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By George V. Smith, Daniel E. Sonon

Various mechanical properties of the Ni-Co-C alloy system were investigated to delineate the strengthening effect of carbon. Carbon concentration, cobalt concentration, vain size, temperature, and strain rate were varied so that thermal activation analysis and the Hall-Petch analysis could be used to evaluate the strengthening effect of carbon. Increasing carbon increased the strength of nickel and a Ni-60 pct Co alloy , with the effect becoming more pronounced at lower temperatures. Yield stress depended linearly on carbon concentration in nickel, but it depended on the square root of carbon concentration in the Ni-60 pct Co alloy. The Hall-Petch slope of nickel increased with carbon concentration; however, that of the Ni-60 pct Co alloy did not. The yielding behavior of these alloys was sensitive to composition, grain size, and temperature. Cobalt eliminated serrations in the flow curve of carbon-containing nickel at 300' and weakened them severely at higher temperatures. Pairs, or clusters, of carbon atoms appear to be responsible for the observed strengthening behavior. FLINN' conducted several experiments with carbon in nickel in an effort to provide information on the strengthening effect of interstitial impurities in solid solution in fcc metals and alloys. Strengthening which increased with decreasing temperature led him to conclude that carbon causes Cottrell locking in nickel. Fleischer2 analyzed Flinn's data and calculated that the strengthening effect of carbon in nickel was smaller by a factor of fifty than the strengthening effect of carbon in a! iron. Fleischer2 termed the magnitude of strengthening of carbon in nickel "gradual" and that of carbon in a! iron "rapid". He attributed "gradual" hardening to hydrostatic strains and localized changes in modulus of elasticity around solute atoms, whereas he attributed "rapid" hardening to tetragonal strains around solute atoms. Sukhovarov et a1.3-7 reported strain aging and serrated plastic flow in nickel, both of which they attributed to the presence of carbon. Serrated plastic flow has been rationalized by a process involving a series of dislocation pinning and multiplication steps.8, This process is more probable when screw dislocations are strongly pinned. Screw dislocations cannot be pinned by pure hydrostatic forces from the symmetrical strains of an interstitial impurity in an fcc lattice, except for small, second-order effects. However, they might be pinned by localized changes in modulus of elasticity around solute atoms,' by the pinning of the edge components of the partial dislocations of an extended screw dislo~ation,'~ or by clustered groups of solute atoms whose net elastic stress field is unsymmetric. The purpose of the present work was to investigate various mechanical properties of the Ni-Co-C a1loy system which are sensitive to pinning effects in order to delineate the specific pinning mechanism of carbon. Carbon concentration, grain size, temperature, and strain rate were varied so that thermal-activation analysis and the Hall-Petch analysis could be used to evaluate the pinning mechanism. Cobalt was added to lower stacking fault energy so that the number and extension of split, screw dislocations would be increased in order to test the possibility of pinning by carbon at extended screw dislocations. EXPERIMENTAL PROCEDURE Nickel and cobalt (both 99.98 pct-. pure) were melted with graphite in stabilized zirconia crucibles and cast at lo-' Torr to form Ni-C and Ni-60 pctCo-C alloys. Two ingots were heated to 1250°C and were forged to 1-in.-sq bars. These bars were machined to 4-in.-round bars, and then swaged cold to 0.144-in. -diam rods. Reductions in area of approximately 75pct were used with intermediate anneals at 900°C for 1 hr. The carbon content of batches of 0.144-in.-diam rods from each ingot was reduced to two levels by annealing 5-in. lengths in palladium-purified, dry hydrogen at 1100°C for 25 and 100 hr. The remaining material from each ingot was annealed at 10"5 Torr for 1 hr at 1100"~. These treatments gave a total of three carbon levels for both the nickel and the Ni-60 pct Co alloy. The 0.144-in.-diam rods were swaged to 70-mil wire, cut into test specimens, and then re crystallized at lom5 Torr in capsules for 1 hr at temperatures ranging from 760" to 1050" ~. The capsules were broken and the specimens were immediately quenched into water. Average grain size was measured using Hilliard's method of circular intercepts." Annealing twin boundary intercepts were counted in addition to grain boundary intercepts to establish an average grain size. Average grain sizes ranged from 5 to 140 p depending on the cobalt concentration and re-crystallization temperature. Tension tests were made in duplicate at various temperatures at a crosshead speed of 8.34 x 10"4 in. per sec with an Instron Universal Testing Machine. Specimens of 1-in. gage length with soldered ball ends were used at atmospheric and cryogenic temperatures. Pinch grips were used on specimens at elevated tem-

