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By Hans Schreiber

Launching a panel session isn't easy but after Associate Dean Howard Hartman from Pennsylvania State had made his statement, it was obvious that the balloon would go up. Hartman sees a crisis and gave its dimensions. Even with enrollments declining, there are not enough graduates being recruited by the mineral industry. Opportunities in the mining field are not attractive to youth in the face of competition from other disciplines. Nor will we be able to fill our ranks with good men from other engineering disciplines because they won't be attracted either. Salaries are too low. In 1966, mining engineers from Penn State averaged $660 per month starting. The average of all other engineers was $683 per month. The mining engineers ranked seventh out of nine disciplines. The bad image of the mineral field is created in part by industry which offers poor working conditions and inconsequential jobs and in part by the schools which have unimaginative curricula and poor teaching. Hartman called for immediate action and had his own set of solutions ready. "The gut of the problem is pay. Boost starting engineers $100 to $150 a month and older employees in commensurate manner. Compensate for poor working locations by better environment on the job." He did not fail to add that improvement of the public image of the mineral industry is needed. He called for elimination of all of the "schisms," or subdivisions of mineral industry curricula, and suggested a unified curriculum with a name such as "Geo-engineering."

Jan 4, 1967

By J. T. Mackenzie

HENRY MARION HOWE, in whose memory we are gathered together, was one of the great thinkers who develop from time to time to whom is given the rare gift of synthesis. Analysis is given to few, but synthesis, the ability to show the relation of all parts to each other and thus to give a clear picture of the whole, is reserved for the very few. Analysis can be achieved by honesty, intelligence, and industry, but synthesis is only given to genius Professor Howe's crowning achievement is the picture of the whole iron-carbon series shown in Fig. I, which places steel, malleable, gray iron, mottled and chilled irons in their proper relation to each other and shows the essential unity of the series. Perhaps his best statement of the case is found on page go of the Metallography of Steel and Cast Iron in these words: "Each member of the gray cast-iron series consists of the metallic matrix approximately equivalent to that member of the steel-white-cast-iron series to which it corresponds in percentage of combined carbon with its continuity broken up-by masses of graphite . . . " Apparently he had taken considerable interest in this idea around the turn of the century, for he refers to a discussion at the Franklin Institute in 1900 in which he said: "Though many others had probably conceived this relation between the steels and cast irons, it was here enunciated for the first time, so far as I know. It was received with great incredulity." The concept was explained in some detail in a paper on 'The Constitution of Cast Iron" presented before the A.S.T.M. in 1902 when Professor Howe was retiring president of that young society. In the discussion Dr. Sauveur stated that he was "very well acquainted with Professor Howe's theory of the constitution of cast iron," and went on to say that while he "shared it to the fullest extent, some foundrymen . . . claim cast iron is a metal entirely different from steel . . . that steel and cast iron have very little in common, and that therefore the knowledge gained in the study of steel is of little or no value in the study of cast iron." Dr. Moldenke, in discussing the same paper, said he had been working on the same theory for 12 years but he laid no claim to publication. Discussing the difference in the micro- structure of the metallic matrix, Professor Howe pointed out that "such minor struc- tural differences are indeed to be expected, because of the difference in the conditions under which these constituents are generated. "One difference in these conditions is that the steel of most micrographs has been either forged or at least treated thermally in such a way as to give a new structure radically different from that which formed during the initial solidification, whereas the cast irons have not. Hence what we see in the steels is a transformation structure, but in the cast irons a solidification structure. By giving the cast

Jan 1, 1944

(This list includes only those who have entered military service within the past month, or whose entry has only recently become known to us; it also includes a few names of those whose titles or assignments have been changed within the month. The last complete list was printed in Bulletin No. 131, November, 1917. A complete Honor List is maintained in the reception room at the office of the Institute.) ADAMS, HENRY, Captain, Asst. to Dept. Engineer, Northeastern Dept. BLAKE, EDWIN T., Captain, Corps of Engineers, U. S. R. CALDER, NORMAN L., Co. A., Y. W. D. Royal Engineers. CAMPBELL, CHARLES W., 2d Lieutenant, 312th Engineers. * See footnote on third page preceding.

Jan 12, 1917

By J. B. Umpleby

PRoduction engineering in 1927 may be characterized by a great. clarification of fundamental conceptions, and many improvements in technique. During the year the profession has received tnarked recogni-tion by the industry and to an extent never before attained has become an integral part of it. History Petroleum production engineering is a new profession. Prior to 1925, when this Institute undertook the work, no forum existed for the open discussion of its technical problems. There was no attempt at a handbook of the subject prior to "Petroleum Production Methods by J. R. Suman, in 1921, and no textbook prior to Petroleum Production Engineering" by L. C. Uren, in 1924. As late as 1926, only six schools and universities offered special courses in petroleum production engineering. Prior to about 1923, engineers engaged by oil companies were used almost exclusively for construction and location work. Two of the leading production engineers in the Mid-Continent field, although with their respective companies more than twelve years, were not definitely assigned to production work until 1924. Both men now head large departments giving almost their entire time to production problems. Because of the newness of the profession, the leading production engineers of today have had their fundamental training in mining, civil, mechanical and electrical courses. Not unlikely this diversified training is in considerable part responsible for the amazing growth of the profession. I believe, however, that recognition is due principally to economic pressure within the industry which has directed attention more and more sharply on costs and efficiency. After all, the justification for the growth and continued development, of the profession is to recover more oil from a given unit of sand at less cost per barrel. In this new profession, it seems to me that greatest progress will result from focusing thought and effort on this single objective, and if I might offer one suggestion to the com-

