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By Roy Neal

THERE are two main sources of the water that floods productive oil or gas sands. The water may rise from the lower depths of the producing stratum, or it may come from beds above or below the oil-bearing formation. Usually the recovery of oil is decreased by water entering the oil sands, and most oil-field waters, especially those of deep wells, tend to foster the formation of an emulsion, which is expensive to treat. This paper deals with a method of distinguishing between waters that encroach upon oil-bearing, beds from sources in the same stratum and waters .that reach the oil sands from horizons above. In order to remedy effectually water difficulties in oil and gas wells, it is absolutely necessary to determine the source of the invading water. Sometimes evidence such as the structural relations between the strata penetrated by neighboring wells and those found in the well under investigation is not adequate; also, data from drill logs and well records, from mechanical tests made on the wells by plugs, testers, drilling tools, etc., and from tests by chemical indicators such as eosin and Venetian red, may he unsatisfactory, for such data may fail to locate the source of the infiltrating waters. As a resort in such cases, the application of chemical analyses, that is, the comparison of an analysis of the water in, question with that of typical waters from the various water horizons in that particular district, has in certain instances proved of value. This method has been used to advantage in the Westside Coalinga field of California, where the source of water may be fairly definitely determined from its composition. The chief conclusions concerning the chemistry of the oil-field waters in California by G. S. Rogers1 are: "Oil-field water is not necessarily salty, as is generally believed, and may not be even slightly salty to the taste. The degree of concentration of chloride in such water is governed primarily by local conditions and is not affected by the position

Jan 1, 1919

By C. W. Washburne

Continued discussion of the paper Of ROSWELL H. JOHNSON, presented at the New York meeting, February, 1015, and printed in Bulletin No. 98, February; 1915, pp. 221 to 226. See also Bulletin No. 101, May, 1915, pp. 1157 to 1162, and No. 103, July, 1915, pp. 1449 to 1450. C. W. WASHBURNE, New York, N. Y. (communication to the Secretary*).-Mr. Johnson recognizes that connate waters must be driven, outward toward the earth's surface. He considers the ascent due to the settling and packing of the underlying sediments and to the formation of gas within the rocks, supplemented by abyssal pressures. The origin of the methane in the sedimentary strata probably is not simple. There are three possible modes of origin: (1) as marsh gas formed near the surface and entrapped in the sediments; (2) from abyssal sources; (3) by the decomposition of organic matter buried in the sediments. The abyssal source is generally negligible, and in all cases doubtful. The third origin is the most important in the gas fields. A fourth mode of origin, by the dissociation of liquid hydrocarbons, frequently has been suggested, but it is improbable, because crude oils are exothermic. Therefore they have no tendency, to split or decompose at low temperatures, as do endothermic substances, such as coal, which is geologically by the loss of methane, water, and carbon dioxide. This cannot happen to a hydrocarbon until its temperature of dissociation (" cracking point") is reached, which is over 250'.C. for the most easily cracked hydrocarbons and over 400° C. for others. Engler says that the dissociation of fats and waxes into oils is an endothermic process, thereby unconsciously nullifying his own theory of the dissociation of these substances at low temperatures. However, recently I have found reason to think that heat is liberated by the disruption of the molecules of fats and waxes, as it is in the molecular decomposition of the substances of wood, coal, etc. If this tentative opinion is correct, and Engler wrong, then it seems that the Engler-Höfer hypothesis of the origin of oil becomes not only possible, but even probable.

Jan 9, 1915

By E. T. Dumble

PROF. EDWARD ORTON, in his Report on the Occurrence of Petroleum, Natural Gas and Asphalt Rock in Western Kentucky, thus clearly states his ideas of the universal dissemination and rare accumulations of the bitumens:1 " We need to bear in mind that the various members of the bituminous series are abundantly and almost universally distributed among the unaltered sedimentary rocks of the earth's crust. The valuable accumulations of these substances are rare, it is true, but one can scarcely go amiss of petroleum, asphalt or gas, at least in small quantities, among the stratified rocks that retain their original structure." Speaking of the Ohio valley, he adds: "A fifth of one per cent. of petroleum, if distributed through a, thousand feet of rock, would make a total to the acre, or square mile far , beyond any production that has ever been realized from the richest oil field, and percentages of this amount are not only not rare to find, but are even hard to miss." Dr. F. W. Clarke in his Data of Geochemistry (Bulletin No. 491, U. S. Geological Survey, 1911), discussing these views of Orton with similar views of T. Sterry Hunt and Szajnocha, says that they "lead to the conviction that the formation of bitumens is a general process and by no means exceptional. Wherever sediments are laid down, inclosing either animal or vegetable matter, there bitumens may be produced."2 The organic origin of the bitumens, including petroleum, has long been an accepted fact with nearly all geologists, but the method, place, and time of the transformation into petroleum or other bitumen is still under discussion.

