturing. A manufacturer will not place an article on the market until he has fully investigated the processes involved, additional investment in equipment, costs of production, and expected profits. These may be modified by actual experience at a later date, but at least he begins with an idea of expected return. It is just as logical that an oil operator should investigate these same factors during the development and the early period of production of an oil reserve. The complexity of the problems existing in oil reservoirs should not be underestimated. Conversely, they should not be regarded as insoluble. Many completely defy solution, but there are others that can be solved completely or attacked intelligently to yield approximate results. The petroleum engineer has many tools, both figuratively and literally, at his disposal. Physical data such as core analyses, electrical logs, bottom-hole sample analyses, and bottom-hole pressures are accumulated extensively. Advances in the analytics of fluid flow have kept pace with the advances in measurement of physical data. It is the purpose of this paper to show how some of these records may be analyzed to define certain phases of reservoir behavior.

Jan 1, 1943

By ERIIL SCHROEDTER

THE death, on May 6, 1908, of Dr. Hermann Wedding, Privy Mining Councilor of the Kingdom of Prussia, and Professor of the Metallurgy of Iron and Steel at the Royal Mining Academy of Berlin, was a loss keenly felt by the whole metallurgical world. Not alone in his native land, but also in foreign countries did he enjoy an esteem of which the title of honorary membership in the American Institute of Mining Engineers, the United States Association of Charcoal Iron-Workers, and the (British) Iron and Steel Institute bears eloquent testimony. Hermann Wedding was born March 9, 1834, in Berlin. At the suggestion of Dr. C. J. B. Karsten, the veteran father of Prussian metallurgy and author of the first German text-book of the metallurgy of iron, lie turned his attention, after gradu¬ating from the gymnasium, to mining and metallurgy. In 1853, he began a practical course at the Malapane iron-works, in Upper Silesia. Subsequently, he studied at the Berlin Mining Academy, and received from the University in 1859 the degree of Doctor of Philosophy. A journey which be made to England, somewhat later, led to his undertaking a German translation, with revision and additions, of John Percy's classic treatise on the metallurgy of iron and steel, the publication of which, in successive installments, stretched through many years. In 1863, lie published, as a thesis in connection with his "Assessor's examination," an essay, entitled The Results of the Bessemer Process for the Production of Steel, and Its Prospects for the Rhenish and Westphalian Iron and Steel Industry, which revealed such ability and knowledge as to secure for him a call to the chair of metallurgy in the Berlin Mining Academy.

Jun 1, 1909

By J. P. Witherow

The Clapp and Griffiths steel-process may be considered a pneumatic system, similar to the Bessemer, with the difference that the converter is fixed or non-tilting, and that the blast is introduced around the lower section of the converter instead of through its bottom. Mr. Griffiths was engineer-in-chief of the Gilchrist & Thomas basic dephosphorizing process during all the time those gentlemen were experimenting and working up their system, as Mr. G. communicated to me. After separating from these gentlemen, he began developing the present Clapp and Griffiths type of converter. Dr. Clapp, of Nantyglow, Monmouthshire, was a prominent physician in a large iron district. Previous to his association with Mr. Griffiths, he took out some patents on a process of his own for the manufacture of steel, which patents stood in Mr. Griffiths' way; hence the consolidation. Early in the summer of 1883, my attention was called to the experiments of Messrs. Clapp & Griffiths in Great Britain by a friend who had just returned from England. Later in that summer I went to Newport, on the border of Wales, where I met Messrs. Clapp and Griffiths and their friends. After visiting two small converters of their type which were in operation at different works, and spending a few days in the iron-districts of Wales, I went to London, where I met my friend Henry W. Oliver, Jr., who had already heard of the new steel-process. We decided to revisit Wales and examine more fully the process, more especially that Mr. Oliver might have the opportunity of coming practically in contact with the men and die process himself, so that his judgment might not be influenced by my sanguine feelings. On

Jan 1, 1885

Denver, the Mile High, Queen City of the Plains, your host for AIME's 99th Annual Meeting has many exciting and picturesque places for you to visit during your stay. A host of restaurants cater to every taste; supper clubs and theaters provide nighttime entertainment; there are sports facilities and a plethora of shops for the ladies. When it comes to dining out, there are many excellent restaurants within walking distance of the Denver Hilton --among them, three in Brooks Towers: the Gitana, the Boston Half Shell serving the finest seafood, and Marvelous Mary's. In the Larimer Square area there in the Bratskellar with a true Germanic atmosphere and Sperte's Laffite offering a typical New Orleans setting.