Jan 1, 1928

By C. H. Jr. Herty

DURING the past few years frequent reference has been made to a certain type of iron known generally as "bad iron," "dirty iron," etc., both by steelmakers and producers of iron castings.1 Open-hearth operators have claimed that such iron was entirely within the specified limits as to ordinary analysis but it was difficult to make good steel from it. It has been suggested that unreduced material in the iron is responsible, also that most trouble is experienced with the iron when the blast furnace is delivering a product whose analysis is more or less variable. Other reasons suggested are the use of scrap or borings, unsintered flue dust in the burden, a cold hearth, too high a proportion of unsuitable grade of ore, or the form of the carbon in the iron. Accordingly, a subcommittee was appointed at the fall meeting of the Open-hearth Committee of the American Institute of Mining and Metallurgical Engineers held in Pittsburgh in October, 1926, to investigate the reasons for the occurrence of this bad iron and suggest methods for preventing its appearance. This committee enlisted the cooperation of the U. S: Bureau of Mines Experiment Station at Pittsburgh in undertaking a study of pig-iron quality as affecting the open hearth. The following is a report of the findings to date:

Jan 1, 1929

By Paul Tyler

THE extensive employment of nonmetallic minerals antedates the use of metals, but only within the last two decades has the production of nonmetals begun actually to keep pace with the complicated activities which characterize the so-called Machine Age. The economic changes ushered in by the Industrial Revolution were reflected first in an increased demand for metals and for fuels. In the modern sense, therefore, the nonmetallic mineral industries are new and afford new opportunities for engineer and economist alike. A certain amount of caution is indicated, therefore, before attempting to apply ready-made formulas to the problems of these industries. Economics is not an exact science. In the field of production technology where the number of variables is fairly well known, the principles of economics are readily applicable, but as the student proceeds through the province of marketing into the unexplored regions of psychology and sociology he must distinguish carefully between scientific reasoning and purely metaphysical speculation, even when the latter masquerades as economics. The present paper attempts to prove no preconceived theorems and is designed primarily to stimulate careful thinking on sundry neglected phases of these industries. An attempt is made to differentiate the general problems into single aspects which afford promise of being comprehended separately; also, some fundamental statistical data are presented, but merely to indicate a method of scientific approach applicable to more intensive studies.

Jan 1, 1933

By Willard L. Hunter

Four solvent extraction systems were studied to determine their efficiency jor extraction and separation of tantalum and columbium. Aqueous feed solutions of varying HF-HCl concentrations and metal content were contacted with equal volumes of cyclohexanone, 3-methyl-2-butanone, and 2-pentanone and solutions of varying HF-H2S04 concentrations were contacted with equal volumes of 2-pentanone. One multistage continuous test was made in a polyethylene pulse column using cy clohexanone as the organic phase. In each system studied, columbium and tantalum purities in excess of 95 pct with respect to each other were obtained in single-stage tests at low acidities in the feed solution. Separation factors ranging from 1700 to 2400 were obtained when rising HF-HCl mixtures in the aqueous phase. Best results were obtained when a solution of HF-H2S04 was used as the aqueous phase and 2-pentanone as the organic phase. A separation factor in excess of 6000 was obtained in one stage with aqueous solution concentrations of 2 _N HF and 2N H2S0,. When acid concentrations were increaszd to 52 HF and 10 _N H2S0,, 99.9 pct of the tantalum and 98.2 pct of the columbium initially present in the feed solution were transferred to the organic phase. The separation of columnbium and tantalum obtainable by means of the solvent extraction systems presented in this paper was found to corn -pare favorably with other systems, including the HF-H2SO4-methyl isobutyl ketone system currently used by most producers for the extraction and separation of these metals. TANTALUM and columbium are always found together in minerals of commercial significance, although the proportion of the two metals in ores varies within broad limits. Columbium is estimated to be 13 times more abundant than tantalum. Five methods generally employed for the separat:ion of these metals are: 1) fractional crystallization (the Marignac process),2 2) solvent separation, 3) fractional distillation of their chlorides, 4) ion exchange, and 5) selective reduction. Of these methods, the one currently used by industry to the greatest extent is that of solvent separation. One of the early technical developments in solvent separation of tantalum from columbium was reported by the Bureau of Mines: the HF-HC1-methyl isobutyl ketone system; data were presented for both laboratory and pilot-plant experimentation.3 Of twenty-eight organic solvents tested for their ability to extract tantalum from an HF-HC1 solution of columbium and tantalum, 3-pentanone (diethyl ke-tone), cyclohexanone, 2-pentanone, and 3-methyl-2-butanone were chosen for further study. Data on the HF-HC1-diethyl ketone system has been published4 and data describing the use of cy clohexanone, 2-pentanone, and 3-methyl-2-butanone as the organic phase are included in this report. RAW MATERIAL The source of tantalum and columbium oxides for this study was ('Geomines" tin slag from the Manono Smelter, Cie Geomines, Gelges, S.A., Congo. In order to extract the valuable Ta-Cb content, the slags were carbided, chlorinated, and the sublimate from chlo-rination was hydrolized and washed free of chloride with water. The washed material was air-dried and stored in a stoppered container. Throughout the paper, "feed material" refers to this mixture of hydrated oxides which was employed because of its high solubility in aqueous solutions. Typical analysis of the hydrated oxides is shown in Table I. I) HF-HC1-CYCLOHEXANONE SYSTEM Batch Separation. Effect of Acid Concentration. To determine the effect of varying the acid concentration upon the transfer of tantalum and columbium, a series of tests was made in which approximately 2.5 g of feed material was added to 25 ml solutions of 2, 4, 6, 8, and 10 N HF and 0 through 5 N HC1. Tantalum pentoxide concentration of the solu%ons was approximately 21 g per liter and columbium pentoxide was 14 g per liter. These starting solutions were shaken with equal volumes of cyclohexanone in 100 ml polyethylene bottles for 30 min. The phases were carefully separated in 125 ml glass separatory funnels. The time of contact of the solutions with the separatory funnels was kept at a minimum to reduce silica contamination. The measured phases were separated into 400 ml polyethylene beakers and the metal contents of each were precipitated by addition of an excess of ammonium hydroxide. Precipitate from each phase was filtered on ashless filter paper, ignited at 800" to 1000°C for 45 min, weighed, and analyzed by X-ray fluorescence.5 Data tabulated in Table I1 and illustrated in Fig. 1, show that maximum separation of tantalum from columbium for each HF concentration was obtained with no HCl present. The purest tantalum product was obtained with some HCl present. The highest separation factor was obtained at 2 N HF and

