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By G. G. Hancock, H. H. Johnson

Hydrogen gas at atmospheric pressure is shown to cause substantial embrittlement in a martettsitic high-stretzgth steel. Subcritical crack growth is observed at very lom stresses and with high growth rates. It is suggested that an adsorbed layer of hydrogen atoms at the crack-tip surface provides the damaging hydrogen. Oxygen in small quantity, as little as O.7 pct by volume, is shown to eliminate subcritical crack growth in gas environments caused by hydrogen or water vapor. However, dissolved oxygen in water has little or no influence upon crack-growth rates. Oxygen-stopped cracks may be restarted by water, or by hydvogen or water vapor if oxygen is removed from the environment. These observations are interpreted in terms of preferential adsorption of oxygen at the crack tip and the formation of an oxide barrier. RECENT investigations1-3 have demonstrated that environmental factors are frequently responsible for delayed failure in martensitic high-strength steels. The environment causes crack initiation from preexisting cracklike flaws at unexpectedly low stresses, often far below the uniaxial yield strength. The crack then propagates at a rate controlled by the environment and the crack-tip stress-field intensity; during this period crack propagation will cease if either the stress or the aggressive environment is removed, and this may be considered a definition of subcritical crack growth. Fracture occurs when the crack has grown to a critical length, such that the fracture toughness of the steel is exceeded. Several liquids are known to cause delayed failure, but water and water vapor are the most severely damaging of the environments investigated to date.'-3 It has been suggested that hydrogen produced during corrosion reactions may be the actual embrittling agent2 The severe embrittlement caused by water vapor inevitably raises the question as to whether other gas environments are damaging. Previous work4'5 has demonstrated that high-pressure hydrogen (2250 psi or greater) is an effective embrittling medium, as measured by such criteria as reduction in area, notch tensile strength, and time to failure. Moreover, the embrittlement was eliminated by the addition of small quantities of air or oxygen to the high-pressure hydrogen, but it was not influenced by additions of nitrogen or argon.4 In the present study attention is focused upon gas environments at atmospheric pressure, in particular hydrogen and oxygen. The influence of these constituents upon the initiation and growth of a crack from a pre-existing cracklike flaw in a high-strength steel was determined directly by the electric-potential method of monitoring crack growth. MATERIALS AND PROCEDURE The H-11 steel was supplied by the U.S. Naval Research Laboratory as 3 by 12 by 0.065 in. sheet specimens with 1-in. transverse center slots. The slot tips were finished by Elox machining to a radius of 0.001 in. or less. The yield strength was 230,000 psi; chemical composition and heat-treatment schedule are given in Table I. The experimental apparatus, precracking procedure, and incremental loading sequence have been described previously.3 In the only significant change, precracking was sometimes carried out by a hydrogen embrittlement and baking technique. All experiments were conducted at room temperature; the hydrogen gas environment was purified by a commercial palladium purifier. Crack initiation and propagation were followed by the electric-potential method,'-3 using a calibration that has been recently dicussed. Stress-field intensities at the crack tip were computed by the conventional Irwin frmula; the plasticity correction was negligible and therefore not included. EXPERIMENTAL RESULTS A striking brittleness associated with molecular hydrogen at atmospheric pressure is demonstrated by the data in Table I1 and Fig. 1, which indicate that subcritical cracks in hydrogen initiate at lower stress-field intensities and propagate more rapidly than in fully humid argon. Ki and Kf are the crack-tip stress-field intensities at initiation and termination of subcritical crack growth, respectively. Termination, of course, corresponds to fracture. In both hydrogen and humid argon Ki is less than Kf

Jan 1, 1967

By H. R. Thresh, A. F. Crawley

THIS paper reports the results of viscosity measurements on cadmium and indium undertaken as part of a continuing program of liquid metals research at the Mines Branch, Department of Energy, Mines and Resources, Ottawa, Canada. For several years this work has continued with support from the Canadian Zinc and Lead Research Committee and the International Lead and Zinc Research Organization. In the literature, existing viscosity data for cadmium are conflicting and for indium are scarce. To achieve reliable viscosity values, further work was deemed desirable. Viscosities were measured using an absolute technique applied to an oscillating closed right cylinder of liquid metal. The apparatus, constructed in this laboratory, and the techniques involved in its use have been described in an earlier paper.' In calculating viscosity coefficients from the experimental data. Roscoe's2 mathematical analysis was used. Because accurate viscosity determinations are dependent on accurate density data, and since the available data in the literature are conflicting, the densities of liquid cadmium and indium were also determined in this laboratory by a pycnometric technique. This increased the control exercised over all the variables contributing to the accuracy of viscosity measurements. For both density and viscosity determinations, cadmium and indium of 99.999 pct purity were used. These materials were obtained from Cominco Ltd. In order to suppress excessive evaporation losses and help prevent oxidation, a technique developed in measuring the viscosity of zinc' was used for cadmium. This involved maintaining an atmosphere of purified hydrogen in the viscosimeter during the rela- tively long periods while the experimental temperature was changed and stabilized between individual determinations of the logarithmic decrement. Then, immediately prior to a decrement measurement. the viscosimeter was rapidly evacuated to a pressure of about 2 X 10-6 torr. On the other hand. with indium. no difficulties arise from vaporization or oxidation. In this case. therefore. the apparatus was held under a constant vacuum of about 2 x 10-6 torr. When all sources of random and systematic error have been evaluated, the technique is considered to yield data accurate within 10.5 pct. The viscosity of cadmium was measured to a maximum temperature of 451.8°C and that of indium to 346.5°C. These temperatures are. respectively. 130° and 190°C above the melting points. Two separate runs were made on indium. The results are given in Table I and, when plotted. yield the smooth curves evident in Figs. 1 and 2. Values of A and C to fit the well-known Andrade1 equation were determined by a regression analysis. The equation is: where n = coefficient of viscosity. i = specific volume. T = temperature in °K Despite its empirical nature. Andrade's equation has been shown by many workers to describe accurately the temperature dependence of viscosity. During the current research program, this equation has been found to fit the data precisely for all the metals and alloys that have been studied.5,6 The A and C' values for cadmium and indium are given in Table 11. Comparing the magnitude of the present data with those of previous workers,7-10 as has been done in Fig. 1, it is evident that the results of Fisher and Phillips10 deviate markedly from the rest. With the exception of one point from Gering and Sauerwald,7 all other data agree within ±2.5 pct. However, the agreement between the present results and the work of Menz and sauerwald9 is especially good over the entire experimental temperature range. Such agreement may be expected since Menz and Sauerwald's