Jan 1, 1969

By T. S. Fuller

The tensile properties of steels at elevated temperatures have been studied by numerous investigatorsll primarily for the purpose of determining their suitability for structural uses. Tests with this objective have been confined largely to the temperature range of approximately 20" to 500' C., because of the rapidly decreasing tensile strength at the latter temperature. Tests have also been extended to higher temperatures2 for the purpose of determining the most suitable forging range. This temperature range is also of theoretical interest. The phenomenon if increased tensile strength and decreased ductility .in the so-called "blue-heat" range, approximately 200" to 300" C., is well known. It was suggested to the Bureau early in 1926 that a study of the properties of rail steels in this temperature range might prove of interest in relation to the studies of transverse-fissure failures in rails. There were available from another investigation3 several new rails from several different heats made to approximately the same specification requirements, the complete manufacturing histories of which were known. It was decided to determine, at least in the preliminary series of tests, only the ultimate tensile strength, elongation and reduction of area, because of the difficulty, time and cost involved in determining the proportional limit and yield point at elevated temperatures.

Jan 1, 1930

By Walter S. Weeks

THE subject of the flow of air through a mine under the influence of natural ventilation has proved an elusive one. To my knowledge only cut and try algebraic solutions have been used where multiple paths are involved. The object of this paper is to present a method for the graphical determination of the flow induced by the natural ventilation pressure (N.V.P.) alone or in combination with a fan. The N.V.P., measured in pounds per square foot, induced by two columns of air between two horizontal planes at different elevations, is equal to the difference in weight of the two columns, assuming each to have a cross-sectional area of 1 sq. ft. Pressure in pounds per square foot is converted into inches of water by dividing by 5.19. Methods of calculating the N.V.P. have been discussed in the literature. In this paper, for simplification of exposition, the change in pressure due to the weight of superimposed air will be assumed directly proportional to the length of the column. The actual methods of calculating the N.V.P. do not affect the solutions to be presented. It must be realized that the precision to be obtained from the small- scale, inked diagrams presented is not as great as would be obtained from large-scale, penciled curves that would be used in practice. The accuracy of the curves does not warrant reading "volumes" closer than the nearest thousand cubic feet per minute. CASE I. DUCTS IN SERIES The simplest type of problem is to determine the flow when two shafts are connected by a crosscut, as shown in Fig. 1. In this example, the resistance of the shafts is to be taken as 0.0001 in. of water for a flow of 1000 cu. ft. per minute for a length of 1000 ft. The resistance of a crosscut is to be taken as 0.0005 in. of water for a flow of 1000 cu. ft. per minute. The small pressures necessary to cause changes in velocity will not be considered, because the accuracy of other obtainable data does not warrant their consideration.

Jan 1, 1938

TO THE BOARD OF DIRECTORS, AMERICAN INSTITUTE OF MINING AND METALLURGICAL ENGINEERS: Gentlemen.-I have the honor to present the following report of the President for the year 1919. In order that this report may be printed and distributed to the members in advance of the February meeting, it is necessary that it end with the calendar year 1919. Any activities during the first six weeks of 1920 will be covered in the Secretary's report for the year 1920. VISITS TO MEMBERS Your President has visited each of the Local Sections of the Institute, with the exception of the ones at Washington, D. C., Tulsa, Okla., and the Nevada Section. These three sections have not arranged meetings at which the President could be present. In addition, your President, accompanied by President Jennings and Secretary Stoughton, in the year 1918, attended meetings of members in Minneapolis and Duluth, Minn., and Houghton, Mich. A dinner and meeting of the members in Pitts-burgh, Pa., was also attended, in company with the Secretary and your President also attended the meeting of Canadian Mining Institute in Montreal, in March, 1919.