Jan 1, 1970

Past-president Philip N. Moore has accepted the position of engineer member of the War Mineral Relief Commission and has already taken up the work. J. E. Spurr is the chief engineer of the Commission and is now organizing the examining staff.

Jan 4, 1919

By A. C. Dorenfeld

In most mineral enterprises, what is the progress, and shift in responsibilities, as the young engineer advances in the corporation? You are all familiar with the normal pattern-in mine production from level boss, to shift boss, to superintendent to manager; in milling from test engineer, to shift boss, to foreman, to superintendent and then manager; in engineering from surveying on to Chief Engineer; and all then aspire to the corporation presidency. Note the shift-from purely technical jobs, say in the first five to ten years in the profession, to administrative positions for 30 to 40 years. What is the average preparation given to mineral engineering students, who can look forward to about 30 years of administrative work? From the catalogs of 21 institutions, offering 36 curricula of four years length, in mining and/or metallurgy, requiring the equivalent of about 150 to 160 semesterhours for graduation, the following results were obtained: Average number of semester hours of economics, 3 hr. Range of requirements, 0 to 8 hr. Thirteen curricula do not require any economics. Accounting and business law, average: 1 semester hr, 26 curricula do not require business law or accounting.

Jan 2, 1955

By J. O. Betterton, D. S. Easton

A detailed investigation was made of the phase diagram of silver-zirconium, particularly in the region 0 to 36 at. pct Ag. The system was found to be characterized by two intermediate phases Zr2Ag and ZrAg and a eutectoid reaction in which the -zirconium solid solution decomposes into a-zirconium and Zr2Ag. It was found that impurities in the range 0.05 pct from the iodide-type zirconium were sufficient to introduce deviations from binary behavior, and that with partial removal of these impurities an increase in the a-phase solid solubility limit from 0.1 to 1.1 at. pct Ag was observed. The phase diagram of the silver-zirconium system is of interest as an example of alloying a transition metal from the left side of the Periodic Table with a Group IB element. Silver would normally act as a univalent metal, its filled 4d-shell remaining undisturbed during the alloying. However, there is a possibility that some of the 4d electrons might transfer to the zirconium. An insight into such a question can occasionally be obtained by comparison of phase diagrams. The silver-zirconium system forms part of a more complete review of various solutes in zirconium in which these valency effects were studied.' Earlier work on the silver-zirconium system was done by Raub and Enge1,2 who investigated the silver-rich alloys. After the start of the present experhents, work on this system was reported by Kemper3 and by Karlsson4 which for the most part agrees with the phase diagram presented here. EXPERIMENTAL PROCEDURE The alloys were prepared by arc casting on a water-cooled, copper hearth with a tungsten electrode and in a pure argon atmosphere. Uniform solute composition was attained by multiple melting on alternate sides of the same ingot. Progressive improvements in the vacuum conditions inside the apparatus during the course of the experiments reduced the Vickers hardness increase of the pure zirconium control ingot from 10 to 20 points, observed initially, to negligible amounts at the end of the experiments. Such hardness changes in zirconium are a well known indication of purity. For example, -01 wt pct additions of oxygen, nitrogen, and carbon increase hardness by 6, 10, and 3 VPN respectively. '9' Further verification that the final casting technique did not add a significant quantity of impurities was obtained when pure zirconium was arc cast and then isothermally annealed in the vicinity of the allotropic transition. The transition was always observed to take place over the same temperature range as in the original crystal bar. The alloy ingots were annealed in sealed silica capsules for times and temperatures which varied between 1 day at 1300°C and 60 days at 700°C. The best method found to prevent the reaction of the zirconium with the silica was foil wrapping of molybdenum or tantalum. With this method, samples of pure zirconium were found to be unchanged in hardness after annealing for 3 days at 1200°C. In most of the experiments the protection of these foils was supplemented by an additional layer of zirconium foil inside the molybdenum or tantalum foil. The alloys, foil, and the capsule were outgassed at pressures in the range 10 to l0-7mm Hg in the temperature range 800" to 1100°C before each anneal in order to remove hydrogen and other impurities, and to provide a suitable container for the high purity, inert atmosphere, which is essential in the annealing of zirconium. The temperature measurements were made with Pt/Pt + 10 pct Rh thermocouples calibrated frequently during the experiments against the melting points of zinc, aluminum, silver, gold, and palladium. For the longer anneals the sum of various temperature errors was generally well within ± 2°C. For short-time anneals and during thermal analysis the overall temperature error is considered to be within ± 0.5°C. The compositions of the alloys from the quenching experiments were determined by chemical analysis at Johnson Matthey and Company, Ltd., under the direction of Mr. F. M. Lever. The actual metallo-graphic samples were individually analyzed in every case, and prior to the analyses two or more sides of each specimen were examined to insure that the specimen was not segregated. The sum of the solute and solvent analyses was in each case within the range 99.9 to 100.1 pct. In the course of the experiments, minor impurities in the range 0 to 500 ppm were found to have significant effects on the zirconium-rich portion of the phase diagram. Similar effects had been encountered previously in other zirconium phase-