Jan 1, 1970

By AIME AIME

ALMOST as many attended the annual dinner this year as last, when the presence of Mr. Hoover was such an attraction that almost two-thirds more than had ever attended before were present. Only by putting the late comers at tables in the balcony could everybody be accommodated. Past President De-Golyer was the toastmaster and in opening the post-prandial exercises referred to the regrettable fact that this was the last of the long series of dinners which have been held at the Waldorf, as the hotel will be torn down to give way to an office building before another year. To the delight of the gathering "Oscar" appeared and, in a delightfully brief but characteristic speech, referred to the long association that had existed and hinted that a new Waldorf-Astoria may arise, where the Institute could continue to gather annually in an enlarged replica of the room they had met in so long. Before taking up the presentation of the medals, Mr. DeGolyer referred to the Institute's "Legion of Honor," the 34 men who have been members continuously for over fifty years. For various reasons only five of them, W. S. Ayres, F. G. Corning, Henry D. Hibbard, A. F. Schneider and Arthur Thacher, could be present. They were all seated at the speaker's table, and W. S. Ayres, 56 years a member, as the dean of the group, was called on to respond for them all. He said: "The introduction I have just received would indicate that this particular group of men to which I belong is considered by the chairman to be a group of real antiques. Possibly you are questioning the accuracy of his judgment. I hope you are, although there may be some first-sight evidences tending to substantiate the view held by the chairman.

Jan 1, 1929

By E. C. Truesdale, W. K. Waring

The Research,Division of The New Jersey Zinc Company (of Pa.) has conducted, over a period of years, numerous tests of the reducibility of various zinc ores and the reactivity of various kids of coal, using a number of different experimental methods. Most of these tests have involved the reduction of mixtures of ore and coal. In such cases the following simultaneous reactions are believed to be mainly responsible for the production of zinc, as was shown by Bodenstein' some years ago: ZnO + CO = Zn + CO2 [i] C + COj = 2CO [2] Each of these reactions is dependent upon the other for the supply of CO and COz, respectively, and the over-all rate of formation of zinc vapor will be determined by the slower of these two reactions. An analogous pair of reactions sometimes of importance is: ZnO + He = Zn + HZO 13] C + Hz0 = CO + He U3 While it is possible to obtain an indication of the relative reducibility of various ores, or of a fine versus a coarse Ore, by testing them with a given coal, and while coal reactivities may be measured in a corresponding manner, a more direct determination of relative reaction rates is possible by carrying out the desired reactions, such as I and 2, separately and under reproducible conditions. It is one purpose of this paper to present some of the results that have been obtained by the latter method. C. G. Maier2 discusses the relative rates of reactions I and 2 and concludes that while at relatively low temperatures reaction I is faster than reaction 2, this difference becomes less with increasing temperatures, although at smelting temperatures reaction is still the faster. He also says (p. 48), "At temperatures . . . be- -tween 1100' and 1300°C., . . . the zinc oxide reduction reaction is intrinsically more rapid than its physical limitations; that is, it is limited by gas diffusion rates.'' In the course of numerous reactivity tests involving the separate use of reactions and I and 2, we have obtained data that show by direct experiment, we believe for the first time, the correctness of Maier's statements concerning these reactions. We also include data on the relative rate of reaction 3, involving reduction by hydrogen. Finally, some interesting results obtained by carrying out the reduction of ' a zinc ore-coal briquet in streaming atmospheres of nitrogen, carbon monoxide and hydrogen, respectively, are presented.*

