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By Koichi Kashida, Mayumi Someno, Kazuhiro Goto

The present work has two objectives: first to develop an experimental method which would give some new information on the micromechanism of the reduction of oxides by gases at elevated temperature; second to clari,fy the intermediate phases of the W-0 system, formed during the reduction. A Galvanic cell with the solid electrolyte , ZrO2 . CaO, was imbedded in powders of W03, CuO, or Fe20s with two measuring electvodes and with a reference electrode. The change of the intraparticle gas composition was measured at An oxygen concentration cell consists of two electrodes separated by an electrolyte through which the transference of electrical charge is accomplished predominantly by the migration of oxygen ions. Many works have been reported on the oxygen con- 600" to loo@ C during the reduction by the gas mixture of hydrogen and argon. The intraparticle gas composition changes stepwise with time. The electromotive force of such temporary interruption corresponds to the equilibrium electromotive force of two solid phases formed during the reduction. The intermediate phases of W-0 system, which are formed in a large quantity during the reduction by hydrogen, are W0 2 W02.72 and WOz. The micromechanism of the reduction of oxides by gases is discussed. centration cells with the solid electrolyte of solid solution of zirconia and lime, since Kuikkola and wagnerl demonstrated the possibility of determination of standard free energy of formation of oxides by an electromotive-force method with the Galvanic cell. One of the present authors (K.G.) and his coworkers have applied the cells with the solid electrolyte of zirconia and lime to the following measurements:

Jan 1, 1969

By J. H. Bechtold, R. Kossowsky

1 HE superplastic behavior of the eutectoid A1-78 wt pct Zn alloy has been thoroughly investigated by Back-ofen et al.' The superplastic elongations and the marked resistance to necking were rationalized in terms of high strain rate sensitivity. In a subsequent paper2 superplastic behavior was formulated to show Nabarro-Herring diffusional creep as rate controlling at low strain rates, giving way to a dislocation climb process at higher strain rates. In a paper devoted to an interpretation of superplasticity in two-phase alloys, Packer and sherby3 have included the results of an examination of the structure of an Al-Zn eutectoid specimen before and after superplastic deformation. No significant change in grain size or directionality was observed in the deformed microstructures. This one observation led the authors3 to suggest that con- tinuous recrystallization or grain boundary migration was responsible for superplasticity. The purpose of this note is to report our observations on the superplastic behavior of the Al-Zn eutectoid alloy which differ in certain respects from works previously reported. Following Hayden et al., the results are discussed in terms of dislocation climb as the important factor during superplastic deformation. A heat of nominally high (99.995) purity 22 wt pct A1-78 wt pct Zn was induction-melted and cast into a 0.5 by 6 by 12 in. slab. The slab was heated to 350°C and rolled to 1/8-in.-thick plate. The plate was then cold-rolled to 0.040-in. thickness, annealed at 35OaC, and rolled to the final thickness of 0.020 in.* Speci-

Jan 1, 1969

By Adolf Gurlt

It has long been known that minute quantities of foreign substances, when alloyed with steel, are capable of materially altering its physical properties. Thus, half a century ago, Faraday and Stodart, in England, discovered in the famous Indian steel, known as " wootz," small quantities of aluminum, from 0.0728 to 0.693 per cent., and attributed its extraordinarily good quality to the presence of such minute quantities of that metal. Since aluminum is now produced by electrolytic means on a large scale and at low cost, its addition to cast-steel has been frequently recommended of late. Chromium was alloyed with steel fifty years ago by the celebrated French metallurgist, Berthier, of Paris, and has recently been successfully applied to the same purpose by Holtzer, of Terre-Noire. In 1860 titanium was alloyed with crucible steel by Robert Mushet, of Coleford, the alloy containing up to 0.50 per cent. of titanium, which was extracted from Norwegian ilmenite. The titanium-steel was much vaunted by him for its excellent qualities. Rhodium, a very rare metal of the platinum series, was maintained by Berthier to improve steel materially in strength and hardness. Manganese has always been held by Sheffield steel-melters to provide steel with excellent qualities, and this influence was quite recently investigated by H. M. Howe and L. Campredon. Nickel was tried as an addition by Berthier, not to speak of gold, silver and platinum ; and nickel-steel has recently been brought into prominence by J. Riley and others, who recommend it for its great strength and toughness, particularly as material for armor-plates.