Jan 1, 1959

In many lines of engineering, much excellent standardization work had been done before the war but the war emphasized its importance and showed most clearly the need of cooperation to prevent the confusion caused by the promulgation of overlapping standards by independent bodies. The American Institute of Mining and Metallurgical Engineers, American Institute of Electrical Engineers, American Society of Civil Engineers, American Society of Mechanical Engineers, and American Society for Testing Materials, recognizing the value of what had been done, invited the Government Departments of War, Navy and Commerce to appoint representatives to act with them to continue this work; the body so formed is the American Engineering Standards Committee. It has required time to definitely formulate its objects and to arrange methods for accomplishing them that would be effective without interfering with the many organizations that have been doing such excellent work in this line. The American Engineering Standards Committee has just completed and adopted a revision of its Constitution, which has been sent to the Governing Boards of all the Departments and Societies represented on the Committee with a request for its ratification. The new Constitution changes the name to American Engineering Standards Association as more fittingly indicating the wide scope of the interests involved. The objects of the association are stated as follows: 1. To unify and simplify the methods. of arriving at engineering standards, to secure cooperation between various organizations and to prevent duplication of standardization work. 2. To promulgate rules for the development and adoption of standards, 3. To receive and pass upon recommendations for standards submitted as provided in the Rules of Procedure, but not to initiate, define, or develop the details of any particular standard. 4. To act as a means of intercommunication between organizations and individuals interested in the problems of standardization. 5. To give an international status to approved American engineering standards. 6. To cooperate with similar organizations in other countries and to promote international standardization.

Jan 7, 1919

By AIME AIME

THIS year's Chairman of the Mineral industry Education Division is, like his predecessors, no novice in that field, having been in 1928 Chairman of the Engineering Education Committee which labored so well that it was enlarged into a Division of the Institute's activities . For almost a quarter of a century lie has been a dean in mining and engineering schools, with considerable experience before that as a teacher. A native-born New Englander (June 23, 1881), he naturally went to Massachusetts Institute of Technology where he received the Bachelor's degree in mining in 1904. Just why a Fitchburg. Massachusetts boy yearned to he a mining engineer he has never explained, but why should any boy ever have to explain why lie wants t? be a mining engineer? Like the old rhyme about the reasons why a man should drink, "any other reason why" is adequate..

Jan 1, 1945

By HERRBERT HOOVER

I AM glad to join with my fellow-members in this celebration of the fiftieth anniversary of the founding of the American Society of Mechanical Engineers. It would be a difficult task to measure the blessings brought by this association through the stimulation to invention, the improvement of methods, the adequate training of engineers and the advancement of knowledge in a large sense. During its span of life it has contributed a great part in the development of an art into a mighty profession upon whose capacity and fidelity rest so much of human progress. "I feel especially honored that the association should, through the beneficence of Mr. Lauer, have established a new distinction among engineers, and should have designated me as its first recipient. The purpose of this medal is to mark the public service of men who have gone outside their strictly professional work to interest themselves in civic and humanitarian affairs. And the engineers have something to contribute to public service. . "With the development of our great national tools -our engines, our railways, our automobiles, our airplanes, our steamships, our electric power and a score of other great implements, together with the supplies of material upon which they depend-the engineer has added vastly to the problems of government, for government must see that the control of these tools and these materials is not misused to limit liberty and freedom, that they advance and do not retard equality of opportunity among all our citizens.