Jan 1, 1944

By Howard Eavenson

EARLY in 1917, the United States Coal & Coke Co. secured options on several tracts in Harlan County, Ky., aggregating about 1.9,000 acres in area, and after careful prospecting by outcrop openings and diamond drilling, completed the purchase late in July of that year. This property is situated in the eastern end of Harlan County, south of the Poor Fork f Cumberland River, and extending across Big Black Mountain to the Clover Fork of Cumberland River, a distance of about 7 mi. (11.3 kg.). It extends from the Kentucky-Virginia line westward for about 6 mi. Looney Creek, which empties into Poor Fork, crosses the property for about 4 mi. (6.4 kg.), and as several of the seams within the property outcrop along this stream, it afforded an easy, and the logical, place for development. The property is on the northern side of the geological trough formed by the uplifting of Stone Mountain, on the southern, and Pine Mountain, on the northern side; the northern boundary along Poor Fork is practically at the base of Pine Mountain. This, area has been described in various geological reports.1 The main seam on this property is the one known variously as the "C," Benham, Keokee, Taggart, and Roda; it is, also called, by the Kentucky Geological Survey, the Kellioka seam of the western portion of Harlan County. This seam averages, in this property, about 5 ft. (1.5 m.) in thickness, although local rolls reduce this thickness considerably over small areas; and at the extreme western end of the property the seam splits. It is usually clean, although occasionally a small parting occurs within a few inches f the bottom f the seam; it is one f the best

Jan 9, 1921

By Paul A. Beck

THE occurrence of the (100) [lOO] or "cube" texture upon annealing of cold-rolled copper has been much investigated.' The conditions favorable for its formation were found to be a high final annealing temperaturez or long annealing time," a high reduction of area in cold rolling prior to the final anneal,' and a small penultimate grain size." The effects of penultimate grain size and of rolling reduction were found by Cook and Richards4 to be interrelated in such a way that any combination of them giving lower than a certain value of the final average thickness of the grains in the rolled material leads to a fairly complete cube texture with a given final annealing time and temperature. Also, according to the same authors, at a higher final annealing temperature a larger average rolled grain thickness, i.e., a lower final rolling reduction, is sufficient than at a lower temperature. These somewhat involved conditions can be understood readily on the basis of recent results obtained at this laboratory. Hsun Hu was able to show recently by means of quantitative pole figure determinations that the rolling texture of tough pitch copper, which is almost identical with that of 2s aluminum: may be described roughly as a scatter around four symmetrical "ideal" orientations not very far from (123) [112]. In the case of aluminum, annealing leads to retain-ment of the rolling texture with some decrease of the scatter around the four "ideal" orientations, and to the appearance of a new texture component, namely the cube texture." A microscopic technique, revealing grain orientations by means of oxide film and polarized light, showed that the retainment of the rolling texture is achieved through two different mechanisms operating simultaneously, namely "re-crystallization in situ," and the formation of strain-free grains in orientations different from their local surroundings, but identical with that of another component of the rolling texture. Thus, a local area in the rolled material, having approximately the orientation of one of the four "ideal" components of the texture, partly retains its orientation during annealing, while recovering from its cold-worked condition, and it is partially absorbed at the same time by invading strain-free grains of an orientation approximately corresponding to that of another "ideal" texture component. The reorientation here, as well as in the formation of the strain-free grains of "cube" orientation, may be described as a [Ill] rotation of about 40°, see Fig. 1 of ref. 6. The preferential growth of grains in such orientations is a result of the high mobility of grain boundaries corresponding to this relative orientation.' " It appears very likely that in copper the mechanism of the structural changes during annealing is similar to that observed in aluminum (except for the much greater frequency of formation of annealing twins in copper). In both metals the new grains of cube orientation have a great advantage over the new grains with orientations close to one of the four components of the rolling texture. This advantage stems from their symmetrical orientation with respect to all four retained rolling texture components of the matrix; they are oriented favorably for growth at the expense of all of these four orientations. As a result, the growth of the "cube grains" is favored over the growth of the others, as soon as the new grains have grown large enough to be in contact with portions of the matrix containing elements of more than one, and preferably of all four component textures. It is clear that this critical size is smaller and, therefore, attained earlier in the annealing process if the structural units, such as grains and kink bands, representing the four matrix orientations are smaller, i. e., if the average thickness of the rolled grains is smaller. Hence, for a given annealing time and temperature, a smaller penultimate grain size and a higher rolling reduction both tend to increase that fraction of the annealing period during which the above condition is satisfied. Consequently, the percentage volume of material assuming the cube orientation increases. The same is true also for increasing time and temperature of annealing when the penultimate grain size and the final rolling reduction are constant, since the average size attained by the new grains during annealing increases with the annealing time and temperature. For the same reason, at higher annealing temperatures a given volume percentage of cube texture can be obtained with larger rolled grain thickness (larger penultimate grain size, or smaller rolling reduction) than at lower annealing temperatures. The well-known conspicuous sharpness of the cube texture may be interpreted as a result of the fact that selective growth of only those grains is favored that have an orientation closely symmetrical with respect to all four components of the deformation texture and exhibit, therefore, a high boundary mobility in contact with each. The effect of alloying elements in suppressing the cube texture, as described by Dahl and Pawlek,' appears to be associated with a change in the rolling texture. For face-centered cubic metals, such as copper, which do exhibit the cube texture upon annealing, the rolling texture is always of the type described above, i. e., scattered around four "ideal orientations" of approximately (123) [112]. The addition of certain alloying elements, such as about 5 pct Zn or 0.05 pct P in copper, has the as yet unexplained effect of changing the rolling texture into the (110) 11121 type. This texture consists of two fairly sharply developed, twin related components. In such cases, as in 70-30 brass and in silver, the annealing texture again is related to the rolling texture by a [lll] rotation of about 30°, however, because of the different rolling texture to start from, it has no cube texture component. At higher temperatures, both in brassm and in silver," grain growth leads to a further change in texture: A [lll] rotation of the same amount, but in reversed direction, back to the original rolling texture.