Jan 1, 1894

By D. B. Smith, John Chipman

THIS investigation was undertaken as a prerequisite to the study of sulphur activities in the liquid system Fe-Cu-Ni, a continuation of the work of Sherman, Elvander, and Chipman,¹ using the same equipment and the same experimental technique. Temperature measurements are made with a disappearing filament optical pyrometer, sighting through a prism onto the surface of the melt which is heated by induction. To obtain true temperatures by this means, a calibration is necessary, since, in the absence of true black-body conditions, the observed temperature is always lower than the true temperature. This calibration is actually an emissivity correction, since the emissivity is a function of both temperature and melt composition. The original furnace was used with a deeper metal bath to provide sufficient depth of immersion for the thermocouple which was inserted through the sampling hole. The atmosphere was a 50-50 mixture or argon and hydrogen passing through the furnace at a rate of 1000 ml per min, and preheated by means of a molybdenum resistance coil. It was assumed that the rapid gas flow effectively eliminated any error which might have resulted from the presence of metallic vapor. The charge in each case consisted of about 300 g of metal, contained in a high purity, dense alumina crucible. At each melt composition, readings of the optical pyrometer and of a thermocouple immersed in the molten metal were taken simultaneously. Calibration curves of optical vs. true temperature were then made for each melt composition investigated. Thermocouples were made of 0.010 in. platinum and platinum-10 pct rhodium. They were checked against the melting point of chemically pure copper. Silica protection tubes with an outer diameter of approximately 1/8 in. were used. The depth of immersion of the tip in the molten metal was approximately 1 14 in. The life of these small thermocouples was relatively short, varying from approximately 1 min at 1550°C to 10 min or longer at 1300°C. Melts containing iron corroded the protection tubes more than those without iron present. Measurements taken while heating checked those taken while cooling, indicating the absence of a temperature gradient between the molten metal and the thermocouple. Results The temperature range of the. measurements on copper-free metals extended from the melting point to 1600°C. For copper the upper limit was 1380°C, and the data were extrapolated linearly for comparison with observations on the other metals and alloys at 1535°C. Examples of typical calibration curves for various melt compositions are shown in Fig. 1. These curves, besides providing a calibration system for the given experimental conditions, also give a basis for the calculation of true emissivities at the effective wavelength of the pyrometer, 0.65 micron. The starting point of the calculations is the value of the emissivity of iron at its melting point. Taking the melting point of electrolytic iron under hydrogen as 1535°C, and using the corresponding emissivity value of 0.43, as determined by Dastur and Gokcen,² the emissivities can be determined as functions of composition (and temperature, if desired). The relationship used is the Wien equation: ln(Ea)=C2/?(1/T1-1/Ta where E is the emissivity; a, the transmissivity of the optical system; C,, the fundamental constant, 14,380 micron-degrees; A, the wave length of light used (0.65 micron); Tt, the true temperature, OK; and T., the apparent temperature, OK. At the melting point of iron the observed temperature was 1358"; this gives 0.62 for the transmissivity, which compares with 0.65 in the similar system used by Dastur and Gokcen. The emissivities of all the compositions investigated were determined at 1535°C, after obtaining from each calibration curve the corresponding temperature. These results