Jan 1, 1930

By C. R. Whitney, G. N. Maniar, D. R. Muzyka

Previous results have shown that Pyromet 860, an Fe-Ni-base heat-resistant alloy, is stable at temperatures as high as 1500°F for aging times as long as 100 hr. This Paper describes the results of long-time creep-rupture testing at 1050" to 1400°F at various stress levels. Times as long as 37,660 hr were employed. The effects of time, temperature, and stress on the precipitates and their morphologies were studied by optical and electron microscopy, X-ray and electron diffraction, and microprobe techniques. phase, containing cobalt, nickel, and molybdenum, was detected after extended exposures from 1200" to 1400°F and careful study was performed to describe the kinetics of its formation in this alloy. µ phase formation apparently has little effect on the elevated-tem-perature properties of Pyromet 860. For times as long as 500 hr at 1300°F and below, with µ phase present, m significant effects on ambient temperature properties were noted. For longer times at 1300°F and after 1400°F exposure, the effects of u phase on ambient temperature tensile strength properties are not clear due to y' effects and grain boundary reactions. Electron-vacancy, N,, numbers were calculated using different methods described in literature and correlated with the present findings. In the selection of alloys for use in gas turbine applications, structural stability ranks as a primary criterion. High-temperature strength and cost are also of major concern. With these factors in mind, Pyromet 860 alloy, an Fe-Ni-base superalloy was designed. This alloy combines the cost advantages of Fe-Ni-base alloys such as A-286, 901, and V-57 with improved strength and structural stability'1,2 and no tendency to form the embrittling cellular 77 phase. A previous study3 reported on the stability of Pyro-met 860 at temperatures from 1375" to 157 5°F and times up to 100 hr. That study showed that the y' precipitates increased in size and separation and decreased in number with an increase in time or aging temperature. No deleterious phases were found to occur. In the present work, samples from four production heats were subjected to long-time creep-rupture testing at 1050" to 1400°F at various stress levels. Various heat treatments were used on the starting samples and tests were run up to 37,660 hr. The effects of time, temperature, and stress on the precipitates and their morphologies were studied by optical and electron microscopy, X-ray and electron diffrac- tion, and microprobe techniques. Electron vacancy numbers, Nv , calculations were made by TRW.4 Experimental results are correlated with the Nv data used to predict occurrence of intermetallic phases such as a phase. EXPERIMENTAL PROCEDURE Mechanical Tests. Material for the present study came from four production size heats of Pyromet 860 alloy, weighing from about 3000 to about 10,000 lb. All of these heats were made by vacuum induction melting plus consumable electrode vacuum remelting. The nominal analysis for this alloy is compared with the actual analysis of the four heats in Table I. Sections of these heats were forged to 9/16-in. round bar,3/4-in. square bar, 3-in. round bar, 4-in. square bar, and a gas turbine blade forging about 16 in, long, about 6 in. wide, and weighing about 20 lb. In general, all forging of this alloy is done from a 2050°F furnace temperature. Longitudinal test blanks were cut from the centers of the smaller bars, from mid-radius positions for the 3- and 4-in. bars, and from the air foil of the gas turbine blade and heat-treated according to the procedures outlined in Table 11. Heat treatment A is the "standard treatment" recommended for this alloy for best all-around strength and ductility. Heat treatment B is a modification of treatment A for improved tensile strength at moderate temperatures. The treatment coded C was designed for treating large sections according to a procedure previously described.' Heat treatment D was developed to yield optimum stress relaxation characteristics at 1050°F for a steam turbine bolting application. After heat treatment, the test blanks were machined either to plain bar creep specimens with a gage diameter of 0.252 in., to combination smooth-notched stress-rupture bars with a plain bar diameter of 0.178 in. and a concentration factor of Kt 3.8' at the notched section, or to notch-only specimens. All specimens conformed to ASTM requirements. Metallography. Most of the creep-rupture tests were continued to failure. A few bars were fractured as smooth or notch tensiles after creep-rupture exposures. After fracturing, ordinary metallographic sections were made primarily in gage areas adjacent to fractures to represent a "high-stress" region and through specimen threads to represent a "low-stress" region. All metallographic sections were made in a longitudinal direction with respect to the test specimen axes. For optical microscopy, the samples were etched in glyceregia (15 ml HC1, 5 ml HNO,, 10 ml glycerol). For XRD analysis, the phases were extracted electrolytically in two media: 20 pct &Po4 in H20 for selective extraction of y' and 10 pct HC1 in methanol for carbides and other phases.