Jan 1, 1952

By John Buch

NEARLY 25 years ago operating officials in the northern anthracite field were confronted with the problem of profitably mining virgin beds of thin coal (those 48 in. and under) or destroying them by mining under-lying thick beds. To solve this problem costly hand-mining methods were replaced by cheaper mechanical methods, which eliminated the need for the lifting of bottom or the brushing of top in excessive quantities, which was essential if proper height for hand loading' was to be provided. During this period long-face mining was an outstanding development. In its favor in comparison with any other method were the ease with which undercutting machines could be used, a differential in powder cost of about fifteen cents per ton in favor of this method over mining from a solid chamber or pillar face, and a greater production per day from a single working place, resulting in lower capital expenditures for a given total production, closer supervision and lower transportation cost. The long faces were drilled by jackhammer and undercut by machines. The coal from the cut was loaded into mine cars placed on the gangway road by means of a double-drum mechanical scraper engine and a mechan-ical V-type scoop. A tugger hoist was used to spot empty cars at the loading point from a supply placed at the operation by an electric mine locomotive. During loading the roof was supported by vertical wooden props paralleling the face. After the loading was completed the scraper engine and the ropes that had been used to propel the scoop in the loading of coal transferred the props to and along the face. A row of unfilled cogs was then built parallel to the new face and about 6 ft. from it. These cogs were usually made 6 by 3 ft., the longer dimension paralleling the face; they were placed on an average at 12-ft. centers. These wooden cogs were left in place and were buried later by falling roof. Attempts to remove them were never successful. When a new long face was started, the cog spacing would be increased to about 20-ft. centers. As successive cuts were made, weight would begin on the cogs, and they

Jan 1, 1939

By AIME AIME

THE convention which met in Washington at the call of the Joint Conference Committee was called to order at ten o'clock on Thursday morning; June 3, by Richard L. Humphrey, temporary chairman, member of the American Society of Civil Engineers, who made a brief statement of the reason for the meeting. Lieut. Col. Charles W. Kutz, Corps of Engineers, U. S. A., and Engineer Commissioner of the District of Columbia, then welcomed .the engineers composing the convention on behalf of the District of Columbia and, the Washington engineers. Although an elaborate program had been prepared on which were many well-known speakers on interesting and important topics, , it was voted to intersperse this to fill in the usual and unavoidable hiatuses in the business program of such a convention[ Calvert Townley, president of the American Institute of Electrical Engineers, was elected permanent chairman, and J. C. Hoyt, of Washington, was elected secretary of the convention. The following committees were appointed: Consti¬tution and by-laws, Richard L. Humphrey, chairman; resolutions, Philip N. Moore, chairman; and program, F. H. Newell, chairman. Then, Gardner S. Williams, member of the, A. S. C. E. and the Grand Rapids Engineering Society of. Grand Rapids, Mich., and one-time member of the American Association of Engineers, offered the following resolutions:

Jan 1, 1920

By John Fritz

TROUGH it is not a condition of the Award, the fact is that the John Fritz Medal never has been given to an engineer who had not already received one or more similar awards. This "medal for medalists," on the evening of April 20, was presented to Daniel C. Jackling at a special dinner held at the Union League Club in New York. The citation read "For notable industrial achievement in initiating mass production of copper from low-grade ores through the application of engineering principles." The present award recognizes the same accomplishment-the launching and guiding to the port of marvelous success of the Utah Copper Co., first of the so-called "Porphyries"-as did the award of the William Lawrence Saunders Gold Medal by the A.I.M.E. in 1930, and before that the Award of the Gold Medal of the Mining and Metallurgical Society of America in 1926. Following the custom a biography of the Medalist had been published in a small pamphlet as a supplement to the John Fritz Medal Book. T. A. Rickard was the au¬thor of the sketch of Mr. Jackling, an innovation being the placing of a copy of the booklet at the place of each of the diners. The committee in charge of the dinner consisted of two past-presidents: R. E. Tally, of the A.I.M.E., who was chairman; Bancroft Gherardi, of the A.I.E.E.; and Thaddeus Merriman, director of the A. S. C. E., the John Fritz Medal being a joint award of the four societies. Frederick M. Becket, President of the A.I.M.E., as chairman for the occasion, briefly stated the purpose of the dinner. He stressed his satisfaction that the award was symbolic of the cooperative professional activities of the four great national organizations of engineers. He introduced Francis Lee Stuart, past-president of the A.S.C.E. and now chairman of the John Fritz Medal Board of Award. Mr. Stuart outlined the history and purpose of the Medal established in 1902 in memory of John Fritz, of Bethlehem, Pa., one of the great pioneers of America's iron and steel industry, metallurgist, and president of the A.I.M.E. in 1894. Mr. Stuart called the roll of former John Fritz Medalists, three of whom, Ralph Modjeski, J. Waldo Smith, and Ambrose Swasey, were present to do honor to Mr. Jackling. He then introduced George Otis Smith, whose privilege it was to present the Medalist for 1933. Dr. Smith was the senior of the four A.I.M.E. representatives on the Board that last year selected Mr. Jackling for the honor. His speech follows in full.