Jan 2, 1920

By Charles A. Ashburner

THE appliances which have been proposed, and the modifications in the construction of boiler-furnaces which have been made for the prevention of smoke, and the utilization of what are ordinarily called the waste products of combustion, have been innumerable.

Jan 1, 1882

By Foster Fraas

MOST commercial electrostatic separators utilize the electrical property of conductivity, but although based on the same principles, they are constructed in a variety of forms, a common one being the simple roll type. Some information obtained during an investigation of that type of separator, and which indirectly is applicable to other types, is presented here. NUMERICAL RELATIONSHIP In Fig. I material discharged from hopper 6 is fed onto grounded rotating roll 2. Electrode 3 is at a high electrical potential with respect to roll 2, and any conductive particle in contact with roll 2 therefore acquires an electrical charge of such polarity that, when present in the electrical field, the force on it is in the direction of electrode 3. A detailed description of the charging by conductance as utilized in electrostatic separators may be found in a previous publication.1 As a result of this force, the path of the projected particle is changed in increasing amounts in the direction toward region C as the magnitude of the charge is increased. With the dividing edge 4 the projected particles may be divided into two fractions -those in region C designated as "deflected" or " deflectant " and those in region B designated as "residue." [ ] When material is passed over the roll only once, a complete separation is seldom obtained, therefore most commercial separators contain several roll-separator units in series, and some practical machines use as many as 12. In this paper a "pass" means the passage of material over a single-roll unit. The procedure is to repass either residue B with a low potential on electrode 3 or deflectant C with a high potential on 3. Most electrostatic separations follow a flowsheet of roughing and cleaning either the concentrate or the tailing, on both. In a specific instance, a dry, heated mixture of wet cleaned chromite and garnet from an

Jan 1, 1942

By E. Stansfield

THIS test was described in a privately circulated First Progress Report on Slacking Characteristics of Coal, by A. C. Fieldner and W. A. Selvig, May 1, 1928. The test was described in detail in U. S. Bureau of Mines Report of Investigation 3055, in November, 1930.1 The test, in brief, is conducted as follows: A sample of freshly mined coal consisting of 18 to 25 pieces approximating 1 ¼ cubes, and weighing 500 to 600 grams, is taken for the test. The sample is subjected to a "blank sieving" of carefully regulated degree, on an 8-in. circular sieve with 0.263-in. square openings; and the undersize and oversize weighed. The oversize is placed on a sheet-iron pan and dried for about 24 hr. in an A.S.T.M. air-drying oven maintained at 30° to 35° C. through which a current of warm air is drawn. The sample is then cooled to room temperature and immersed for one hour in water at the same temperature. The water is then drained off, the sample dried for 24 hr. as before, cooled, sieved as before, and the oversize and undersize weighed. The percentage weight of the undersize, is calculated and reported as the first cycle loss. This loss, corrected by subtracting the percentage loss in the blank sieving, is termed the slacking index. The sample may be subjected to further cycles of wetting, draining, air-drying, sieving and weighing. In a letter (August, 1932) W. A. Selvig approved making the blank sieving on a duplicate sample, rather than on the sample used for the test, where sufficient coal was available. This method is now employed in these laboratories. The accelerated weathering test has been employed in the labora-tories of the Research Council of Alberta, at Edmonton, since 1928, but not found entirely satisfactory as repeat determinations with samples taken from the same or adjacent mines frequently showed serious differ-ences. Differences must be expected as the coal may vary in the seam, and the selection of a typical set of lumps approximating 1 ¼ -in. cubes