Jan 1, 1970

By S. G. Cupschalk, F. A. Dahlman, J. J. Wert

Studies have been undertaken to determine the indicidual effects of particle size, degree of long-range ovder, antiphase domain size, and root mean square stran on the microhardness and yield strength of ordered alloys. Dnta have been analyzed for Cu3Pt initzally ordered to a value of 0.82 and after deformations of 1 and 6 pct. It was observed that deformation fleatly reduced the degree of long-range order. Furtherrnore, wztkin this range of relatively small deforntntlons, the average particle size changed very little while the antiphase domain size was greatly reduced. Smultaneosly, the mcrohardness changed by a factor of two durzng the deforrtation process. PREVIOUS studies have reported some of the effects of cold work on the broadening of X-ray diffraction peaks. These investigations were performed on powder and wire samples representing both ordered and disordered states; i.e., the specimens were initially studied in a severly cold-worked condition. By comparing the difference in line shape between the annealed and cold-worked peaks, fundamental information was obtained concerning particle size, strain distribution in different crystallographic directions, degree of long-range order, and change in antiphase domain size. Considerable theoretical work has been done concerning the analysis of diffraction data obtained from cold-worked metals. Stokes' expressed the change in diffraction profiles in terms of Fourier coefficients. Much of the work in this area has been summarized by warren2 in an extensive review article concerning the analysis of plastic deformation by X-ray diffraction. Cohen and Bever3 applied these techniques in studying the effects of cold work on alloy systems exhibiting long-range order. They utilized the Fourier coefficients of fundamental peaks in conjunction with those of the superlattice peaks to determine the change in antiphase domain size. Little work of this nature has been reported for ordered systems that have undergone small degrees of plastic deformation. The purpose of this investiga-tion was to determine the effects of small deformations in such a material with respect to particle size, strain distribution in various crystallographic directions, antiphase domain size, degree of long-range order, and hardness. EXPERIMENTAL PROCEDURE CusPt was used for the initial investigation since the order-disorder transformation takes place with- out a change in crystal structure. The transformation is readily detectable via X-ray diffraction techniques due to the large difference in the scattering factors of copper and platinum. Additionally, the alloy is relatively low melting (approximately 1300°C) and is easily deformable in both the ordered and disordered states. 1) Specimen Preparation and Cold Working. A 100-g, 12-in. diam., cylindrical specimen of Cu3Pt was prepared by melting and casting 99.99 pct pure Cu and Pt i.n vacuo. Prior to any mechanical working, the material was homogenized in a vacuum for 60 hr at 100O0C, and surface defects were removed by machining to a depth of approximately 116 of an in. The material was then cold-rolled, with an intermediate anneal, into a strip approximately 12 in. wide by 14 in. thick. Straightening and flattening removed another 0.025 in. from the thickness. After a recrystallization treatment at 750°C for 30 min, the specimen was slow-cooled from 55OoC, at the rate of 6°C per hr, down to 150°C to induce superlattice formation. This treatment yielded an ASTM grain size of 7 and a degree of long-range order equal to 0.83 0.06. After obtaining X-ray and Knoop hardness data, the sample was cold-rolled approximately 0.75 pct in one pass through a hand-operated jewelers' mill. X-ray and hardness data were again obtained and the specimen was reduced an additional 5.41 pct in a single pass through the mill. 2) X-Ray Measurements. The specimen was examined in the ordered condition and after the two degrees of cold working previously mentioned using a General Electric XRD-5 unit equipped with a spectrometer and scintillation counter. Using Mo-Ka radiation with a zirconium filter, six orders of the 100 reflection were obtained. It was anticipated that point counting would be necessary for an accurate determination of the low-intensity peaks and tails: however, it was demonstrated that, by using a scanning speed of 0.2 deg per min and the appropriate time constant, the recorded data were sufficiently accurate. Thus, for ease of experimental procedure, all peaks were recorded on chart paper. Specimen position in the holder was considered to be insignificant after making a series of measurements of the same peak area in different positions with respect to the beam. Since peak overlapping did occur at high values of 20, it was necessary to separate the peaks graphically prior to analyzing the data in order to minimize this source of error. The peak tails were also carefully drawn to obtain the best possible data. Fourier coefficients of the line profiles were calculated on an IBM 7072 computer, and graphical meth-ods2j3 were employed in analyzing the results. For this type of calculation, in which the line profile is represented by intensities taken at set intervals, the intervals selected must be sufficiently small to give an accurate representation of the line profile. It was decided that for 20 = 0.02 deg the line profiles were

Jan 1, 1967

By Karl A. Bauer, Cornelis Bezemer

The deposition of calcium carbonate scale on surface and subsurface production equipment creates an operation problem in many oil fields. The formation water in which the carbonate-scale-forming components are initially dissolved becomes supersaturated with calcium carbonate as a result of the drop in pressure during production. The continuous flow of a supersaturated solution through the production equipment results in the growth of a dense layer of calcium-carbonate crystals. For a scale layer to be built up, the supersaturated formation water should contact the walls of the production equipment. The tendency for scale to be deposited, therefore, will be low, if the crude has a low water cut and if the water is finely dispersed in the oil. A scale problem will occur, if at a high water cut part of the water is present as free water. The rate of scale deposition will then be approximately proportional to the rate of free water production. Depending upon where the formation water becomes supersaturated, scale may be deposited in the flow line only, in both flow line and tubing, and in some cases even in the perforations and in the formation near the wellbore. In the South Sumatran fields (Indonesia) the main difficulties encountered due to the deposition of calcium-carbonate scale have been restriction of flow through tubings and flow lines, wear and abrasion of plungers and liners, and stuck plungers or wellhead valves. So far, the only methods of combating the *Presently associated with Brunei Shell Petroleum Co., Ltd.. Seria. scale problem have been routine acidizing and additional well pulling. As for the pumping wells, it was estimated that some 50 percent of the total well-pulling effort was directly attributable to scale deposition. The most promising alternative was to prevent the deposition of calcium carbonate scale by means of chemicals. Inorganic polyphosphates such as sodium hexametaphosphate and trisodium polyphosphate are known to retard the formation of scale by the "threshold action". They are adsorbed on specific faces of the crystal nuclei and thus prevent crystal growth, thereby stabilizing supersaturation. Polyphosphates are effective at very low concentrations ( a few ppm), and far less than stoichiometric quantities are required to keep the scaling ions in solution. Recent investigations on barium sulfate scale1 have confirmed this mechanism. The types of polyphosphate mentioned can be applied as concentrated aqueous solutions either squeezed into the formation, lubricated down the annulus or injected via macaroni string. Several squeeze jobs with polyphosphate solutions have been carried out in the South Sumatran fields, however, with disappointing results. Lubrication down the annulus and injection through a macaroni string were not considered attractive in this area because of the kind of equipment and the degree of supervision these techniques require. Polyphosphates are also available in a granular, glassy form, which, in contrast with the readily soluble types already mentioned, show an extremely low