Jan 1, 1970

By George W. Maynard

For an account of the discovery and the determination of chromite on Port au Port Bay I am indebted to Mr. Obalski, Government mining engineer for the Province of Quebec. He writes: " In June, 1894, with the authorization of our Government, I went to Newfoundland to examine some asbestos property. Passing through Halifax, I had interviews with some gentlemen who told me that besides the asbestos there was in the same district a big deposit of iron-ore. They handed me some specimens, and, after ascertaining that they were not magnetic, and learning that they were found in serpentine, I said they were chromic iron. I visited the place on June 27, 1894, and confirmed my opinion, pointing out at the same time the importance of the deposit, as appears in my report of July 9, 1894. I do not claim any credit for the discovery of chrome-ore in Newfoundland; but, as a matter of fact. when I came in contact with the Halifax gentlemen they did not appear to know the nature or the value of the mineral until I mentioned to them that it was chromite. "' Mr. Obalski's report was mainly devoted to the asbestos-deposits. That portion relating to the chromite was as follows: " On the right side of the creek there is a show of chromic iron of good quality, which appears scattered through the serpentine in several places on the face of the cliff for 40 to 50 feet. A few boulders are found farther up at a distance of 100 feet, and also in the ckeek itself. From this point the deposit exists on a relatively large area, the widest exposures being from 6 to 7 feet. Chromic iron deposits in serpentine rock have no regularity, and are merely pockets. In the case of the property in question this rule is not changed, but the pockets look to be of large extent, and could be easily worked." My own preliminary investigation of the property was made

Jan 1, 1898

By James Douglas

I had the good fortune to visit the Stockholm Exposition just before its close in October last, and to get a glimpse of the methods used in Sweden in making the wonderful steel and iron for which its furnaces are so famous. My time and opportunities for observation were limited, but some points which I noted may be worth bringing to the notice of the Institute. The Exposition itself was confined to the natural and artificial products of Scanclinavia, and therefore iron and steel held a very prominent place in it. There was a complete collection of the rocks and ores of the Peninsula made by the Geological Survey; and every iron-mine of note exhibited a glass model of its workings, as well as classified specimens, accompaniecl by thorough analyses of the ores. Another feature of interest was the display of models of the old mining-machinery, in the invention and introduction of which Sweden led the way, and of the old and new surveying-instruments and compasses devised for the exploration of the Swedish iron-ore bodies, all of which are more or less magnetic. The magnetometric collection and exhibit of methods of operation made by Prof. Nordestrijm were supremely instructive. The larger metallurgical works, such as those of the Kopparberg and Sandvik companies, exhibited their wares in separate pavilions, in which crude and manufactured objects were arranged most eflectively and tastefully; while the smaller companies erected in the Industrial Arts Building trophies, every one of which was an object of beauty. One was struck on all sides by the fine asthetic feeling exhibited in the ingenious installation of materials and objects not easily lending themselves to artistic treatment. Hammers, picks and drill-steel were grouped into mural designs which it was a delight to look at.

Jan 1, 1899

By John Dilworth

THE word "development," as used in connection with .mining, is a rather general term and in most instances must be qualified or explained before the exact thought in the mind of the user is made clear. For instance, by the development of a mining district is often meant its entire facilities of mineral production, such as railroads, towns, mine plants, etc. In speaking of the development of a property its prospecting by test pits or diamond drill borings may be referred to; or it may be the mines, strip pits or quarries from which the coal, ore or rock is won. But, as a rule, when the development of an individual mine is spoken of the idea in mind is the system of underground workings by means of which the mineral is recovered and transported to the surface. It is this character f development that is considered in this paper. The discussion will be confined to the ordinary room-and-pillar, system of mining. practically horizontal coal seams that is used in most bituminous coal mines in this country, and to only two phases of this subject; viz., what is properly included under the head of "Development"' as it appears on the books of a coal company or the inventories of an examining engineer, and how its "value" should be determined -by the accountant or engineer. No absolute rule or definite agreement covers these points, yet these questions are far more than academic. Development is often an important part of a mining company's assets, affecting the amount of its invested capital (and hence its rate of taxation under present Federal income tax laws) as well as the value of its total assets and the amounts chargeable to cost of coal and to depreciation.