Jan 1, 1953

By F. W. Glaser, Benjamin Post

A LTHOUGH most transition metals form a wide variety of boride compounds, the existence of only one zirconium boride, ZrB2, had been established prior to this investigation.' The crystal structure and some properties of a hitherto unreported zirconium boride, ZrB12, are described in this paper. Only one other dodecaboride of a transition metal, UB12, has been reported up to the present.' Chemical analysis of the new compound showed 44 pct Zr and 56 pct B, compared with 41 pct Zr and 59 pct B computed for ZrB12. The difference is within the range of error of the analytical method employed. ZrB12 shows marked metallic properties. It is obtained as a fine black powder. Measurements of electrical resistivity were made at —79°C, + 22°C and +64°C. At 22°C the electrical resistivity is approximately 60 microhm-cm. Over this range the temperature coefficient of resistivity is +0.00162. The thermal conductivity at room temperature is 0.122 watts per cm per "C. The product of the electrical resistivity and thermal conductivity is therefore 8.05, which is not far from the normal Wiedemann-Franz ratio (approximately 7.5 at room temperature). These measurements were made on hot pressed samples which were not always high density specimens. The hardness of ZrB12 on the Rockwell A scale varies between 92 and 92.5. Crystal Structure Determination Single crystals of ZrB12 of a size suitable for X-ray diffraction analysis could not be obtained and powder samples had to be used. Filtered Cu radiation was used throughout. Powder diagrams were indexed on the basis of a face-centered cubic unit cell. After correction for film shrinkage, a Bradley and Jay extrapolation³ to ? = 90" indicated that a, = 7.408 ±0.002A. The volume of the unit cell is 406.5A.V he assumption that there are four "molecules" of ZrB12 per unit cell leads to an X-ray density of 3.63 g per cc. The measured density is 3.7 g per cc (as measured by the immersion method). Relative intensities of reflections were determined by integrating the intensities of diffraction peaks using the count register of a North American Philips wide range spectrometer. Intensities measured in this way showed good agreement with photographic intensities estimated visually using multiple film techniques. The usual Lorentz, polarization, and multiplicity corrections were applied to the observed intensity measurements. There are striking similarities between ZrB12, and UB12. The unit cell of the latter is also face-centered cubic and contains four molecules. a, = 7.473, compared with 7.408 for ZrB12. The radius ratio rB/rU is 0.57; rB/rZr is 0.54. In both ZrB12, and UB12 the four metal atoms in each unit cell are in special positions; only the boron positions need be determined. The latter may be inferred from the extent to which diffraction of X-rays by the 48 boron atoms reinforces or weakens the diffraction by the metal atoms. This effect is relatively much greater in the case of the zirconium compound. In their determination of the crystal structure of UB12, Berthaut and Blum' assumed holohedral symmetry (space group Oh5 , Fm3m) and reported that the U atoms are in positions 4(a): 000; 01/2 1/2; ½ 0 ½ ; ½ ½; the boron atoms were reported to be in positions 48(i) with x = 1/6: ½xx; ½xx; x½x; x½x; xx½; xx½; ½xx; ½xx; x½x; x½x; xx½; xx½

Jan 1, 1953

By H. C. Chang, N. J. Grant

Creep of very coarse grained high purity aluminum was studied at 400°, 700°, and 1100°F at initial stresses of 50 to 1200 psi. Local strain measurements were made across the grain boundaries and in different regions of various grains during creep, thereby permitting the drawing of component creep curves. The relative amounts of elongation as measured across a grain boundary and in the grains adjacent to the boundary depend on the temperature of testing. The significance of creep curve equations and activation energies is discussed. THIS paper presents some of the results of a research program devoted to the study of the mechanism of creep in high purity aluminum. Previous publications have dealt with the cyclic processes of alternating grain boundary sliding and migration, and the deformation in the grains caused by these processes;' the direction and the driving force of grain boundary sliding and migration;' the deformation in the grains and the restricting effects of the grain boundaries on this deformation." These previous papers were based mainly on either microscopic observations or X-ray data, or both. Sometimes creep curves across two closely spaced reference marks (about 0.6 to 0.7 mm apart) were also presented with a view to correlating the elongation values with the optical observations in general, and with certain deformation processes in particular. These curves shall henceforth be referred to as component creep curves. No attempts were made, however, to compare either the component creep curves which were obtained in different regions of a specimen, or those obtained from different specimens subjected to different creep test conditions. It is the purpose of this paper to present these component creep curves. Among the factors influencing the behaviors of these curves, those studied were stress, temperature, and grain arrangements in the specimens. It is proposed to show how greatly the deformation can vary from grain to grain and within an individual grain in a coarse grained specimen. The experimental technique and procedure have been presented.' It remains necessary to emphasize that the reference marks were produced by pressing a thin sewing needle into the surface of the specimen before the final annealing at 900°F for 24 hr and at 1150°F for 12 hr. The cold work around the needle indentations was therefore removed. The depth of these holes after electropolishing the annealed specimens was about 0.01 mm. This depth and area were negligible in comparison with the thickness of the specimens, 2.3 mm, and hence would not affect the creep behavior. Results Fig. 1 shows a development diagram of specimen P-8. The dots on the surface locate the needle point reference marks used to obtain the component creep curves. A curve obtained between two dots across a grain boundary measures not only the boundary deformation but also the deformation associated with boundary sliding occurring in the grains in the region between these indents. The original distance between two reference marks was about 0.6 to 0.7 mm. The maximum error of measurement was 0.01 mm, or in terms of percentage elongation, of the order of & 1.5 pct. Whereas the component creep curves shown in the figures to follow were drawn as a gross average of the points, in view of the fineness of some of the steps of grain boundary sliding and migration, as shown in the previous publications,¹,2 it appears logical to expect that some of the finer cycles of movement have not been delineated for the strain sensitivity of the measuring system. It seems justifiable to say that the curves are not as smooth as shown. 700°F Tests: Fig. 2 shows component creep curves across four of the grain boundaries in specimen P-8, tested at 700°F and 85 psi. These curves clearly show alternate cycles of increasing and decreasing