Jan 1, 1934

By K. C. Gilbart, E. Stansfield

This test was described in a privately circulated First Progress Report on Slacking Characteristics of Coal, by A. C. Fieldner and W. A. Selvig, May 1, 1928. The test was described in detail in U. S. Bureau of Mines Report of Investigation 3055, in November, 1930,1 The test, in brief, is conducted as follows: A sample of freshly mined coal consisting of 18 to 25 pieces approximating 1 1/4 cubes, and weighing 500 to 600 grams, is taken for the test. The sample is subjected to a "blank sieving" of carefully regulated degree, on an 8-in. circular sieve with 0.263-in. square openings, and the undersize and oversize weighed. The oversize is placed on a sheet-iron pan and dried for about 24 hr. in an A.S.T.M. air-drying oven maintained at 30" to 35" C. through which a current of warm air is drawn. The sample is then cooled to room temperature and immersed for one hour in water at the same temperature. The water is then drained off, the sample dried for 24 hr. as before, cooled, sieved as before, and the oversize and undersize weighed. The percentage weight of the undersize is calculated and reported as the first cycle loss. This loss, corrected by subtracting the percentage loss in the blank sieving, is termed the slacking index. The sample may be subjected to further cycles of wetting, draining, air-drying, sieving and weighing. In a letter (August, 1932) W. A. Selvig approved making the blank sieving on a duplicate sample, rather than on the sample used for the test, where sufficient coal was available. This method is now employed in these laboratories. The accelerated weathering test has been employed in the laboratories of the Research Council of Alberta, at Edmonton, since 1928, but not found entirely satisfactory as repeat determinations with samples taken from the same or adjacent mines frequently showed serious differences. Differences must be expected as the coal may vary in the seam, and the selection of a typical set of lumps approximating 1 1/4-in. cubes

Jan 1, 1934

By H. C. Fowler

No exact demarcation can be made between producfion engineering and engineering research projects which interest production engineers because the results of today's engineering research make possible many of the applied production engineering methods of tomorrow. A corollary of the development of fundamental research is that so-called practical research becomes necessary. Assuming engineering research to include all subjects related to oil and gas production on which knowledge is being increased through experimentation and through analyses of data obtained from both the laboratory and the field, a review of the work of 1932 shows that the fundamental concepts of at least three major problems have become better understood—bottom-hole pressures, solubility of gas in oil, and fluid movement—and that the established data on the relationships of oil and gas have been applied to obtain more efficient and more economic production of both. Engineers no longer are concerned primarily with the initial development of devices for obtaining the pressures at the bottom of wells. Advancement in the technique of obtaining reliable pressure readings in wells has been rapid. One of the first public suggestions regarding apparatus for obtaining precise information at the bottom of oil wells was made before the Petroleum Division of the A.I.M.E. in 1928. Even during the early development stages in East Texas, reservoir pressures were estimated from well-head observations. Soon, however, a number of proved devices and methods were available, and today bottom-hole pressures in many fields are being recorded and studied as an essential part of the production programs. The research now turns to interpretations of data, obtained with these devices, in terms of reservoir energy and to the development of methods whereby the oil and gas will be withdrawn in accordance with rational and equitable programs based on oil-gas-energy relationships. The term ((bottom-hole pressures" should not be interpreted as indicating the full scope of all research on this problem. By using pressure (and temperature) data obtained in related vertical-flow studies,

Jan 1, 1933

By G. P. Sewell

Callow-Type flotation cells, with various modifications, have been employed at the Hayden concentrator since 1917. Other flotation machines, such as matless-air and mechanically agitated types, which have been tested in competition, have failed to handle tonnages or give metallurgical results equal to the modified Callow-type cells on the Ray ores. The original type consisted of wide, deep launders with a relatively flat bottom constructed of porous concrete, through which the air was introduced into the flotation pulp. These cells were constructed to handle the tailings from the gravity concentrating process and no special attention was given to pre- conditioning the pulp ahead of flotation.

Nov 1, 1955

By William B. Plank

THERE are 19 pct fewer undergraduate and graduate mineral engineering students enrolled in the ECPD accredited schools of the United States this year than there were a year ago. The figures are: 8727 this year and 10,674 last year. The entire engineering group in both countries numbers 171,070, as compared with 184,547 last year and 252,250 in 1947-48, the peak year. This is a decrease of 7.3 pct since last year, less than half as much as the decrease in the mineral engineering group. These figures on engineering enrollment for the current year, 195.1-52, in colleges of the United States and Canada were prepared jointly by the U. S. Office of Education and the American Society for Engineering Education. The seriousness of the situation is shown. by the reported demand for 60,000 to 90,000 engineers this year for civilian and defense industries and only 35,800 will graduate next June. Many of the 1952 graduates are subject to Selective Service, having been granted deferments while in college, and ac- [ ]