Jan 3, 1914

By Benjamin C. Craft, Frank Perkins

The wall-building properties of salt-water muds can be maintained at high temperatures by additions of gum karaya, gum ghatti, gelatinized starch, or commercially prepared starch. A germicide should be used to prevent fermentation. Introduction The behavior of drilling mud has received special attention from the petroleum industry within the past few years in numerous research projects dealing with such subjects as chemical treatment, gelation, and filtration characteristics. The importance and control of filtration, or water loss, is readily apparent* It affects the analysis of side-wall cores and interpretation of electric logs; it controls to a large extent the work of primary cementing, reduces the amount of expensive fishing, and permits the running of long strings of casing. It has been found that among the many factors that have an adverse effect on filtration, the presence of electrolytes, in general, and of salt, in particular, is outstanding. The effect is one of flocculation of the colloids due to neutralization of the negative charges on the clay particles. This reaction is further increased on the Gulf Coast because high temperatures reduce dispersion, to a minimum, causing increased flocculation in both fresh-water and saltwater muds. The problem of reducing water loss in salt-water muds by the addition of gums and starch at atmospheric temperature has been investigated,' and many successful field tests in West Texas indicate its solution. From the work of Byck2 it is concluded that no existing method will permit an approximate determination of the filtration rate at high temperatures from data taken at room temperatures. Filtration should be measured at the ternperature actually anticipated in the well, or at least at a number of lower temperatures and extrapolated over a small range. A laboratory study has been made of the chemicals available for the filtration characteristics of salt-water muds at high temperatures, and the use of germicides to prevent fermentation. Laboratory Investigations Procedure Since the purpose of this investigation was to compare several different gums and starches at elevated temperatures, mud from the same source was used for all the tests. Viscosity was measured in a Stormer viscosimeter at 600 r.p.m. and water loss was determined with a Baroid High-pressure and High-temperature Wall-building Tester3 at temperatures from 80' to 250°F. and at a pressure of 500 lb. per sq. in. for 30 minutes. The samples tested consisted of 150 grams of commercial Louisiana mud, 50

Jan 1, 1943

By Craig R. Barrett, Alan J. Ardell, Oleg D. Sherby

It is shown that the apparent activation energy for creep of pure poly crystalline metals increases with increasing temperature in the temperature range 0.5 to 1.0 of the absolute melting temperature. This increase is probably associated with the influence 0-f the elastic modulus on the creep rate. By accounting for the variation of Young&apos;s nodulus with temperature, the true activation energies for creep of pure cadmium and aluminuvl are shown to be equal to the activation energies for self-diffusion in these metals, within experimental error, at all temperatures above 0.5T,. New creep parameters are proposed for cmrelation of steady-state creep rate and time-to-rupture data. These are respectively, where u is the creep stress, E is Young&apos;s rrodulus, i,is the steady-state creep mte, t, is the time -to-rupture, and D is the self-diffusion coefficient [equal to Do exp (-QSd/RT)] . It has been established experimentally1 and theoreticallyZm4 that high-temperature creep of poly-crystalline pure metals is a thermally activated process and may be represented by the general expression where <, is the steady-state creep rate, A is a constant dependent on the internal structure of the material, f is some function of the applied stress (0) and test temperature (T), and D is the self-diffusion coefficient. If D is separated into its temperature-dependent and independent portions, then it is possible to rewrite Eq. [I] as where Qsd is the activation energy for self-diffusion. Assuming a simple Arrhenius-type relationship between creep rate and temperature at a given constant stress, the apparent activation energy for creep, Q,, is given by the expression It is obvious that if is not a function of temperature It has been shown that the steady-state creep rate for pure polycrystalline metals1 can be represented by where S is a constant, L is the grain diameter, E is the isotropic polycrystalline (unrelaxed) elastic modulus, and n is a constant equal to approximately 5 over a wide range of stress. The apparent activation energy for creep calculated from this expression at constant grain size and stress is given by

Jan 1, 1964

From the cold Pacific waters in June rolls a blanket of white clouds that tucks up around the mountains at around 8000 or 9000 ft. This is the way it happens in southern Peru and so the mining operations and daily living at Toquepala have an ethereal quality not often encountered. Besides looking down on the clouds from the brightly sunlit mountain tops, one can discern the trace of a different era in the brown barren mountain slopes. This trace is like a delicate net laid over the surface of the earth-a criss-crossing of innumerable trails that are so omnipresent, yet faint, that the local people have long since ceased to notice them. It is difficult at first to ask about them because no one understands what you are talking about. It finally comes out though, that the markings are indeed trails, but fossil trails made by animals in times when they were in abundance in a countryside that was green in some bygone century. In a way Toquepala is still pristine, it is the way the engineers planned it-from the ground up. There are no additions or expansions- those tackings-on that spoil the symmetry of design while increasing the profit. This does not deny that annual production has gone up over the years. Daily mill throughput has been increased from 30,000 to 42,000 tpd. Initial design of the concentrator was for 30,000 tpd but in 1964-65 milling capacity was increased to 36,000 tpd at a cost of $3 million.