Jan 1, 1970

By Don M. Jackson, Robert W. Howard

Techniques for the epilaxial growth of single -crystal silicon carbide films on silicon were developed. The vapor-phase decomposition and bydrogen reduction of silicon tetrachloride (SiC14) and Propane (C3H8) resulted in clear films of silicon carbide, lip to seveval microns in thickness. The growth took place in a horizontal . silicon epilaxial reactor at 1100°C (pyrometer) at a rate of- 3000Å per minute. Electron diffraction and X-ray diffraction studies demonstrated that the films were single-cyrstal, ß -phase, or cubic silicon carbide. SiO2 film were used to mask areas of the silicon sur-lace in order that the silicon carbide might be grown in controlled geometries. Both n- and p-type films were grown on p-type silicon waters.. Heavily doped silicon films of the same conductivity type as the silicon carbide films were deposited over the silicon carbide in order to affect better probe contact to the structures. when n-type silicon carbide mesas were grown on p-type silicon substrates the de vollage-current relationships between films and substrates were that of junction diodes. These diodes showed a sensitivity to while light ill that the incident light increased forward- and reverse-satro,ation currents, P-type silicon carbide mesas grown on p-type silicon were ohmic rather than rectifying in their voltage -current relationship. No conclusions could he reached concerning heterojunc-tiou rectification in the structure. SILICON carbide is a semiconductor with many interesting properties. It decomposes at temperatures above 2200°C.1 It occurs in two general crys-tallographic forms—hexagonal (a Sic) and cubic (ß Sic)—with the cubic form having a forbidden-gap energy of 2.32 ev and the hexagonal form (specifically the 6H polytype) a gap energy of 2.86 ev.3 It behaves as an extrinsic semiconductor at temperatures approaching 5003C. It has been shown to have a high resistance to radiation damage4 and p-n junctions formed in Sic have been shown to radiate visible light under forward- or reverse-bias conditions. Epitaxial silicon carbide on silicon carbide has been successfully grown through the use of a variety of techniques, such as gaseous cracking of SiCL4 and CC4, nearly all of which require a deposition temperature above 1500°C.6 This paper will cover very recent work on the gas-phase deposition of highly ordered films of silicon carbide on high-quality silicon single-crystal substrates. The films have been shown to ex- hibit junction-rectification properties when geometrically isolated regions are electrically biased with reference to the silicon substrate. There will be no discussion of the mechanism of heterojunction rectification, but the methods of film fabrication, geometry control, and structural evaluations will be covered in detail. Electron diffraction, X-ray diffraction, and diode electrical properties were used to characterize the films and the junctions. GAS-PHASE DEPOSITION OF Sic The techniques for the deposition of silicon carbide films were a logical outgrowth of the standard silicon epitaxial process. The major premise followed was that, for any film to nucleate in an ordered fashion where there is considerable mismatch in lattice parameters (in this case 22 pct), an extremely clean, damage-free substrate surface must be presented to the gas stream. Thus a standard gas-phase HCl etching step was used to prepare the substrates for growth. A minimum of 5 µ of substrate-surface material was removed prior to the deposition of Sic overgrowth films. The techniques used for growing silicon carbide films were those of growing silicon alone, with the added injection of a hydrocarbon gas into the hydrogen and silicon tetrachloride gas stream. The hydrocarbon gases used thus far have been research-grade (99.99 pct) methane (CH4) and propane (C3H8). Propane ultimately gave the best results. The gas flows were controlled through a panel shown schematically in Fig. 1. A hydrogen main stream of 30 liters per min passed through the horizontal quartz-tube epitaxial reactor, while SiC14, C3H8, HC1, and doping gases were injected as side streams. The