Jan 1, 1952

By R. S. Dean

THE first attempt to establish an equilibrium diagram of the lead-antimony series was made by Roland-Gosselin1 in 1896. This investigation classified the system as a purely eutectiferous one, with the eutectic at 12.5 per cent. antimony and 228° C. In the next year, Stead2 placed the eutectic temperature at 247° C. The error in temperature made by Roland-Gosselin, however, has been perpetuated in the literature with a remarkable degree of persistency; this value was accepted by Campbell (1902), and Ewen (1910),3 and will be found in the last edition of Desch's3 Metallography (1922). Gonterman's investigation, made in 1907, was the most complete one available at the time the present investigation was started. He concluded' that the system was a simple eutectiferous one and placed the eutectic at 13 per cent. antimony and 247°C. Other investigations by Tammann (1907),5 Garbow (1909),6 Rudolfi (1910),7 Loebe (1911),8 and Leroux (1913)9 added little, if any-thing, to Gonterman's diagram. A number of investigations have been made of physical properties of the alloys. The electrical conductivity of the series was studied by Matthiessen (1860)10 and by A. W. Smith (1921);" the thermoforce by Rudolfi (1910),12 and Pelabon (1923);13 the specific heat by Durrer

Jan 2, 1926

By Saluja, Sunder S.

Man had to learn to break rocks as early as the Stone Age, when they formed his main source of raw material. He started with chipping and over the years has reached a stage where he can employ atomic blasts and break, with one blast, millions of tons of rock. In between these two extremes there have been several stages of development including fire setting, use of the expansion of water on freezing in chipped cracks in cold climates, the use of low or deflagrating explosive black powder in about the 17th century, the use of high explosives with the discovery of nitroglycerine in 1846 by Sobrero, followed by the monumental discoveries of the great Swedish scientist Alfred Nobel in the latter half of the nineteenth century.

Jan 1, 1968

By Wilfrid R. Foster

The industrial importance of the sillimanite group of minerals depends upon the beneficial properties exhibited by porcelains and refractories in which substantial amounts of these minerals are utilized as raw materials. The presence of "sillimanite" (now known to be the closely related mineral, mullite) in conventional porcelains and refractories has been known since before the turn of the century. As early as 1906 German investigators observed a direct correlation between the "sillimanite" content of a porcelain and its electrical and mechanical properties. Acting upon this discovery, U. S. Bureau of Standards investigators during World War I developed improved pyrometer tubes and spark plug porcelains, by increasing substantially the amount of "sillimanite" at the expense of quartz. The success of these experiments, first reported in 1918, at once aroused a lively interest in the location of natural sources of sillimanite and its related minerals. As a result of diligent search, the large andalusite deposits in California were discovered in 1919. Within the next several years large deposits of kyanite and sillimanite in India and kyanite in the United States had been reported. The search for these minerals in quantity, by both private and governmental agencies, has continued unabated during the ensuing forty years. A number of domestic deposits of kyanite have been worked during the past 30 years. Of these, only the Virginian and South Carolinian deposits are currently in substantial production. The only commercial andalusite production in the United States has been in California and Nevada. A dumortierite deposit in Nevada, known since 1917 but ignored for want of a commercial use, began production in 1925. A topaz occurrence in South Carolina has yielded a small production since about 1940. Domestic production of andalusite, dumortierite and topaz had virtually ceased by 1950. There has never been any commercial development of domestic sillimanite deposits. Kyanite has been mined almost continuously in India since about 1922. The remoteness of the large deposits of Indian sillimanite had caused it to be neglected until 1949. In that year sillimanite production began, and it has continued to the present. South African andalusite has been marketed from the 1930's until the present time. From 1944 to 1955 Kenya, British East Africa, was an important producer of kyanite. Commercial deposits of kyanite in Ontario, Canada should soon be in production. The first production of kyanite in Europe began in Austria in 1953. No commercial deposits of mullite are known anywhere in the world. It is of interest to note that synthetic mullite, which as "sillimanite" first elicited interest in the A12O3-rich aluminosilicate refractories, has enjoyed a marked increase in production in recent years. This is a result of the gradual depletion of known deposits of high-quality kyanite and related minerals."' Composition The sillimanite group includes kyanite, andalusite, and sillimanite, all having the same chemical composition (A12O3•SiO2) but different physical properties. Two other minerals, dumortierite and topaz, are also included in