Jan 11, 1969

By J. N. Hobstetter, J. J. Becker

Slip lines in deformed copper single crystals exhibit very pronounced cross-slip and clustering if the stress axes are not too far from <100>. This orientation dependence seems to persist whether or not attempts are made to reduce the bending constraints of ordinary mechanical tests. THE purpose of this paper is to report some microscopic features of the plastic deformation of copper single crystals. The material used was OFHC copper obtained from the American Brass Co. Single crystals about 3 in. long and 5/16 in. in diameter were made by lowering graphite crucibles containing this copper out of the hot zone of a vertical tubular furnace at a rate of 1 1/4 in. per hr. The furnace atmosphere was nitrogen. The orientations of the crystals were determined by the back-reflection Laue technique.&apos; The X-ray spots usually indicated a slight lineage structure of not more than a degree or two. The crystallography of slip is discussed in Schmid and Boas.&apos; The terms classical slip, cross-slip, and conjugate slip are used here with the same meanings as in ref. 3. Compression Specimen 17 (Fig. 1) was selected because the resolved shearing stresses on eight slip systems dif- fered at most by a factor of 1.2. It was hoped that in this situation such effects as cross-slip might be made more prominent. Two intersecting planes parallel to the stress axis were ground on the crystal, using optical abrasive on a lead lap. The large plane was approximately perpendicular to the plane of the axis and the primary slip direction. Its exact orientation was determined by X-ray. The smaller made an angle of 49" with the larger, measured by reflecting a small light source. The specimen was etched with nitric acid until its diameter had been reduced 0.010 in., and then was given a metallographic polish and very

Jan 1, 1954

By L. F. Rooney

In June 1964 the Indiana Geological Survey discovered gypsum beds more than 10 ft thick in rocks of Devonian age in La Porte County, Ind. Although the extension of the Michigan Basin evaporites into northern Indiana has been recognized for some time, the gypsum beds have been regarded as either too thin or too deep for exploitation. Current Survey research, however, indicates that exploration by industry might find commercial deposits of gypsum less than 50 miles from Chicago. In four cores taken by the Survey within 1 sq mile in La Porte County, the maximum thickness of inter-bedded gypsum and anhydrite is 35.8 ft. Both gypsum and anhydrite beds contain irregular masses of limestone and dolomite that average a few inches in cross section and total about 20% of the rock by weight. The maximum thickness of gypsum in one minable unit verified by core is 12.5 ft, and its purity is 81.3%. Chloride content of the gypsum beds is less than 0.005%. Depth to the gypsum in La Porte County is 330 to 500 ft, about the same depth as the gypsum being mined in Martin County, Ind. In June 1964 the Indiana Geological Survey discovered gypsum deposits of probable commercial thickness near La Porte, Ind. (Fig. 1). This article presents preliminary data on the distribution, thickness, depth and chemical composition of the gypsum, the possible causes of gypsification, and economic considerations of immediate interest to industry. Because of the preliminary nature of the work, only a few geologic relationships concerning the genesis of the deposits will be mentioned. DEFINITIONS The following terms used throughout this article have been restricted to the following definitions: evaporites: anyydrite (CaSO4) or gypsum (CaSO4 . 2H2O). minable evaporites: any evaporite unit which may contain more than 80% evaporites, which is more than 10 ft thick, and which in places may be completely gypsified. PREVIOUS WORK The presence of gypsum and anhydrite in the Devonian rocks of northern Indiana has been recognized for at least 70 years1-4 and can be inferred from a number of reports on the geology of Michigan. For example, in a cross section from southwestern to central Michigan, Ells5 indicated the presence of