Jan 1, 1954

By LESTER H. WOOLSEY

IT IS doubtful whether anything new can be said upon this subject and, therefore, it is with considerable hesitation that l prepare this paper. On account of my recent connection with the Department of State as its law- officer, perhaps I will be pardoned if I discuss this subject briefly from the point of view of that branch of the Government. , I cannot, of course, speak for that department, since I have-no connection with it at-present, but it may be helpful if I set down certain* of the factors which in my opinion and from my experience have a bearing on this international problem. With oil-burning ships, motor vessels, motor vehicles, airplanes-all consuming, astonishing quantities of petroleum or petroleum products; with the United States having within its borders only 12 per cent. of the petroleum resources of the world, and consuming about 70 per cent. of the world's output; with the more enterprising nations wide awake to the necessity ; of obtaining and preserving as large a share as possible of the oil resources extant ; the 'problem is peculiarly and in a, very practical sense an international one.

Jan 1, 1921

By Harvey N. Davis

MUCH has been written and said during the last twenty years about the place of the engineer in modern life, about the fundamental role that he plays both in developing and in maintaining the material foundations of modern civilization, about the advantages, and also the dangers, of the machine age that he has inaugurated, about the Frankenstein problems that he has unconcernedly foisted upon a generation utterly unable to cope with them, and about the obligation that rests upon him to stop inventing machines and turn his almost legendary energy and skill to inventing institutions that will constitute a solution of the problems he has raised, and contrariwise about his utter inability to offer wise or useful counsel in fields outside the narrow boundaries of his technical training.

Jan 1, 1938

By Joseph Jensen

THE history of the normal oil field is supposed to show an oil graph stalting high in flush production, descending more or less steeply into the curve of settled production and dropping gradually to the vanishing point of economical operation. Together with this at somewhere in the early history of the field, there appears from a vanishing point a graph showing the production of water. During the period of settled production this graph rises higher and, toward the close, unless extensive work is done in the line of correction, rises far above the oil graph to where the cost of operation terminates profitable pumping. Fields that start out with a high relative content of water are generally very short lived. Fields that never develop a water problem are exceedingly rare.

Jan 1, 1930

By JAMES H. McGRAW

P UBLZCLTY and engineers do not mix. In the very words of my subject, there is an apparent contradiction. In the past, publicity has been abhorrent to the engineer. It seems to be true that the engineer, because of his training or his background, has developed a state of mind which omits publicity. At any rate he has done a poor publicity job for himself. The average engineer is self-conscious; he ought to be class-conscious. If T should ask the men in this hall to get up one by one and tell who they are and what they have done, there would be an instinctive reaction in the mind of each man-a feeling that this was out of place. If I should ask each man to get up and tell something about his neighbor, I should find that each neighbor, once he got acquainted with the man next to him and understood what he was doing, would be as human and as generous-hearted in telling about his brother engineer as is any professional man.

Jan 1, 1920

By AIME AIME

AMONG the industrial motion pic¬tures released in the last year of possible interest to people in the mining industry are the following: "A New World Through Chemistry," made by the public relations department of E. I. du Pont de Nemours & Co., Wilmington, Del. This film, which is in sound and color, interprets in twenty minutes of narration and ingenious photography many of chemistry's newest developments. It may be borrowed either in 16-mm. size on an 800-ft. reel, or 35-mm. size on a 2000¬ft. reel, the only charge being the cost of returning the film. Douglas D. Rothacker, 729 Seventh Ave., New York City, is prepared to loan free of charge except for transportation each way several films prepared in the plants of the International Nickel Co., 16 mm. with sound. These include: "Nickel High Lights," 35 minutes; "Nickel Mining," 18 minutes; "Nickel Smelting," 18 minutes; "Nickel Refining," 9 minutes; and "Copper Refining," 6 minutes.