Jan 1, 1960

By Bernard Kopelman

The particle size of tungsten metal powder used to make tungsten wire for use in radio tubes and incandescent lamps must be closely controlled if the highly desirable feature of nonsagging is to be achieved. Our knowledge of factors affecting the particle size of tungsten powder has been limited by lack of any extensive literature on the subject. There are no publications in the English language discussing this problem in any but the most general terms. In this paper the published experimental information on this subject is reviewed. Based on the published data and some experimental data obtained by the author, a general theory of factors affecting the particle size of tungsten metal powder obtained by reduction of the oxides in hydrogen is offered. The various forms of the tungsten oxides and tungsten metal used in the experiments described were those prepared by commercial processes, so that the experimental results obtained on a laboratory scale would be more directly applicable to actual commercial reduction conditions. The effects of time of reduction, temperature. and concentration of water vapor in the hydrogen were observed by counting microscopically the particle distribution obtained. Such a method is very time-consuming, but the data obtained by this method are more reliable and more fundamental than those obtained by any of the several instruments available for measurement of particle size. Review of the Literature Until the year 1912, tungsten powder was prepared commercially by reducing tungstic oxide in the presence of carbon or one of its compounds (such as glycerin or ethylene glycol), usually by firing the mixture in a closed fire-clay crucible. The resultant powder contained about 95 per cent tungsten.' When reduction of tungsten oxides by H² was introduced Commercially,²,³ several investigators became concerned with the equilibria between tungsten metal and its several oxides in an atmosphere of hydrogen and water vapor.4-l3 While these many investigations were in fair agreement on the equilibria WO³ + H2 = WO2 + H2O and WO2 + 2H2 = W + 2H2O there arose considerable controversy as to the chemical composition of the oxide between WO³ and WO², because of very poor agreement on the equilibrium constant of this intermediate oxide reduction reaction. The controversy on this intermediate oxide has been in progress for more than 100 years. Thus Malguti,14 in 1835, decided it was WO2.56 In 1857, Riche15 proposed the formula W³O8. Usler,16 in 1865, confirmed the existence of WsO8 and further proposed W1O1l. In 1897, Desil7 agreed upon W²O8 but also found W5O14.

Jan 1, 1947

By Bernard Kopelman

The particle size of tungsten metal powder used to make tungsten wire for use in radio tubes and incandescent lamps must be closely controlled if the highly desirable feature of nonsagging is to be achieved. Our knowledge of factors affecting the particle size of tungsten powder has been limited by lack of any extensive literature on the subject. There are no publications in the English language discussing this problem in any but the most general terms. In this paper the published experimental information on this subject is reviewed. Based on the published data and some experimental data obtained by the author, a general theory of factors affecting the particle size of tungsten metal powder obtained by reduction of the oxides in hydrogen is offered. The various forms of the tungsten oxides and tungsten metal used in the experiments described were those prepared by commercial processes, so that the experimental results obtained on a laboratory scale would be more directly applicable to actual commercial reduction conditions. The effects of time of reduction, temperature. and concentration of water vapor in the hydrogen were observed by counting microscopically the particle distribution obtained. Such a method is very time-consuming, but the data obtained by this method are more reliable and more fundamental than those obtained by any of the several instruments available for measurement of particle size. Review of the Literature Until the year 1912, tungsten powder was prepared commercially by reducing tungstic oxide in the presence of carbon or one of its compounds (such as glycerin or ethylene glycol), usually by firing the mixture in a closed fire-clay crucible. The resultant powder contained about 95 per cent tungsten.' When reduction of tungsten oxides by H² was introduced Commercially,²,³ several investigators became concerned with the equilibria between tungsten metal and its several oxides in an atmosphere of hydrogen and water vapor.4-l3 While these many investigations were in fair agreement on the equilibria WO³ + H2 = WO2 + H2O and WO2 + 2H2 = W + 2H2O there arose considerable controversy as to the chemical composition of the oxide between WO³ and WO², because of very poor agreement on the equilibrium constant of this intermediate oxide reduction reaction. The controversy on this intermediate oxide has been in progress for more than 100 years. Thus Malguti,14 in 1835, decided it was WO2.56 In 1857, Riche15 proposed the formula W³O8. Usler,16 in 1865, confirmed the existence of WsO8 and further proposed W1O1l. In 1897, Desil7 agreed upon W²O8 but also found W5O14.