Jan 1, 1965

NEW MEMBERS The following list comprises the names of those persons who became members during the period Oct. 10 to Nov. 10, 1915: Members BECK, WESLEY HUDSON, Civ. and Min. Engr., Ellsworth Collieries Co., Ellsworth, Pa. BRADSHAW, GRANT D., Pres., Andrews-Bradshaw Co, 409 Diamond Bank Bldg., Pittsburgh, Pa. BUTLER, BERT S., Geol U. S. Geological Survey, Washington, D. C. CAMERON, FRANK, Asst. Mine Foreman, Braden Copper Co., Rancagua, Chile, So. Amer. CHEN, YEFAH FRANCIS, Asst. Min. Engr., Pinghsiang Colliery, Pinghsiang-Ki, via Changsha, China. CLAGHORN, DAVID MONTGOMERY, Mining Engr., Timekeeper, Wilkeson Coal & Coke Co., Wilkeson, Wash. DAVIS, REUBEN WALDO, Min. Engr., Supt., Cannel Coal Co., Dolores, Webb Co., Tex. DOUTHETT, GEORGE M., Supt Crescent Metals Co., Glenwillard, Pa. DUNSFORD, ENSOR R., Min. Engr., Asst. Supt., Victoria Gypsum Min. & Mfg. Co., Ltd., Quarry, St. Alms. C. B.. Nova Scotia. Canada.

Jan 12, 1915

By Benjamin C. Craft, Frank Perkins

The wall-building properties of salt-water muds can be maintained at high temperatures by additions of gum karaya, gum ghatti, gelatinized starch, or commercially prepared starch. A germicide should be used to prevent fermentation. Introduction The behavior of drilling mud has received special attention from the petroleum industry within the past few years in numerous research projects dealing with such subjects as chemical treatment, gelation, and filtration characteristics. The importance and control of filtration, or water loss, is readily apparent* It affects the analysis of side-wall cores and interpretation of electric logs; it controls to a large extent the work of primary cementing, reduces the amount of expensive fishing, and permits the running of long strings of casing. It has been found that among the many factors that have an adverse effect on filtration, the presence of electrolytes, in general, and of salt, in particular, is outstanding. The effect is one of flocculation of the colloids due to neutralization of the negative charges on the clay particles. This reaction is further increased on the Gulf Coast because high temperatures reduce dispersion, to a minimum, causing increased flocculation in both fresh-water and saltwater muds. The problem of reducing water loss in salt-water muds by the addition of gums and starch at atmospheric temperature has been investigated,&apos; and many successful field tests in West Texas indicate its solution. From the work of Byck2 it is concluded that no existing method will permit an approximate determination of the filtration rate at high temperatures from data taken at room temperatures. Filtration should be measured at the ternperature actually anticipated in the well, or at least at a number of lower temperatures and extrapolated over a small range. A laboratory study has been made of the chemicals available for the filtration characteristics of salt-water muds at high temperatures, and the use of germicides to prevent fermentation. Laboratory Investigations Procedure Since the purpose of this investigation was to compare several different gums and starches at elevated temperatures, mud from the same source was used for all the tests. Viscosity was measured in a Stormer viscosimeter at 600 r.p.m. and water loss was determined with a Baroid High-pressure and High-temperature Wall-building Tester3 at temperatures from 80&apos; to 250°F. and at a pressure of 500 lb. per sq. in. for 30 minutes. The samples tested consisted of 150 grams of commercial Louisiana mud, 50

Jan 1, 1943

By W. E. Bruce, R. J. Morrell, James Paone

This chapter is a partial summary of an investigation by the U.S. Bureau of Mines (USBM) made in response to a recent request by the Assistant Secretary, Water and Power Development of the U.S. Department of the Interior, for a comprehensive review of horizontal boring technology related to underground power-line installation. This review is concerned primarily with 3 to 36-in. diam horizontal holes from several hundred to several thousand feet in length. An electric power system consists of three essential functions: generation, transmission, and distribution. The generation component includes the generating station and step-up substation; the transmission component includes the transmission line and stepdown substation at typical voltage levels ranging from 69 to 345 kv for underground lines and 69 to 500 kv for overhead transmission lines; the distribution component includes the distribution line carrying the commonly used voltages of 120, 208, and 240 v, the distribution transformer, and the line to the service customer.l The Federal Power Commission reports that 1600 miles of underground transmission lines of 60 to 345-kv capacity are now in service in the United States. By 1980, it is estimated that approximately 3000 miles of trans- mission lines will have to be placed underground.2 The cost of burying electric transmission lines underground in metropolitan areas, approximately 30 miles from the center of each of the most populated cities, will exceed $1.5 billion with the methods now available. The wide spread in unit costs of overhead and underground transmission lines narrows as right-of-way costs for overhead transmission in congested areas increase. Improved methods of underground emplacement will certainly reduce this difference in costs and even further favor underground emplacement. Also, in the future, overhead transmission lines will probably not be permitted in highly built-up areas.