Jan 1, 1941

By Galen H. Clevenger

THE real and permanent advances which take place in any industry are for the most part slow evolutions which frequently develop and grow almost imperceptibly from clay to clay. A meritorious idea may and generally does require long and patient development and commercial application under a variety of conditions and in a number of localities before it emerges as standard and generally accepted practice. There must be not only technical perfection but also economic advantage. Thus a cross-section taken at any particular time of an industry may reveal little that is distinctly new and yet there may have been considerable progress. During the past year there has been little that is new in milling and yet there has been real progress; some problems have been solved and some of what we may term the newer developments have become more firmly, established.

Jan 1, 1930

By Russell Webster

In having maintained production for more than 40 years Arizona's Magma mine is unique in a mineral district that includes several major copper mines. Other past and present producers in this area are Miami and Inspiration at Miami, the Old Dominion in Globe, the Ray mine in Ray, and to the south the new San Manuel mine near Tucson. Magma's production of copper, silver, gold, and some zinc has come from nearly parallel east-west striking mineralized faults, one called the Main or Magma vein and the other the Koerner vein, about 1100 ft to the south. This vein system has been prospected and partially mined for some 9000 ft horizontally and 4800 ft vertically. In ascending order from the deepest exploration level, the Main vein cuts Pre-Cambrian schist, Pre-Cambrian Apache Group, Post-Devonian diabase, and Devonian, Mississippian, and Pennsylvania limestones. Until 1950 very little ore was obtained from replacement mineralization.

Jan 10, 1958

By James J. Bean

Although determining and controlling specific gravity of operating medium in a heavy-media plant manually presents no problem, there are advantages to automatic recording and control. The two installations discussed employ the usual method of measurement. Pneumatic control with band control and reset features is used to regulate dilution water and hence specific gravity. Difficulties have been mechanical in nature and associated with obtaining a proper I sample and maintaining tight air connections in bubble-tube piping:

Jan 1, 1950

By G. D. TRANT

HOT metal is commonly transported from the blast furnace to the open hearth by one or the other of two general methods: (1) by hot-metal ladles, usually in conjunction with a stationary mixer, or; (2) by means of mixer-type ladle cars, taking the place of both the hot-metal ladles and the stationary mixer. In both cases, the use of transfer ladles for charging the metal into the open-hearth furnaces is necessary. The American Rolling Mill Co. at its Middletown division, adopted hot metal practice on. June 2, 1928. The pig iron is produced' in a .blast furnace about 11 miles from the open-hearth furnaces, and is trans- ported in Pugh-type mixer cars having a capacity of 150 gross tons each. Three cars are in service and handle the delivery of hot metal to the pig machine and the open-hearth furnaces. The capacity of the blast furnace is 550 tons and casts are made every four hours.

Jan 1, 1929

By T. L. Johnston

MUCH has been said and written about deep mine shafts and deep drill holes as man in his search for mineral wealth digs deeper into the earth's crust. Each year some new extra depth is heralded as a record, but with unlimited possibilities of going still deeper. In contrast to "digging deep," "mining high" is limited by the height of the mountains (Mt. Everest being the maximum with its 29,000-ft. elevation) and also by the extent of human endurance. An ex- ample of what might be called near- stratosphere mining in what is probably the highest mine worked by compressed air in the world is seen in a recent project in the Andes mountains of southwestern Bolivia.