Jan 1, 1965

By G. K. Manning, E. R. Stein, E. E. Underwood

Columbium, carbon. and nickel additions were made to iron-base alloys with 20 pct CY. The effects on microstructure, precipitation-hardening characteristics, and High-temperature properties were investigated by means of metallographic, hot-hardness, and magnetic measurements. An austenitic alloy consistilzg of Fe-20Cr-14Ni-0.8C-2.5Cb had higher hot-lzaciness at 1700°F than the other alloys investigated. Its favorable standing is attributed to an enhanced interaction of Cb and Cr4C particles dispersed within a stable austenitic matrix. FOR the past 20 years, cobalt- and nickel-base alloys have been used for the more stringent high-temperature applications because of their excellent creep resistance. Although their performance is quite satisfactory, other base materials must be considered for large tonnage, low-cost applications such as for the automotive gas turbine. Iron-base alloys are also used extensively, but at somewhat lower temperatures, primarily because of the instability of particles or because precipitation occurs at relatively low temperatures. Since unusual stability has been reported for Fe-Cb and Cb-C compounds.1-3 it was hoped that effective amounts of these compounds could be taken into solution at temperatures just below the melting range, then precipitated upon reheating. Actually, strengthening was found to occur by both precipitation hardening in some alloys and by phase transformations in others. Among the alloys investigated, that with the best high-temperature properties owes its strengthening to a combination of carbide particle interaction and a relatively stable austenitic matrix. EXPERIMENTAL PROCEDURES Small preliminary melts of about 100 g were made in a vertical Glotube furnace, using alundum crucibles and an argon atmosphere. Alloys weighing 35 lb were melted in a basic-lined induction furnace, also under argon. The compositions of the alloys are given in Table I. The nickel-free alloys were usually ferritic, while those containing nickel were generally austenitic. Depending upon the particular heat treatments, or the combination of alloying elements, two-phase alloys of ferrite and austenite could be obtained. In the following text, however, the nickel-free or nickel-bearing alloys are referred to simply as either ferritic or austenitic alloys respectively. The small ingots were swaged at 2000°F, in steps, to rods of approximately 3/16-in. diam. The large ingots were forged at 2100°F to 1-in. sq bars. No difficulties were encountered in swaging or forging any of the alloys to as much as 90 pct reduction in area. For heat treating at temperatures above 2000°F, specimens were sealed in quartz tubes under a partial pressure of helium. No special precautions were found to be necessary at lower temperatures. Intermetallic compounds in the preliminary alloys were identified by means of X-ray diffraction measurements. Correlation of these results with micro-structural characteristics (such as color, shape, size, and location) of the compounds aided in their identification. Magnetic susceptibilities were also obtained at room temperature with a Magne Gage instrument after the various heat treatments. To

Jan 1, 1962

By Cyril Stanley Smith

THE art of metallography is mature and the forms in which various micro-constituents appear are well known. Investigations almost without end have disclosed the importance of the exact manner of distribution of phases on the physical properties and usefulness of an alloy. Surprisingly, however, relatively little attention has been paid to the forces that are responsible for the particular and varied spatial arrangements of grains and phases that are observed. Like the anatomist, the metallurgist has been more concerned with form and function than with origins. In this paper it is proposed to develop the simple concept that many microstructures result from an attempted approach to equilibrium between phase and grain interfaces whose surface tensions geometrically balance each other at the points and along the lines where they meet. From this follows a number of principles which may prove to be of interest to the metallographer and of practical use in explaining failures and in designing alloys for particular service. In general, the discussion will be limited to structures obtained after full annealing. The simple principles do not apply to structures resulting from Widmanstatten mechanisms in precipitation, or to other structures not in local equilibrium and in which lattice coherency is a determining factor. INTERFACIAL TENSION Much has been written by physical chemists about the free energy of surfaces, which manifests itself as a measurable surface tension. Two- and three-phase interfaces in fluids seek a condition of minimum energy and approach a geometrical configuration in which the various forces are in vectorial balance.* Measurement of the angles established between the interfaces when in equilibrium provides a quantitative value for the relative value of the surface forces involved. The case of two fluids meeting at the surface of a solid (of great importance in connection with the flotation of minerals) has often been studied, but there have been few investigations of the equally definite interface between two or more crystals of a single solid phase, or the more complex cases where crystal grains of more than one phase are involved. The principles are best illustrated by considering first the case of two and three immiscible liquids. If, as in Fig I, a liquid, 2, is dropped into a less dense liquid, I, it will form a sphere-if gravity and viscosity can be ignored-for in this shape the interface has the smallest possible area. If these two phases should together encounter a third phase in which they are both immiscible, the geometry will change to become that which gives the lowest total energy for all three interfaces. Thus, if the spherical drop of liquid, falling through r, eventually reaches the interface between liquids 3 and I (we are assuming that the density of 3 is greater than 2, and 2 than I), it will assume the shape of a lens, the angle

Jan 1, 1948

By Eldon N. Dunlap

Recently the producing branch of the petroleum industry has shown a considerable and growing interest in the quantitative determination of the water, oil, and gas content of cores as it relates to estimation of reserves, to providing a basis for judging as to the feasibility of applying various secondary-recovery and pressure-maintenance processes, and in general to the operation of producing properties. For years it has been known that oil, gas and water coexisted in the pores of many semidepleted oil measures. It is now generally believed that oil-bearing beds contain connate water in amounts varying up to 50 per cent of the pore space. However, only lately has reliable direct evidence of the extensive occurrence of connate water in oil sands been published. Very little work has been done to ascertain the effect of this water on the productivity and ultimate recovery of oil from wells. It was the intent of this research to study the influence of interstitial water on the flow of oil through unconsolidated sands, with the hope that the results could be applied qualitatively to the flow of oil in underground reservoirs partly saturated with water. Obviously, ultimate recovery estimates based on the void volume of the reservoir will be in error unless a correction is made for the volume of water that occupies a portion of the effective pore volume of the reservoir. Evaluation engineers in the past have applied arbitrary saturation and recovery factors that may inadverently have compensated for the failure to consider specifically the water content. Nevertheless, the evidence available indicates that these factors need revising if each is to be independently correct and truly representative. Although the fact that the connate water renders part of the pore volume of the reservoir incapable of containing oil is of primary importance to the operator, it is also to his interest to know to what extent the presence of varying amounts of interstitial water influences the permeability of the sand to oil.

Jan 1, 1938