Jan 1, 1970

By H. M. Chance

By courtesy of the officials of the Chicago, Burlington and Quincy railroad, I am permitted to publish the results of an examination made in 1887 and 1888 of&apos; the country west of the Black Hills, and lying between the Black Hills and the foot-hills of the Big Horn Mountains in the northeastern part of Wyoming. With the exception of the country constituting the foot-hills, or the encircling ridge or rim of the Black Hills proper, all of this area is occupied by rocks of Cretaceous age. In the central part of the Black Hills are found the tin-bearing granites, the mica-schists, and gold-bearing slates, already so well known. Surrounding this central area of older rocks (which should be considered as the "Hills" proper) are the attenuated representatives of the Palzeozoic, dipping gently away from the Hills in every direction, overlaid by the gypsum-bearing Mesozoic, which here forms a bold high ridge or rim, completely encircling the Black Hills, and known as the inner ridge. Overlying, and apparently conformable to this, we find the Dakota sandstone, which likewise forms a prominent ridge or rim, known as the first or outer ridge. This is the formation which contains the coal now worked at the mines near Newcastle. It is also the formation in which the best oil-wells have been obtained in the "Stoakdale," or "Beaver," and the " Belle Fourche " oil-districts. Overlying it are the Colorado shales, forming the great plains drained by Beaver creek and the south fork of the Cheyenne river, and extending west to the Belle Fourche, near Donkey creek, where the overlying Fox Hill formation (thin) and the Laramie group, the great lignite-formation, are first seen. The Laramie group occupies the surface from the Belle Fourche at Donkey creek west to the foothills of the Big Horn mountains at Buffalo, an air-line distance of some seventy or eighty miles.

Jan 1, 1891

By C. H. Li, R. J. Stokes

This paper compares the fracture behavior of tungsten rods in three conditions: recrystallized. recovered, and wrought. Notched specimens suhjected to a 50 in.-lb impact load showed ductile-brittle transitions at 700, 4.90°, and 440°C, respectinely. The recrystallized material had an equiaxed pain structure and jracbred by simple cleavage from a grain boundary source at all temperatures up to 700°C. The wrought and recovered material had an elongated fibrous structure and at low temperatures fractured by cleavage originating from the notch. As the transition temperature was approached cleavage was preceeded by more and more intergvanular splitting which deflected the crack front into planes parallel to the tensile axis. The enhanced toughness of wrought and recovered tungsten was attributed both to its inability to initiate cleavage because no pain boundaries were suitably oriented perpendicular to the tensile stress and to its inability to maintain cleavage because of intergranular splitting ahead of the crack. It has been appreciated for a long time in a qualitative manner that the room-temperature brittleness of fully recrystallized tungsten may be alleviated by working the material at relatively low temperatures.&apos; More recently this difference in mechanical behavior between wrought and recrystallized tungsten has been examined quantitatively by measurement of the tensile properties as a function of temperature. In these experiments brittleness has been expressed in terms of ductility or reduction in cross-sectional area upon tensile fracture or in terms of the bend radius before fracture under bending.&apos; This work has shown the existence of a fairly sharp transition from brittle to ductile behavior with an increase in temperature. The ductile-brittle transition temperature for recrystallized material is approximately 200°C higher than for wrought material. An increase in strain rate, small additions of impurity,&apos; or an increase in grain size4 shift the respective transition temperatures to higher values, but the difference between them remains approximately the same at 200°C. A number of explanations for this embrittlement by recrystallization have been given. It has been blamed either on the concentration of impurity at the grain boundaries, the increase in grain size, or the change in texture which occurs upon recrystallization. The present paper examines the effect of different heat treatments on the notch-impact behavior of commercial powder-metallurgy tungsten rods. The change in the ductile-brittle transition temperature for this method of loading and the fracture mode has been related to the different mi-crostructures produced by heat treatment. EXPERIMENTAL PROCEDURE Commercial swaged powder-metallurgy tungsten rods 1-3/8 in. in length and 1/8 in. in diameter were machined to introduce a sharp V notch 0.030 in. deep. To change the microstructure from that of the as-received wrought material some of the specimens were subjected to an anneal in nitrogen either at 1300° or 1400°C for 8 hr or at 1600° or 2000°C for 1/2 hr. The notched rods were then placed in a miniature Charpy-type impact machine and struck at their midpoint (opposite the notch) with a hammer designed to deliver 50 in.-lbs of energy. The strain rate at the base of the notch was estimated to be approximately 100 sec-1 at the instant of impact. The specimens were heated in situ to the desired impact temperature. The microstructures produced by the various anneals were studied by both X-ray diffraction and metallographic techniques. Fig. 1 reproduces the microstructures observed metallographically following a 10-sec electroetch in a 10 pct KOH solution. Fig. l(a) shows the elongated fibrous grain structure of the as-received material. Following the anneal at 1300" or 1400°C the grain structure was still elongated as shown in Fig. l(b) but the etch pits delineated dense polygonized dislocation arrays within many of the grains. Occasionally a relatively dislocation-free recrystallized grain was found growing into the matrix. The anneals at 1600° and 2000°C resulted in complete recrystallization and some grain growth. The grains produced at 1600°C were still slightly elongated as shown in Fig. l(c) whereas the anneal at 2000°C produced equiaxed grains. The changes in grain size produced the expected changes in the X-ray back-reflection patterns; there was no indication either in the as-received material or the annealed material of any preferred orientation. RESULTS a) Impact Behavior. Fig. 2 reproduces the ductile-brittle transition curves measured in the manner described in the previous section. It can be seen that under these testing conditions the as-received