Jan 1, 1933

By Franklin R. Carpenter

Pyritic smelting, so-called, as practiced in the Black Hills is pyritic smelting only in the sense that Dr. John Percy uses the expression in his " Metallurgy of Silver," where he describes a process for smelting dry silver-ores in connection with iron pyrites, to form a regulus. The ores treated by this process in the Black Hills are very siliceous, averaging about 74 per cent. of silica, from 10 to 20 of iron oxide, 4 or 5 of alumina, and from 2 to 4 of lime. In 1889, while Dean of the South Dakota School of Mines, I took up the question of their smelting. There were neither copper- nor lead-ores in the Hills; hence pyrite and pyrrhotite, of which there are large deposits, were employed to form a regulus. This mixture of pyrite and pyrrhotite, besides being absolutely barren of gold and silver, carried an average of 30 per cent. of silica. The only basic material available as a flux for the great excess of silica in the ores and in the pyrite was a dolomitic limestone. Moreover, the local coke gave 24 per cent. of ash, 60 per cent. of which was silica—as unpromising a set of conditions as can well be imagined. We had before us the examples of Mr. W. Lawrence Austin, of this Institute, who had experimented at Toston, Montana,"

Jan 1, 1901

By Donald B. Gillies

WE HAVE come a long way since the time of the old steel master who declared that chemistry would ultimately bring the steel business to ruin. Yet I sometimes doubt whether even now we fully recognize the great debt we owe to the institutions that today are initiating young men into the fascinating mysteries of science and training them in the art of engineering. I am not sure that we recognize the importance of the contribution that the schools of applied science and the technical colleges are making to our industrial economy. That contribution is neither narrow nor restricted. It covers the whole range of industry. Dr. Compton, himself, has shown in his survey of leading American corporations that the engineer is twelve times more likely than the nonengineer to become president, five times more likely to become treasurer, and thirty times more likely to become an officer. So the hand of the engineer not only is all-powerful in the laboratory and in the drafting room but his control is increasing in all departments of management.

Jan 1, 1940

By Henry Tobelmann

THE location, mode of occurrence of ore, and preliminary tests leading to the development of the present leaching process and the building of the present plant on the property of the New Cornelia Copper Co. at Ajo, have been described in previous papers presented to the Institute and in the, discussions thereof.1 It is sufficient to say that these tests began early in July, 1912, and were continued to the close of January, 1916; that small tests at Douglas were followed by the construction of a 1-ton plant at the mine; and this was followed by the operation of a 40-ton plant for 14 mo. In all about 15,000 T. of ore were treated experiment-.

Jan 2, 1919

By H. C. Gatos, J. T. A. Pollock

It is well known that the superconducting critical current densities of many alloy superconductors may be increased by cold working and in some cases further enhanced by a short heat treatment. This latter enhancement has been attributed to the redistribution of dislocations into cell-like networks' and to the precipitation of second phase particles,2'3 which act as flux pinning centers. In a manner analogous to dislocation pinning in precipitation hardening alloys,4 it is expected that here also a critical distribution of the pinning centers should result in maximum pinning effect. Concentration inhomogeneities exist in most or all commercial alloys yet there have been only a few attempts made to determine their effect on critical current capacity in the absence of cold working. Sutton and Baker,5 and Kramer and Rhodes6 have found that the complex precipitation processes occurring during the aging of Ti-Nb alloys can result in critical current density enhancement. Livingston7-10 has clearly shown, for lead and indium based alloys, that the distribution of precipitated second phase particles is of critical importance in determining magnetization characteristics. However, these '(soft" alloys age at room temperature and the time involved in specimen preparation prevents metallographic examination in the state in which the superconducting measurements are made. Thus results with such alloys are expected to be biased towards larger precipitates and interpar-ticle spacing. The present study of Ta-Zr alloys was undertaken to examine the influence of second phase precipitation, as controlled by heat treatment, on the critical current capacity of well annealed polycrystalline material. A study of the published phase diagram11 indicated that annealing supersaturated samples containing up to 9 at. pct Zr at suitable temperatures would result in the precipitation of a zirconium-rich second phase. It was MATERIALS AND PROCEDURE The alloys were prepared from spectrochemically pure tantalum and zirconium. Analysis was carried out by the supplier. Major impurities in the tantalum were: 12 pprn of 02, 17 pprn of N2, 19 pprn of C, and less than 10 ppm each of Mo, Nb, Al, Cr, Ni, Si, Ti. The crystal bar zirconium was pure except for the following concentrations: 15 pprn of 02, 17 ppm of C, 23 ppm of Fe, 11 ppm of Cu, and less than 10 pprn each of Al, Ca, N2, Ti, and Sn. Samples were prepared in the form of 8 to 10 g but-tons by arc melting using a nonconsumable electrode on a water-cooled copper hearth in a high purity ar-gon atmosphere. Each button was inverted and re-melted three times to ensure an even distribution of the component elements. The samples were then homogenized at temperatures close to their melting points for 3 days in a vacuum furnace maintained at 5 x 10-7 mm Hg. After this treatment the buttons were cold rolled to sheets approximately 0.020 in. thick from which specimens were cut, 0.040 in, wide and 1 in. long suitable for critical current density (J,) and critical temperature (T,) measurements. These strips were then recrystallized and further grain growth was allowed by an additional vacuum heat treatment at 1800°C for 60 hr. Some second phase precipitation occurred during cooling of the furnace and a solution treatment was necessary to produce single phase supersaturated samples. This treatment was successfully carried out by sealing the samples together with some zirconium chips in quartz tubes under a vacuum of 5 x 10-7 mm Hg, heating at 1000°C for 5 hr and then quenching into water or liquid nitrogen. The samples were then heat treated at either 350" or 550°C and quenched into water or liquid nitrogen. All samples which were heat treated at 350°C were quenched in both cases by cracking the capsules in liquid nitrogen. The samples treated at 550°C were quenched by dropping the capsules into water. Analysis for oxygen in randomly selected samples indicated that the oxygen content was in the range of 175 to 225 ppm. Values of Tc were determined by employing a self-inductance technique. Jc measurements were made at 4.2oK by increasing the direct current through the wire in a perpendicularly applied field until a voltage of 1 pv was detected with a null meter. The risk of resistive heating at the soldered joints during these latter measurements was reduced by first plating the ends of the wires with indium and then soldering to the copper current leads using tin. Metallographic examinations were performed after mechanical polishing of the same samples and etching in a 4H20:3HN03 (conc):lHF(conc) solution.