Jan 7, 1921

By B. M. Larsen, T. E. Brower

A perspective is presented of the steel plant sulphur distribution and elimination problem from coal to liquid steel ready for teeming, giving distributions of sulphur over a range of coke sulphur content, and some methods of sulphur control, in the blast furnace, external desulphuriza-tion between blast furnace and open hearth, distribution between fuel, slag, and metal, and methods and limitations of control of sulphur in the open hearth furnace. AS a part of the 1951 AIME symposium on sulphur in steelmaking, it was thought that a discussion of the distribution of sulphur throughout the whole series of operations, from coal and ore to finished steel ingots, might have some value in giving a perspective on the whole problem. The following discussion is an attempt to present such an overall picture. The order is that of the actual plant operations, beginning with a very brief consideration of the coking process. Sulphur in Coal and Coke Since by far the largest source of sulphur entering the steelmaking cycle is in the coal used to make coke for the blast furnace, it would seem reasonable to eliminate some of it, either from the coal, or the coke, or during the coking process. This has appeared impracticable up to the present, at least, for two main reasons: the low activity of the organic sulphur in either coal or coke, and because of price limitations involved in treating a low cost material such as coke. A variable portion, usually M or less, of the sulphur is present in coal in the form of pyrites or similar compounds, and a large part of this sulphur may be removed in the coal washery. Most of the sulphur, however, is normally present as "organic" sulphur, intimately associated with the coal structure. Its distribution prevents any separation by mechanical means. Its low activity makes improbable ' any rapid chemical removal, although hydrogen will remove sulphur from both coal and coke. Thus, prolonged recirculation of coke oven gas in the coking process would tend to leave a smaller percentage of the total sulphur in the coke residue. Table I shows a typical distribution of sulphur from coal into products in the coking process. As the sulphur in the coal increases, the sulphur in the coke tends to increase in about the same proportion. Sulphur in the Blast Furnace The best picture of the situation in the blast furnace is provided by a sulphur balance of raw materials entering, and of products leaving, the furnace. The difficulties in accurate weighing and sampling of the variable solid materials entering this process, and the number of hours required for the raw materials to descend through the furnace under variable operating conditions, make it difficult to obtain an accurate balance. However, balances made over periods of weeks or months tend to average out some of these uncertainties. Table I1 presents three typical sulphur balances similar to a number that the writers have calculated. In most of these the slag volume calculated from the sulphur balance is, in some instances more, and in other instances less, than the value corresponding to the best input and output balances of the other slag constituents (lime, silica, alumina, etc.). Probably the greatest source of error in these calculations is the sulphur content of the slag. Despite some possible inaccuracies the balances of Table II show rather definitely the following points: 1—That 87 to 95 pct of the total sulphur input is in the coke and 95 to 97 pct of the total sulphur output is in the slag. Also, that if any sulphur leaves the furnace with the gas it is relatively small, amounting to a possible 1 pct or less. 2—At the lower sulphur coke level of 0.86 pct the total amount of sulphur charged is 15 Ib of sulphur per ton iron increasing to 26 lb per ton at the higher sulphur, intimately associated with the coal struc-rare burdens containing sulphur-rich ores will the total sulphur burden fail to be nearly proportional to the content in the coke used. 3—The 7 to 9 pct of the total sulphur input from the limestone of furnaces B and C is due to the relatively high sulphur content of the stone, 0.226 and 0.265 pct, respectively. In the case of furnace A, the sulphur content of the limestone was only 0.06 pct which resulted in only 3 pct of the total sulphur input coming from this source. It is rather interesting to compare the sulphur balances of a typical ferromanganese furnace with