Jan 1, 1964

By B. C. Wonsiewicz, W. W. Wilkening

Following a procedure proposed by Wheeler and Ireland, Plane stress yield loci were constructed from Knoob hardness numbers. Basically, six differently oriented hardness measurements were made on three orthogml surfaces through pure poly crystalline magnesium sheet, a magnesium single crystal, and sheet of the magnesium alloys: Mg + 0.5 pct Th, Mg + 4 pct Li, AZ31B, and EKOO. Hardness loci were found to be in poor agreement at small strains (E < 0.05) with loci established by a more rigorous technique. At larger strains (E - 0.10) the agreement is fair, but at this stage in deformation the conventional locus has lost much of the asymmetry that characterizes these anisotropic materials. Two effects which will lead to distortions in the Khn locus are discussed with reference to the geometry of plastic flow during a hardness test. DETERMINING a material&apos;s resistance to multiaxial loading is of interest not only from a structural design viewpoint but also from that of deformation processing. Unfortunately, the determination of the yield locus, although simple in principle, involves tedious procedures if the results are to be at all rigorous.&apos; The idea, first proposed by Wheeler and 1reland2 of determining the yield locus by means of six Knoop hardness impressions along the principal directions in a material has obvious appeal. It is simple, quick, and should be applicable to very thin sheets. If such a technique could be demonstrated to produce consistently reliable results, it would be of interest to both researcher and designer. Lee, Jabara, and ackofen have compared the yield locus determined by Knoop hardness measurements (the Khn locus) to a locus determined by more rigorous techniques. They found good agreement for two titanium alloys at a plastic strain of about 1 pct. The purpose of this paper is to investigate if the Khn locus construction is a reasonable approximation to the locus of a highly anisotropic material. Examples of such materials are magnesium and magnesium alloys which have severely distorted yield loci which in turn reflect markedly dfferent yield strength in different directions.&apos; In pure magnesium, for example, the yield stress in tension along the transverse direction may be four times the yield stress in compression in the same direction and twice the tensile yield stress in the rolling direction. Predicting such large differences ought to serve as a severe test of the Khn locus construction. EXPERIMENTAL PROCEDURES Samples of rolled sheet, 0.250 in. (6.35 mm) thick, of pure magnesium and four magnesium alloys (Mg experimental materials. The pure magnesium together with the lithium and thorium alloys were those used in the study of Kelley and Hosford. The grain size was ASTM number 4 for the pure magnesium and number 6 for the alloys. HARDNESS TESTING The materials were sectioned along the rolling and transverse planes, mounted in a quick setting resin, and mechanically polished. Most of the hardness tests were performed on a surface prepared by electro-polishing (30 pct nitric acid in methanol at 0°C and 20 v) with the exception of the AZ31B and EK00 alloys which were made directly on a metallographically polished surface. However, subsequent hardness tests on the same sample after heavily electropolishing, revealed essentially the same hardness as before. At least twenty Knoop hardness impressions under a 100-g load were made in each of the six orientations shown in Fig. 1. The average hardness number and standard deviation were then calculated for each orientation. CONVENTIONAL LOCUS CONSTRUCTION Yield loci were constructed using a technique described in detail by Lee and ackofen,&apos; in which the flow stress (stress at a given plastic strain) fixes the coordinates of a point on the locus and measurements of the strain ratio serve to establish the slope of the locus at that point. The loading paths which correspond to uniaxial tension or compression tests establish the four intercepts of the locus with the coordinate axes plus one point on the balanced biaxial tension line Tensile testing was performed along the rolling and transverse (r, t) directions. Samples had a uniform rectangular gage length 1 by 4 by 4 in. (25.4 by 6.35 by 6.35 mm) and were deformed at a strain rate of 3.33 x 104 sec-&apos;. The tests were interrupted periodically to unload the sample and measure the plastic strains by means of X-Y post yield strain gages. Compression tests in the rolling, transverse, and through-thickness (r, f, z) directions were performed on 1/4 in. (6.35 mm) cubes at an initial strain rate of 8.33 x sec-&apos;. Lubrication was provided by 0.002 in. (51 pm) Teflon sheet which was renewed after unloading for micrometer measurements used to calculate the strains.