Jan 1, 1970

By Lloyd B. Underwood

Dr. Gardener, in Chapter 2, has presented a comprehensive state-of-the- art review of site investigations For tunneling. Nearly all of the techniques he discussed will also be required for future site investigations. Therefore, this chapter will be devoted to a few rather new exploration techniques plus ideas for improving some of the present-day methods. In March 1962, the first symposium on "Remote Sensing of Environment" was held at the University of Michigan.l Since that time, four additional symposiums have been held at the same University. Also, the technical Literature has recently included a number of articles on remote sensing techniques. A recent one appeared in the February 1968 issue of Materials Research and Standards.Vt was entitled "Developments in Remote Sensing Applicable to Airborne Engineering Surveys of Soils and Rocks," and was written by Dana C. Parker. Mr. Parker predicts that aerial reconnaissance will someday supplant soil augers, rock drills, surface reconnaissance, and geophysical surveys as the engineer's primary means of obtaining information about soils and rocks. He states, "The engineer wishing to survey a route or a site or to locate rock and soils suitable for construction projects will be able to push some buttons in an airplane and record all the data required for determining the relevant conditions. In a short time after he returns to earth with his rolls of film and charts, he will be able to reduce and analyze the data by partially computerized techniques and to compile a concise and comprehensive engineering report that gives all the relevant information about rocks, soil, water, and vegetation in the area he surveyed. Most important he will feel as confident with his recommendations, derived primarily from image characteristics and spectral power distributions, as his predecessors did with recommendations based on more tangible evidence obtained from drill cores and surface reconnaissance." The airborne sensors for engineering surveys of soils and rocks are those that sample some electromagnetic property of the materials that com- prise the terrain and cover its surface. In addition to cameras, these include

Jan 1, 1970

By Joseph L. Patrick

Geologic exploration, which has experienced an upward trend in the United States since 1962, continued with increasing activity through 1965. New, spectacular discoveries of recent years and continued questionable economic and political climates in many areas of the world have continued to focus the exploration attention of an increasing number of companies on the United States. Traditional geologic field methods are being bolstered by development of new methods, techniques and geophysical instruments. Reports from the states emphasize that successful exploration is dependent upon the combined effort of geochemistry, geophysics and geology, with high quality laboratory support of the field effort becoming increasingly necessary. PROGRAMS NOW UNDERWAY IN WEST During 1965 mineral exploration reached an all- time high in Nevada. Although examinations are being carried on throughout the State, much of the work is limited to two areas. The first area to attract recent exploration interest, initiated by discovery of the Carlin gold mine by Newmont Mining Corp., is an area of windows near the leading edge of the Roberts Mountains thrust fault in northeastern Nevada. Included in this area are the old camps of Mountain City, Battle Mountain, Cortez, Mineral Hill and Eureka. Major mining companies are using a combination of surface mapping, geochemistry, geophysics (largely induced potential surveys), following up with drilling. The second area of exploration is along the Walker Lane, a wide shear zone that parallels the Nevada-California boundary from Virginia City to Las Vegas. Activity has been intense in the Tonopah-Yerington area. Discovery of a large copper-iron deposit following an airborne magnetometer survey first focused recent attention on Walker Lane. Sixteen major companies are involved in exploration in the State.

Jan 2, 1966

By John V. Beall

HEAVY-DENSITY separation processes, a commercial application of the sink-float test used in mineralogical laboratories for the separation of mineral particles by their difference in specific gravity, are the biggest development in mineral dressing since flotation, which was at about the same stage of development thirty years ago. The scope of their application has broadened and, though still in the development stage, they are being accepted in a constantly increasing number of commercial installations. This progress in mineral beneficiation is especially satisfying when we realize that our high-grade ore deposits are fast disappearing and a big factor in determining whether a hole in the ground is being sat upon by a liar or an honest citizen is how economically the ore dressers can concentrate comparatively low-grade ores. As early as the middle of the nineteenth century attempts were made to use aqueous salt solutions in a heavy-liquid separation for cleaning coal. But the original and recovery costs of these liquids were high and further, the fact that they were corrosive, unstable, and toxic added to the difficulty in using them.