Jan 1, 1952

The paper relates to the laboratory and pilot plant studies that have been carried out by Sherritt Gordon Mines Ltd., Metallurgical Research Div., in developing the ammonia pressure leach process for extracting Cu, Ni, Co, and S from high grade Ni concentrate produced from Lynn Lake ores and describes in some detail the chemistry of the process. In the leaching stage air, ammonia, and sulphide minerals react in a sequence of inter-related steps to produce soluble amines of Ni, Cu, and Co in a solution containing sulphate, thiosulphate, polythionate, and sulphamate ions and a controlled amount of free ammonia, the iron and other components of the concentrate remaining as an insoluble residue which is separated from the leach solution by filtration. The pregnant solution produced in leaching is further treated by boiling to precipitate and remove Cu as cuprous sulphide, leaving a copper-free solution with a composition suitable for subsequent precipitation of Ni and Cu by H,

Jan 3, 1955

By Donald K. Weaver

THERE have been eight different oil zones identified and produced at Santa Fe Springs, of which three or four are in turn divided into two or three parts. These zones are, from top to bottom, the Foix, difference of opinion over this nomenclature, with reference to the different zones referred to as Clark, it has no particular bearing on the water problems. Each of these oil zones has had waters of varying salinity associated with it, either within or at the bottom of the 'zone. Table 1 is a tabulation of the zones, their maximum thicknesses, salinity and heads of various waters. Surface waters are fresh, and of high head, giving artesian flow in some instances.

Jan 1, 1930

By B. S. Butler, H. D. McCaskey

The New London copper mine, about 8 1/2 miles east of Frederick, Md., was visited by the writers for a few hours in the spring of 1909 and the following brief notes on ore specimens collected are presented as a contribution to studies in chalcocite ores. For certain data on the structural and areal geology of this portion of Maryland the writers are under obligation to the unpublished notes and maps of Arthur Keith. The detailed study of the ores is the work of B. S. Butler. The deposit here discussed has many similarities to those of the Virginia district of Virginia and North Carolina, which have been described by Gratonl and Laney,2 except that in the deposits of the New London mine chalcocite is by far the most important ore mineral, while in the Virginia deposits bornite is commonly the most important sulphide. In the New London occurrence calcite is the most important gangue mineral. Field relations The -town of Frederick lies in the center of a narrow belt of limestone ranging in age from Ordovician on the east to Cambrian on the west. This belt is about + mile wide at Noland's Ferry, on the Potomac, and broadens to a width of 3 miles at Frederick. The general direction is east of north. The eastern boundary is, in places, a fault plane along which a series of metamorphic rocks of presumptive pre-Cambrian age have been thrust up. These ancient rocks, for several miles east and west of New London, are phyllites in the main, but closely inter-folded near the New London mine are long, narrow lenses of epidote

Jan 1, 1915

By Joseph J. Yancik

In Moscow, the delegation received a briefing on the Soviet coal industry from First Deputy Minister Vladimir Fedanov. A similar briefing was given to us on the Donets coal basin by Deputy Minister S. Saratikyanz of the Ukrainian Coal Ministry. Lengthy technical discussions were held with the mines staff and research personnel at the institutes we visited. In addition, we had detailed discussions with key staff members of two combinats; Donetskugol and Tulaugol. In all these meetings, principal topics were matters of safety related to hazards associated with face mechanization, coal transport, methane gas control measures, gas outbursts, coal and rock outbursts, fire fighting and control, explosion suppression and control measures, and other related hazard factors. There was also much discussion on miner training, miners' attitudes toward safety and accident prevention practices, and preparation and enforcement of safety rules and regulations. It would be helpful to briefly review Soviet coal production statistics for comparison purposes with the U.S., and for the purpose of referencing some of the delegation findings mentioned in this report. For an excellent, comprehensive picture of Soviet coal production and other related fuel statistics, the reader is referred to Strishkov's, et d. report.1 Strishkov's estimates agree with the numbers given us by Coal Ministry officials except in clean coal tonnage. The figures of 604 million mt of clean coal out of a total production of 655 tons raw coal in 1972 is much higher than Strishkov's estimate of 375 million mt clean coal.