Jan 1, 1947

By M. Herman, G. J. London

A series of dilute Fe-Co alloy specimens were prepared from zone-melted iron. The iron used was given ten floating-zone passes in purified hydrogen. Alloying was accomplished by plating a gradient of metallic cobalt onto a 1/4-in.-diam bar of material from a pure plating bath. The deposit was radioac-tively tagged by a small addition of co80 to the plating bath. Alloy homogenization was accomplished by passing an additional floating-zone pass through the plated section of the bar. The final concentration gradient achieved was from residual to about 1000 ppm (0.1 pct) added Co. After homogenization, the bar was swaged to 0.057 in. wire and cut to tensile specimen blanks 1-1/16 in. long. Each specimen was counted in a well-type scintillation counter. The concentration of cobalt was computed by combining the normalized specimen counting rate with the known weight (measured to the nearest 0.01 mg) of cobalt added during plating. Fig. 1 shows the cobalt gradient obtained, exclusive of residual cobalt which was estimated by neutron-activation analysis to be approximately 50 ppm. Results of recrystallization for 1 hr at 750°, 700°, 650°, and 600°C with specimens containing 40, 170, 470, and 870 ppm added Co are shown in Figs. 2, 3, 4, and 5. Recrystallization was accomplished in a dynamic vacuum of less than 1 x 10 torr. The specimens were mounted and polished parallel to the swaging direction. The recrystallization re- sults show a radical coarsening of structure with increasing cobalt concentration. The coarsest structure obtained was at the 470-ppm level (at all recrystallization temperatures) with a slight grain refinement at the 870-ppm level shown. A more normal solid-solution effect is seen in Fig. 5 (60OoC, 1 hr) where the only specimen completely recrystallized is the one containing 47 ppm Co. Since the possibility existed that some atmosphere-contamination phenomenon might be responsible for the observed results the recrystallization series was repeated using sealed quartz capsules. These were filled with purified argon which was gettered during heat treatment on metallic titanium included in the capsules. The results obtained were essentially the same as shown. Another identical alloy was made using a 5-mm-diam bar of Westinghouse Puron. Specimen preparation and recrystallization treatment were also as described. The results obtained (see Table I) were somewhat erratic. Some coarsening in structure does appear at the highest cobalt concentrations. There is no apparent relationship between the coarse, columnar, directionally solidified structure of the as-melted bars and any of the recrystallized grain structures observed, all of which are much finer than the former structure. A recrystallization process can be most simply described as one of homogeneous nucleation of recrystallized grains in a cold-worked matrix followed by more or less uniform growth of the strain free grain into the cold-worked material.' An impurity element may influence one or both of these processes. Aust and utter' have shown that impurities strongly influence grain boundary mobility in lead. Moreover, definite recrystallization textures are produced by small concentrations of tin,3 while additions of silver or gold4 produce large boundary in-