Jan 1, 1970

By R. F. Hehemann, R. H. Goodenow

Thermal arrest, hot-stage microscopy, and transtnission electron microscopy techniques have been employed to study the transformations in low-carbon iron and Fe-9 pct Ni alloys. In continuous cooling experiments, each alloy transforms at an essentially constant temperature for cooling rates below the critical rate required for martensite formation. However, high-tenzperature transformation in pure iron takes place by a different mechanism than that in the 9 pct Ni alloys. Pure iron exhibits an equi-a a structure with a low and random dislocation density while the 9 pct Ni alloy exhibits a cell or lathlike substructure analogous to that of low-carbon martensite. This same substructure characterizes upper bainite in higher-carbon inaterials. UNTIL relatively recently, diffusionless transformations have been considered to take place by the same mechanism and have been termed mar-tensitic transformations.l-3 The most characteristic feature2 of this mode of transformation is the shape change produced by a shear deformation and growth of the product phase frequently occurs at an extremely high velocity approaching that of an elastic wave.4&apos;5 A different mechanism of diffusionless transformation was recognized first in Cu-Ga and other copper-base alloys.6,7 From the absence of surface tilting in these alloys, it has been concluded that transformation is not accomplished by the cooperative shear displacements that occur in mar-tensitic reactions. Transformation presumably takes place by the rapid movement of an incoherent interface which is capable of propagating across parent grain boundaries. Although the transformation is diffusionless in the macroscopic sense, advancement of these interfaces is accomplished by an atom by atom rearrangement. Transformations of this type therefore require thermal activation and are generally operative only at high temperature. Although requiring short-range diffusion at the interface, propagation still occurs so rapidly that the reaction cannot be suppressed with normal cooling rates.7 The resulting microstructures exhibit large, irregular-shaped regions of the product phase, which are essentially free of crystallographic features. Consequently, these reactions have been termed massive transformations. Transformation by the massive mechanism has been reported to occur in ferrous systems involving pure iron and binary alloys of iron with nickel, chromium, and silicon by Gilbert and owen.&apos; The Fe-Ni system is of special interest in that the massive transformation was observed in alloys with less than 15 pct Ni while alloys having more than about 28 pct Ni transformed by the conventional mar-tensitic mechanism. By employing cooling rates substantially higher than those used by Gilbert and Owen, Swanson and Parr have been able to suppress the massive transformation in alloys with 0 to 10 pct Ni9 and produce martensite as revealed by surface relief. The massive transformation in the alloys having less than 15 pct Ni was identified by the lack of surface relief and an irregular rather than clearly acicular microstructure.&apos; Speich and Swann, using thin-foil electron microscopy, identified three distinctly different structures10 in quenched binary Fe-Ni alloys. From 0 to 4 pct Ni the structure consisted of blocky grains of a with a low and random dislocation density. Alloys with 4 to 25 pct Ni exhibited a cell structure with a high dislocation density; and at greater than 25 pct Ni the structure consisted of internally twinned plates. The structural change at approximately 4 pct Ni suggests that alloys with low nickel content transform by a different mechanism than those with intermediate nickel contents and the transition from the cellular to the internally twinned structures at approximately 25 pct Ni is analogous to the transition from needles to internally twinned plates that occurs over a narrow range of carbon contents in Fe-C martensites.11,12 Conventional bainitic and martensitic modes of austenite decomposition operate in ternary Fe-C-Ni alloys having less than 10 pct Ni. This investigation was conducted in order to explore the conditions under which the massive, bainitic, and martensitic transformations occur and the relationships between these modes of decomposition.