Jan 7, 1974

By L. F. Mondolfo

An aluminum-copper 4 pct Cu alloy aged at room temperature for times increasing up to 78,000 hr was annealed at 170°C and the hardness and electrolytic potential determined during retrogression and subsequent aging. It was found that there is a change of behavior with increasing time of aging at room temperature which indicates that, given sufficient time, retrogression disappears and the room-temperature aging tends to progress directly into the high-temperature aging. WHEN an age-hardenable alloy is aged at low temperature after proper quench, changes of properties and structure take place. If this material is then heated to a temperature higher than the previous one, but still well below the solution-treatment temperature, the properties and structure changes produced by the low-temperature aging disappear and the material apparently reverts to the as-quenched condition, ready to undergo aging from the start. This phenomenon is termed reversion or retrogression. First discovered by Cayler3l it has been extensively investigated, as shown by the number of publications listed in the bibliography. From all the information available the following facts emerge: 1) All aeg hardenable alloys can be retrogressed.9 13, 19) 24, 33, 41, 42, 44, 47, 53, 54, 61, 63, 64, 66, 73, 78 2) All the properties changes that take place during aging at low temperature can be retrogressed to a smaller or larger extent.4,5,7,12,19,32,49,50,57,58,60,67,75,76 67, 75, 76 3) Retrogression requires that the temperature be well above the preliminary aging temperature. If the difference between the two temperatures is small, Little or no retrogression takes place.7,20,32,33,41,49 57. 65 4) The larger the difference between the preliminary aging and the retrogression temperature, the faster and more complete is the retrogression.20, 33, 41, 48, 65, 67 5) Retrogression can be produced several times in the same alloy.23, 35,41,57,59 6) The amount of retrogression that can be obtained depends on the aging temperature. Alloys aged at the lower temperatures can be retrogressed the most. The higher the preliminary aging temperature the less retrogression can be produced.20,25,33,37,44,49,54,58 7) Appreciable retrogression after aging at elevated temperatures is possible only if the preliminary aging has lasted a short time. After a certain time of aging at high temerature retrogression does not take place any more,:5,6,9,10,11,21,40,58 8) During retrogression the Guinier-Preston zones redissolve and disappear. The other precipitate

Jan 1, 1960

Texture Transition in Ordered CuAu, by E. A. Starke, Jr., J. C. Ogle, and C. J. Sparks, Jr., Trans. TMS-AIME, 1969, vol. 245, pp. 169-70. pole figures should have had two parts not one. On the Estimation of Oxygen Absorption by Continuous Molten Metal Streams, by J. Szekely, Trans. TMS-AIME, 1969, vol. 245, pp. 341-44.