Jan 1, 1964

By Milton Williams

IT is generally recognized that fluid is lost from rotary drilling mud s to permeable strata during normal drilling operations;1,2,3 but that this fluid is the filtrate from the mud, rather than the mud itself, has been shown by various workers.1,4,5 . The presence of this filtrate in oil-bearing or gas-bearing strata is undesirable and harmful. The decreased permeability of the stratum to oil effected by the presence of water has been pointed out by several investigators,6,7 and since, in the production of the reservoir fluid, the greatest pressure drop occurs immediately adjacent to the borehole, it follows that infiltered water is particularly objectionable in this region. Again, this filtrate tends to make electrical logs less reliable, since oil in the proximity of the borehole is probably flushed out to an appreciable ent by the water.8 Observation of side wall cores may be misleading for the same reason. Drill-stem tests in low-pressure areas may be of doubtful value where no oil is recovered, unless sufficient time is allowed for production of water lost from the mud. The infiltered water may hinder drilling operations by softening shales and causing sloughing; the "tight hole" occasioned by excessive deposition of filter cake in the hole is a common occurrence. The filter cake remaining on the face of the producing formation may itself sometimes be detrimental to production.9 In view of these implications of the importance of filtration of mud, an investigation was undertaken to determine the factors involved in the infiltration process, and to correlate these in such a manner that the values obtained in routine filter tests employing a conventional filter of the "wall-building tester" type,10 together with data on size of hole, drill pipe, and rate of mud circulation, could be used to estimate water loss and distance of penetration of the filtrate into strata.

Jan 1, 1939

By J. E. Lawrence

Copper-decorated lattice disorders in silicon have been analyzed by electron transmission microscopy, chemical etching, and P-N junction reverse current measurements before and following different gettering treatments. Lattice disorders acted as the nucleating sites for copper precipitation. Copper precipitates in silicon resist chemical etching, absorb electron beams more than silicon, and cause excess reverse currents. Totally gettered disorders will chemically etch rapidly, be transparent to electron beams at extinction contrast, and not contribute to excess reverse currents. Three different gettering procedures were performed to determine the effectiveness of different EXTRANEOUS metal contamination can alter the minority carrier lifetime and resistivity of bulk silicon as well as cause excessive reverse currents in semiconductor devices. Previous workers have reported such activity for gold,1,2 copper,'-* iron,' and rnanganese.2,5 Gettering is a method employed to render these impurities electrically inactive. However, some property of the junction-degrading metals prevents gettering procedures from being wholly reliable. The comparative effectiveness of gettering with different agents has been the topic of earlier publications.2,3,6-11 Two mechanisms for gettering metallic impurities have been proposed: the distribution coefficient mechanism by Thurmond and Logan7 and the compound formation mechanism by Goetzberger and Shockley.2 Both of these models evolved from data gettering mechanisms. First, phosphorus was allowed to enter a protective SiO2 film but remain away from the Si-SiO2 interface to test the effectiveness of the compound formation gettering mechanism. Second, phosphorus was allowed to enter the backside of silicon wafers to test the effectiveness of the lattice strain gettering mechanism. Finally, nickel was diffused into the backside of silicon wafers to test the effectiveness of the distribution coefficient gettering mechanism. In each case, copper precipitates dissolved as a result of the gettering treatment. Tightly packed precipitates will resist gettering more than loosely packed copper precipitates. acquired by the electrical analyses of gettered semiconductor materials. An electrical analysis, however, cannot identify the fate of the gettered metals. The radiotracer technique has recently been applied to determine the redistribution of metals following different gettering treatments.3,9,10 The spatial resolu tion of the radiotracer technique prevented the analysis of metal precipitates which contribute to the excessive reverse currents of P-N junctions. The gettering processes employed by the earlier workers, almost without exception, allowed the gettering agent to enter the silicon lattice. This procedure makes it quite difficult to differentiate between the distribution coefficient and the compound formation mechanisms. The metallographic analysis of gettered copper precipitates discussed in this work supplements the earlier work by obtaining direct evidence of silicon lattice defects decorated with copper before and following different gettering treatments. The effectiveness of a process which restricts the gettering agent, phosphorus, to a dielectric film and thus away from the silicon lattice is discussed in addition to the ef-

Jan 1, 1969

By K. Koneko, T. Nokoyama, S. Shibato

SEYBOLT et al.' have detected various silica films formed on a 3 pct Si-Fe alloy after heating at low oxygen potentials with the electron diffraction method, and they have made some observations on the H,0/H2 ratios required to form them. The purpose of this note is to describe the structure of the oxide film formed on either mechanically or electrolytically polished surfaces of a 3 pct Si-Fe alloy containing small amounts of manganese after heating at low oxygen potential. The samples were prepared from a Si-Fe alloy made in the laboratory using electrolytic iron, 76 pct ferrosilicon, and 76 pct ferromanganese, vacuum-in-

Jan 1, 1969