Jan 1, 1939

By R. A. Anderson, T. E. Tietz, J. E. Dorn

Recent investigations1,2,3,4 have conclusively shown that the strain hardened state of metals depends upon the temperature and strain rate of pre-straining as well as on the total plastic strain. A typical example of the effect of temperature of prestraining on the work hardening of metals is reproduced in Fig 1. When pure aluminum is strained at liquid nitrogen temperature the upper solid stress-strain curve (OFGH) is obtained. But when pure aluminum is prestrained to e2 = 0.153 at atmospheric temperature and the test is then completed at liquid nitrogen temperature, the curve OBCD results. Thus a prestrain E2 = 0.153 at atmospheric temperature gives a flow stress C when continued at liquid nitrogen temperature, whereas a higher flow stress G results when the specimen is strained exclusively at liquid nitrogen temperature to the same strain E2. Consequently the metal strain hardens more rapidly at the lower temperature. Obviously the strain alone is not a measure of the strain hardened state in metals. Inspection of Fig 1 reveals that the flow stress at C is identical with that at F. This fact suggests that a strain E2 = 0.153 at atmospheric temperature induces the same work hardened state as a strain E1 = 0.058 at liquid nitrogen temperature. But this concept of equivalent strains is also in error. If curve CD is shifted to the left so that point C falls on F, point D becomes D'. Inspection of the curves reveals that the rate of increase of stress with strain at C is greater than the rate of increase of stress with strain at F even though the flow stresses are identical. Consequently C and F do not represent identical work hardened states. It therefore becomes important to ascer- tain how the strain hardened states at C and F might differ from each other. In a more recent report1 it was shown that straining at higher rates of strain increases the amount of strain hardening in a manner quite analogous to straining at lower temperatures. These observations suggested that the flow stress is not only a function of the strain but also a function of the strain rate-temperature history of straining, perhaps in accord with the Zener- ?H Hollomon parameter p = Ee /RT (where

Jan 1, 1950

By V. A. Phillips

Transmission-electron micrographs of electro-thinned samples of bulk-aged Cu-3.1 pet Co alloy show an aging sequence, supersaturated solid solution — coherent particles — quasi -coherent particles — noncoherent particles. Hardening is due to precipitation of coherent spherical fee coball-rich particles showing coherency strain fields, which are resolved at between 15 and 30A diameter. Loss of- full coherency did not occur until well into the overaged region, even with the assistance of deformation after aging. Different average particle diameters of 123, 92, and 149 ± 10Å were observed in samples aged to peak yield strength at 600°, 650°, and 700°C, respectively, indicating that there is no critical size for peak hardening. Noncoherent particles tended to develop (111) faces and became octahedral in shape. Dislocations tended to nucleate spherical coherent particles which eventually grew together forming large elongated particles. The surface energy of a noncoherent (low-angle) inter-phase boundary is estimated to he about 50 ergs per sq cm. A number of particle lining-up phenomena were observed. Overaging is principally attributed to increase in particle spacing, progressive loss of coherency, and increase in amount of discontinzdous precipitation. COPPER dissolves about 5.6 at. pet (5.2 wt pet) of cobalt at 1110oC1 and the solubility decreases to 0.75 at. petl (0.54 at. pet)2 at 650°C and to 0.1 at. pet or less at lower temperature.' It has been known for many years3-5 that Cu-Co alloys are capable of age hardening. Since cobalt is fee above 417°C and its atom size is only about 2 pet smaller than that of copper, precipitation of coherent particles would be expected. The equilibrium phase precipitated at 700°C and below contains about 10 pet Cu in solution which tends to stabilize the fee structure, lowering the transformation temperature to 340oc.l The alloy is known to undergo discontinuous precipitation in addition to general precipitation; while the former can be seen with an optical microscope, the latter precipitates are not visible except in the grosly overaged condition.5, 6 Extensive use has therefore been made of the ferromagnetic properties of the precipitate in order to follow the course of aging, and it has proved possible to measure the average particle size, spacing, approximate shape, and volume fraction and to determine that the particles are coherent without ever seeing a particle (see for example Refs. 2, 7, and 8). The magnetic measurements of particle size are limited to diameters below about 120Å.7 The present study was undertaken using the techniques of transmission-electron microscopy in order to check the above conclusions, to extend the previous magnetic work to larger particle sizes, and to attempt a more detailed correlation of properties and structure. A portion of this work has already been published.9-11 The present paper is concerned with the metallographic features of precipitation in relation to aging curves. Bonar and Kelly12'13 have published preliminary results of a similar study on single crystals of Cu-2 at. pet Co. EXPERIMENTAL Preparation of Alloy. A Cu-Co alloy, containing 3.12 wt pet (3.36 at. pet) Co by analysis, was prepared from 99.999 pet purity oxygen-free copper and electrolytic-grade cobalt. The alloy was melted and cast in vacuo in a high-frequency furnace using a graphite crucible and mold: Analysis showed chat 0.004 pet C was picked up during melting. The 1-1/2-lb ingot was homogenized in hydrogen for 24 hr at 1000°C. Slices were cold-rolled to 0.005 or 0.003 in. thickness, with an intermediate 650°C anneal in hydrogen at 0.080 in. thickness. Batches of six to ten strips were solution-treated in sealed-off quartz tubes in high vacuum in a vertical furnace and quenched by dropping into iced brine containing a device which snapped off the nose of the tube. Solution treatment consisted of 1 hr at 990°C or 2 hr at 965°C. The latter was employed for all mechanical-property studies, since a tendency was noted for the higher temperature to give porous material. Strips were usually aged individually in a horizontal vacuum furnace, inserting into the hot zone and withdrawing into a cold zone without breaking the vacuum. This method gave a rapid heating rate, permitting the use of short aging times. In some cases, particularly for the longer aging times at the higher temperatures, samples were sealed individually in quartz tubes in high