Jan 1, 1970

By M. Metzger, J. C. Bilello

Microyielding in 99.999 pct Cu occuwed in two distinct parabolic microstages and was substantially indeoendent of grain size at the relatiz~ely large grain sizes stzcdied. The strain recouered on unloading was a significant fraction of the forward strain and was initially higher in a copper-coated single crystal than in poly crystals. Results were interpreted in terms of cooperative yielding and short-range dislocation motion activated otter a range of stresses, and a formalism was given for the first microstage. It was suggested that models involving long-range dislocation motion are more appropriate for impure or alloyed fcc metals. THERE are still many unanswered questions concerning the degree and origin of the grain size dependence of plastic properties. In the microstrain region, a theory of the stress-strain curve proposed by Brown and Lukens,' based on an exhaustion hardening model in which the grain boundaries limit the amount of slip per source, accounted for the variation with grain size of microyielding in iron, zinc, and copper.' This theory assumes N dislocation sources per unit volume whose activation stress varies only with grain orientation. Dislocations pile-up against grain boundaries until the back stress deactivates the source, which leads to a relationship between the axial stress and the strain in the microstrain region given by: where G is the shear modulus, D the grain diameter, a the flow stress, and a, is the stress required to activate a source in the most favorably oriented grain.3 If this or other grain-boundary pile-up models are correct, then the reverse strain on unloading would be much larger for a polycrystalline specimen than for a single crystal. Also, the microplasticity would become insensitive to grain size if this could be made larger than the mean dislocation glide path for a single crystal in the microregion. These questions are examined in the present work on polycrys-talline copper and a single crystal coated to provide a synthetic polycrystal. EXPERIMENTAL PROCEDURE Tensile specimens 3 mm sq were prepared from 99.999 pct Cu after a sequence of rolling and vacuum annealing treatments similar to those recommended by Cook and Richards4-6 to minimize preferred orientation. Grain size variation from 0.05 to 0.38 mm was obtained by a final anneal at temperatures from 310" to 700°C. Dislocation etching7 revealed pits on those few grains within 3 deg of (111). For all grain sizes dislocation densities could be estimated as -107 cm per cu cm with no prominent subboundaries. The single crystals, of the same cross section, were grown by the Bridgman technique with axes 8 deg from [Oll] and one face 2 deg from (111). An anneal at 1050°C produced dislocation densities of 2 x 106 cm per cu cm and subboundaries -1 mm apart in these single crystals. A Pb-Sn-Ag creep resistant solder was used to mount the specimens, with a 19 mm effective gage length, into aligned sleeve grips fitted to receive the strain gages. All specimens were chemically polished and rinsed8 to remove surface films just prior to testing. The synthetic polycrystal was made by electroplating a single crystal with 1 µ of polycrystalline copper from a cyanide bath. Mechanical testing was carried out on an Instron machine using two matched LVDT tranducers to measure specimen displacement, the temperature and the measuring circuit being sufficiently stable to yield a strain sensitivity of 5 x 107. At the crosshead speeds employed, plastic strain rates were, above strains of 10¯4, about 10¯5 per sec for polycrystalline specimens and 10-4 per sec for the single crystals. Plastic strain rates were an order of magnitude lower at strains near l0- '. A few checks at strain rates tenfold higher were made for reassurance that the initial yielding of polycrystalline copper was not strongly strain-rate dependent. Test procedures followed the general framework outlined by Roberts and Brown.9,10 An alignment preload of 8 g per sq mm for polycrystals, and 2 to 4 g per sq mm for single crystals, was used for all tests. These gave no detectable permanent strain within the sensitivity of the present experiments; although at these stress levels, small permanent strains are detectable in copper with methods of higher sensitivity.11 12 stress and strain data are reported in terms of axial components. RESULTS General. The initial yielding is shown in the stress vs strain data of Fig. 1. For polycrystals, cycle lc, the loading line bent over gradually without a well-defined proportional limit, and almost all of the plastic prestrain appeared as permanent strain at the end of the cycle. The unloading curve was accurately linear over most of its length with a distinct break indicating the onset of a significant nonelastic reverse strain at the stress o u, indicated by the arrows. The yielding in subsequent cycles, Id and le, had the same general character. The single crystal behavior, shown to a different scale at the right of Fig. 1, was different in that initially the nonlinear reverse strain was unexpectedly much greater than for polycrystals. It should be noted that these soft crystals had a small elastic

Jan 1, 1970

By Robert H. Richards

IT will hardly be worth while to spend time over the discovery of this mine, how lumps of galena, were picked up and brought to town, and how legends were told of an old mine from which Revolutionary bullets were made. This is an entirely new mine, with no evidences of former or ancient workings in its immediate vicinity to guide or attract the prospector. The first pit was opened in May, 1874. In August I made a visit to this pit, which was 6 feet wide in the northwest direction, 12 feet long north 80° east, and 6 feet deep. About 4 tons of a galena carrying gray copper, siderite, and quartz, had been taken fron this pit. The lumps were all of them evidently float specimens, and varied from 8 to 12 inches thick, and showed very distinct indica- * An abstract of this paper was kindly presented by Dr. T. Sterry Hunt at the February meeting of the Institute, but as it was not fully written out until the following December, it will describe the mine in a little more advanced stage than when the paper was originally presented.

Jan 1, 1875

Jan 1, 1967