Jan 1, 1948

By W. D. France, H. l. Burghoff

FABRICATORS of copper and copper alloys have contended with the problems of reconversion during the past year in endeavoring to return to the full-scale production that is demanded of them. The problems have not been easy, for the industry, like so many others, has had to deal with strikes of long duration, and material shortages, particularly in the raw materials, copper, zinc, lead, and tin. Despite all these obstacles, it was possible to gear production to new peacetime records during the latter part of the year. This was made possible not only by the use of multiple shifts of personnel, but also by the improved production equipment, the development of which had been stimulated by wartime necessity. The work of installing new and better equipment is still continuing, and virtually every company is engaged in improving or planning to improve its processes.

Jan 1, 1947

By A. S. Grove, C. T. Sah, E. H. Snow, B. E. Deal

A summary of- several recent investigations in to the properties of the metal-oxide-silicon system is presented. A major portion of these studies makes use of the MOS capacitance-z)oltage method of' analysis. The particular areas of investigation which are reported include: 1) a general survey of the electvical properties of thermally oxidized silicon surjbccs; 2) a study of ion migration through silicon dioxide films ; 3) measurements of electron and hole mobilities in surface inversion layers; 4) a study of impurity redistribution due to thermal o.ridatiotz; and 5) measurements of the rates of oxidation oj-heavily doper7. silicon. THE importance of the metal-oxide-semiconductor (MOS) system in the semiconductor industry is well-known. In addition to its importance in the "planar" device technology,' the MOS structure is now also used in the fabrication of active solid-state devices. Consequently, extensive efforts have been made recently to obtain a better understanding of the characteristics of this system. A summary of some studies of the MOS system conducted in our laboratories during the past year is presented. For the most part these studies used silicon as the semiconductor, along with silicon dioxide and aluminum as the other two components of the system. Since the MOS capacitance-voltage method of analysis was used extensively in these studies, we will first briefly describe its nature and consider some of the possible causes of deviation of experimental observations from the simple theory. We will then outline the various related areas of investigation carried out in our laboratories and will briefly indicate some of the results. It should be noted that the purpose of this paper is merely to provide a brief summary of MOS studies. More detailed discussions of the various areas of investigation are given in the references cited. PRINCIPLES OF THE MOS C-V METHOD OF ANALYSIS' A sketch of the MOS structure is shown in the upper portion of Fig. 1. In this case the insulating film is Si02 and the semiconductor p-type silicon. If a large negative bias is applied to the metal field plate, holes are attracted to the silicon surface. The silicon then behaves much like a metal and the capacitance measured is that of the oxide layer alone, Co. If a small positive bias is applied to the aluminum, holes are repelled and a region depleted of majority carriers is formed at the silicon surface. This depletion I-egion adds to the width of the dielectric and the measured capacitance begins to drop. With increasing positive bias, the width of the electrical depletion region increases. At some large positive bias an inzevsion regiotr is formed at the surface and additional charges induced in the silicon appear in the form of electrons in this narrow inversion region. Thus the depletion-region width approaches a maximum value and, consequently, the capacitance reaches a minimum value and then either levels off or rises again depending on the measurement frequency and the rate of equilibration of the minority carriers in the inversion layer.3 Band diagrams, along with the corresponding charge distributions, are shown in Fig. 1 for the above bias conditions. If minority carriers cannot accumulate at the surface to form an inversion region, the depletion-region width continues to increase with increased positive bias and the capacitance drops toward zero as in a reverse biased p-n junction. The effect of a work-function difference $hs between the metal and the silicon, and of surface charges per unit area Qss located at the oxide-silicon interface, is simply to attract charges in the silicon much like the applied bias. It can be shown that this results in a parallel shift of the capacitance-voltage characteristic along the voltage axis by an amount corresponding to AV = -$bIs + Qss/Co. Theoretical curves have been calculated4 giving the capacitance of the MOS structure C normalized to the oxide capacitance Co vs the quantity VG here VG is the voltage applied to the metal field plate. In Fig. 2 such calculations are shown as points for a particular oxide thickness and bulk impurity concentration for a p-type semiconductor. (For an n-type semiconductor the curves would be mirror images of these.) All three cases, i.e., low frequency. high frequency, and depletion, are indicated. Also shown in the figure are recorder tracings of the characteristics of actual devices. These characteristics have been shifted along the voltage axis to compensate the effect of surface charges and work-function difference. It is evident that agreement between experiment and theory is good. The nature of this shift along the voltage axis is