Jan 1, 1964

By G. S. Ansell, J. Weertman

The creep behavior of an aluminum alloy hardened with a finely dispersed phase of aluminum oxide was investigated. The as-extruded alloy shows an approximate steady-state creep in which the creed rate depends exponentially on the applied stress. The activation energy of creeb is abbroximately 150,000 cal per mole. The recrystallized alloy shows no steady-state creep. ONE method of improving the creep resistance of a metal is to introduce a finely dispersed second phase into the metal matrix. The improvement of the creep resistance has been qualitatively explained by assuming that the dispersed second-phase particles act as obstacles to dislocation motion. If the main effect of second-phase particles is simply to hinder dislocation motion then it is possible to derive a high-temperature creep equation for a dispersion-hardened alloy in a straightforward manner. In the Appendix of this paper such an equation is derived from a creep model which works very well for pure metals. Recently, F. V. Lenel has fabricated, for the first time, powder extrusions of aluminum-aluminum oxide in a large-grained recrystallized form. This alloy, designated as MD 2100, consists of a fine dispersion of aluminum oxide plates in a matrix of commercial purity aluminum. A considerable amount of investigation has been carried out concerning the microstructure and physical properties of this alloy.&apos; ) The aluminum oxide is present in the form of flakes 130A units thick and 0.3 u on edge. They are dispersed in the aluminum matrix with an average spacing of approximately 0.5 jx. The spacing varies in the range of 0.05 to 1.5 µ. The alloy structure is extremely stable at high temperatures. For this reason the alloy offers a unique opportunity for a fundamental study of creep of a very finely dispersed two-phase alloy. Lenel supplied specimens in both the unrecrystallized and recrystallized condition. This paper reports high-temperature creep experiments carried out on these specimens. The results obtained were rather unexpected. No steady-state creep was observed in the recrys-tallized material. In fact, after some transient creep which takes place upon loading, the creep rate is essentially zero ( < 10-8per min). If the second-phase particles acted solely as obstacles to the motion of dislocations, measurable steady-state creep would be expected. Since none is observed it appears that the main effect of the fine dispersion in the recrystallized material is to inactivate the dislocation sources themselves, rather than hinder the motion of dislocation loops created at these sources. EXPERIMENTAL DETAILS Specimens were tested in wire form, 0.087 in. in diam for the as-extruded alloy, and 0.035 in. in diam for the recrystallized alloy. These samples were held in friction-type wire grips; a gage length of 2.5 cm was used for all the creep tests. The specimens were held at 600°C in the test apparatus for at least 15 hr prior to each test. The tests were run under the condition of constant loading and, since the creep strains were small, can be considered as constant stress tests. The temperature of testing was held constant within 3°C. Elongations were measured with an optical cathetometer which was capable of measuring strains as smaIl as 0.00012. This allowed the measurement of strain rates as low as l0-8&apos;per rnin. In addition to the creep tests optical micrographs were made in order to determine both the grain size and microstructure of these materials. RESULTS Fig. 1 shows a few typical creep curves obtained from the as-extruded material. The elongations were somewhat erratic, but each curve shows a region of quasi-steady-state creep from which an approximate steady-state creep rate can be obtained. In general the higher the stress at a given temperature, the greater the total elongation before fracture. The lower the applied stress, the longer is the region where the creep rate is almost constant. Summary data from the creep tests of the as-extruded material are listed in Table I. The steady-state creep data of the as-extruded material for a range of stresses at a constant temperature follow a creep equation of the type creep rate = K&apos; = A exp (&) [11 where A and B are constants, k is Boltzmann&apos;s constant, T is the absolute temperature, and a the stress. The standard error of estimate of the data received is less than one order of magnitude. As shown in Fig. 2, if one compensates the creep-rate data for the effect of temperature over the range of test temperature, the steady-state creep data roughly follow a creep equation of the type Temperature compensated creep rate = K* = A exp

Jan 1, 1960

By D. V. Edmonds, C. J. Beevers

Tensile tests were carried out on a! titanium containing 850, 1250, and 2700 ppm 0, and up to -500 ppm H. The tests were performed at -196", -78", 20°, 150°, and 300°C at a strain rate of -1.0 x 10??3 sec-1. Increasing oxygen content, increasing grain size, and decreasing test temperature resulted in enhanced embrittlement of the a titanium by the hydrogen additions. Metallographic observations showed that this can be correlated with the influence of these parameters on the introduction of cracks into the a! titanium by fracture of titanium hydride precipitates. CRAIGHEAD et al.1 reported that the hydrogen content normally found in commercial-purity a! titanium (60 to 100 ppm) was sufficient to cause a substantial lowering of the impact strength, and they attributed this embrittling effect of hydrogen to the precipitation of titanium hydride. Lenning et al.&apos; found that in commercial-purity a titanium there is an almost complete loss of impact strength at about 200 pprn H, which is approximately half the value needed to eliminate the impact strength of high-purity a titanium. They also showed that the presence of 3000 ppm hydrogen reduces the room-temperature tensile ductility of commercial-purity material to a value of the order of 10 pct; the corresponding hydrogen concentration for high-purity titanium is over 9000 ppm. It thus appears that the detrimental effect of hydrogen on the mechanical properties of commercial-purity titanium becomes evident at much lower hydrogen contents than for high-purity titanium. The main difference between the two types of a titanium might be expected to be the higher level of interstitial impurity in the commercial-purity grade. Jaffee et a1.3 studied the influence of temperature and strain rate on the hydrogen embrittlement of high-purity and commercial-purity ! titanium. In general, the behavior was the same for both materials; embrittlement was enhanced by decreasing temperature and increasing strain rate. Recent results from tests on commercial-purity a titanium containing 850 ppm O and varying amounts of hydrogen up to -500 ppm showed that the degree of embrittlement by hydrogen is intimately related to the fracture characteristics of titanium hydride precipitates.4 The present paper considers the interrelationship between the mechanical properties and micro-structural features of commercial-purity a! titanium containing 850, 1250, and 2700 ppm 0 and varying amounts of hydrogen up to -500 ppm. 1. EXPERIMENTAL PROCEDURE Three types of commercial-purity titanium supplied by IMI* were used in the investigation, and for the *Address: Witton, Birmingham 6, United Kingdom. purpose of this paper are designated Ti 115, Ti 130, and Ti 160. The principal impurity elements are given in Table I. The material was received in the form of 12.7 mm diam bars having a fully recrystallized structure. Tensile specimens with a round cross-section of 4.5 mm diam and a gage length of 15.2 mm were machined from the bars. In order to develop the same grain size (mean linear intercept of grain boundaries) in each of the three types the specimens were annealed under a dynamic vacuum of <10?5 mm Hg, Table 11. Specimen hydriding was carried out in a modified Sieverts apparatus;&apos; hydrogen was taken into solution at 450°C and after holding the specimens at this temperature for 24 hr they were furnace-cooled to room temperature at an average rate of -100 C deg per hr. By this method nominal hydrogen contents of 0, 50, 100, 250, and 500 ppm were introduced into specimens of Ti 115, Ti 130, and Ti 160 (100 ppm (wt) -0.5 at. pct). The actual hydrogen contents were calculated from the weight differences obtained by weighing the specimens before and after the hydriding treatment. Tensile tests were carried out at temperatures of -196", -78", 20°, 150°, and 300°C on a 10,000 kg In-stron machine at a nominal strain rate of -1.0 x 10-3 sec-1. Fractured specimens were sectioned in planes parallel to the tensile axis, mechanically polished to 0.25 µm grade of diamond paste, and then attack polished using a solution containing by volume 99 parts H2O, 1 part HF, and 1 part HNO3. Although the latter treatment unavoidably opened out cracks and voids visible after mechanical polishing, it did reveal the grain structure, titanium hydride morphology, and deformation twinning structure.

Jan 1, 1970