Jan 1, 1965

By R. W. Regehr, R. A. Burmeister

Epitaxial growth of GaAs 1-xPx on germanium substrates was achieved using an open tube vapor transport system. The compositional range of 0.3 < x < 0.4 was examined. The best results were obtained with (311) orientation of the germanium substrate. The physical and chemical properties of the resulting layers were investigated using several techniques. Spectrographic analyses of the layers indicate substantial incorporation of germanium into the GaAs t-X Px layer. Evidence is presented which indicates that this incorporation occurs via a vapor phase transport process rather than by solid phase dijfu-sion. Electrical measurements suggest that the germanium thus incorporated behaves predominantly as a deep donor in the compositional range of 0.33 < x * 0.40 and has a deleterious effect upon the luminescent properties of GaAs1-x Px. The increasing technological importance of GaAs1-xPx for use in light-emitting devices has led to an evaluation of several aspects of existing growth processes. The method most commonly used to prepare GaAs1-xPx for electroluminescent device applications is vapor phase epitaxial growth on GaAs substrates.&apos;-4 In a typical electroluminescent diode structure the active region of the diode is entirely within the epitaxial layer and thus the electrical properties of the substrate are relatively unimportant since it is effectively a simple series resistance (assuming hetero-junction effects to be negligible). The use of germanium rather than GaAs as the substrate material is of interest for several reasons. First, GaAs of reasonable structural quality has been epitaxially grown on germanium4-2 and it is reasonable to expect that GaAs1-xPx could subsequently be deposited on the GaAs layer. Second, germanium substrates are readily available with both lower dislocation densities and larger areas than GaAs. Finally, single crystals of germanium are more economical than GaAs single crystals. The principal objective of the present investigation was to test the feasibility of growing GaAs1-xPx epi-taxially on germanium substrates, and to evaluate the properties of such layers with regard to electroluminescent device requirements. The approach used was to a) demonstrate epitaxial growth of GaAs1-xPx on germanium, and b) characterize the relevant structural, electrical, and optical properties of the GaAs1-xPx layers. The possibility of germanium incorporation into the grown layers was of special interest since there was some indication of this in previous studies of GaAs growth on germanium.5&apos;11,12 Although a study of the electrical properties of germanium in GaAs1-xPx was not an intent of this investigation, several features of the electrical properties of the layers grown in the present study which appear to be due to germanium are described. EXPERIMENTAL PROCEDURE The open-tube vapor transport system used for the epitaxial growth of GaAs1-xPx is illustrated in Fig. 1. This system utilizes the GaC1-GaC13 transport reaction and is similar in most respects to the larger system described elsewhere.&apos; The germanium substrates were n-type, with a resistivity of 40 ohm-cm (Eagle-Picher Co.). These were cut to the orientations of {100), {111), and (3111, and were mechanically polished and chemically etched in CP-4 (5 min at 0°C) prior to growth. In some cases, a GaAs substrate was employed in addition to the germanium. The orientation of the latter was {loo}, and they were also mechanically polished and chemically etched prior to growth. The initial composition of the deposited layer was pure GaAs. After approximately 10 microns of GaAs was deposited on the germanium substrate, the phosphorus content of the layer was gradually increased over a distance of approximately 15 microns to the desired concentration and maintained at this value throughout the remainder of the growth. Typical operating parameters used during growth are given in Table I. Selenium was used as a n-type dopant in several runs to facilitate comparison of the electrical properties of the layers grown on germanium with those of layers grown on GaAs substrates, which are usually doped with selenium. The concentration of H2Se in the gas phase was adjusted to a value which would normally yield a carrier density of 1 to 5 x 101 7 at room temperature in layers grown on GaAs substrates. The terminal surfaces of the epitaxial layers were examined by optical microscopy for structural characteristics. Laue back-reflection photographs (Cu radi-ation) were also made on the terminal surface to verify the epitaxial nature of the deposit. After these steps

Jan 1, 1970

By Maxwell Adams

OLIVER C. RALSTON, Salt Lake City, Utah.-We are indebted to these two gentlemen for the work which they have done with the oils derived from sage brush. Their work should not be confused, however, as the work of Mr. Adams deals with steam-distilled oils and that of Mr. Clevenger with destructively distilled oil, largely. In other words, Mr. Adams&apos; oil is probably the original essential oil that existed&apos; in the brush before distillation while Mr. Clevenger&apos;s oil not only contained this essential oil but also some products of destructive distillation of the wood constituents. I had noticed the work of Mr. Adams on attempting to separate the various constituents in the oils of some of the Western conifers and had sent to him to ask if he could send me small samples of some of. these pure products. This he very kindly did, and with them included some samples of oil from the common sage brush, whose characteristics he has here described, as well as a sample of oil from the common "rabbit brush." Only the sage brush oil proved of much value for flotation, but it, was very powerful, and I so informed Mr. Adams. Even in amounts as small or smaller than 1/10 lb. per ton of ore, it gave very quick and positive flotation of many ores, with high-grade concentrates and good extractions. It proved to be especially desirable for the flotation of carbonates of lead and of copper which had received an artificial coating of sulphide by treatment with a solution of a soluble sulphide. I also received a sample of crude pyroligneous acid from sage brush prepared by Dr. W. C. Ebaugh, of Salt Lake City. It did not do very good work in flotation, but it is possible that by concentration of this product to obtain the residual tar a good flotation oil might result. This has not been done as yet and I am sorry to see that Mr. Clevenger has not done this. It might be that the dissolved tar, added to the settled tar, would make a total yield of flotation oil higher than the 4 per cent. which Mr. Clevenger feels is a safe estimate. The importance of this point will be seen in the following discussion of the possible costs of sage brush oils for flotation.

Jan 10, 1916