Jan 1, 1965

By R. Silverman, H. Blumenthal

It was found that despite the similarity of chemical analyses of different titanium carbides used as base materials for cermets, the physical properties, especially transverse-rupture strengths, of test bars were different. Hence this metallographic study attempts to link physical properties to micro-structures. It is shown that microstructure, grain shape, and grain growth are functions of three interrelated factors: 1—powder production procedure, 2—surface conditioning of the particles, and 3—impurities either contained in the original powder or acquired during ball milling. An explanation is offered for the "coring effect," long observed, but heretofore of unknown origin. The explanation is based on assumption of an oxide film and on chemical analyses which substantiate these findings. TITANIUM carbide has become in recent years a material of great interest in the high temperature field. Consequently, many manufacturers in the United States and Europe are producing titanium carbide for cermet applications as well as for additions to the well known tungsten carbide tools. All present commercial processes of titanium carbide production utilize the chemical reaction of titanium dioxide and carbon to form as nearly as possible stoichiometric Tic. This reaction is carried out in three ways: 1—in a menstruum of molten metal,&apos; 2—in the solid state, either in a protective atmosphere2 or in vacuum;" or 3—in an are-melting operation. In spite of the fact that the pure carbides obtained in these operations are almost identical chemically, the physical properties vary considerably when they are combined with a binder (Ni, Co) to form cermets. This fact led the authors to examine metal-lographically nickel-bonded titanium carbide in order to find the possible reasons for this behavior. Materials and Methods Five different titanium carbides were used in this investigation. They are identified in Table I. The first four materials were used in the as-received condition. Material E, received in lumps, was crushed to —100 mesh and carried through a flotation process in order to bring its graphite content in line with the other products. A Galagher flotation cell was used with pine oil as frothing agent. The chemical analyses of the investigated materials are given in Table 11. The binder used was carbonyl nickel of 9 to 14 microns particle size, supplied by A. D. Mackay. The materials were ball milled at a ball to charge ratio of 6:1 using procedures described under "Experiments and Results." All particle sizes mentioned are averages determined with a Fisher Sub-sieve Sizer. Test bars (lx0.40x0.16 in.) were prepared by 1—hot pressing to 85 to 95 pct of theoretical density at pressures between 1 and 1½ tsi and temperatures from 1600" to 1800°C, 2-—-cold presssing after 3 pct camphor had been added, or 3—wet pressing, both 2 and 3 at pressures between 5 and 10 tsi. All pressed bars were sintered in a vacuum of 105 to 10-6 mm Hg for 2 hr at 1350 °C. Transverse-rupture strengths were determined by breaking on a Baldwin Universal Testing Machine over a 9/16 in. span. Densities were measured by water displacement. The preparation of the specimens for micrographs was done according to Silverman and Doshna Luscz." All magnifications are at X1000. A sodium picrate electrolytic etch was used. Experiments and Results The influence of ball-milling procedure, ball-milling medium, pressing procedure, and sintering procedure on the microstructure of 80/20 — TiC/Ni were investigated. Ball Milling of Materials A, B, and C in a Steel Mill: Figs. 1 and 2 show microstructures of hot-pressed and vacuum-sintered test bars of materials A and B after the respective materials had been ball milled to 2.1 microns particle size in a steel mill and mixed with 20 pct Ni binder. Material A (Fig. 1) shows considerable grain growth. Also evident is a tendency of the carbide grains to coalesce. The density is 98 pct and the low transverse-rupture strength of 111,000 psi is probably caused by many large grains and an unfavorable packing factor. Almost all grains show a slight indication of "coring." Material B (Fig. 2), although showing grain growth, still has many small particles and a better distribution of binder and carbide due to the relative absence of the coalescing tendency. "Coring" can be observed in almost all grains. The high transverse-rupture strength of 179,000 psi and the density of 100 pct are believed to be due to the many small grains completely surrounded by the binder phase. There is also a preference to form spherical grains with material A, while most grains of material B preserve their angular shapes. Material C, of which no picture is given, stays between A and B in every respect. Rounding of some grains can be observed as well as coring, but the latter to a lesser degree than with material B. Its densification is good and the transverse-rupture strength obtained is 142,000 psi. Ball Milling of Materials A, B, C, and E in a WC Mill: When the Tic powders were ball milled to 2 microns particle size in a we mill, then ball-mill mixed with 20 pct Ni binder, hot pressed, and vacuum

Jan 1, 1956

By A. U. Seybolt, V. A. Phillips

Binary iron alloys containing 1 pct of Al, Cr, Mn, Mo, Si, Ti, or V, and 0.4 pct C, 1 pct Cr steels with and without 1.2 pct A1 or 2.0 pct Ti additions, were ion-nilrided at 550° to 600° in N-H mixtures. Nitriding increased the inicrohardne ss of all the binary alloys except those containing manganese or molybdenutn, and also hardened the heat-treated steels if aluminum or titanium urns present. Transmission electron microscopy revealed particle formation in all casts where hardening occurred. Electron diffraction gare positive identifications for ALN, CrN, and a, Si3N4 in the binary alloys, and AlN and CrN in the aluminum- cold chromium-bearing steels, respectil&apos;uly. Cubic VN with a, = 4.13A was tentatively identified. Particles, apparently of CrN, also formed in the base steel but did not increase the hardness very much. Chromium and vanadium formed nitride platelets on {001}° matrix planes, while titanium gave clusters <15A diam. Aluminum nitride precipitated at grain and subgrain boundaries, and within the grains. Silicon gave profuse precipitates of several Morphologies at grain boundaries and cubical particles within the grains. No effect of the alloy carbides on nitride precipitation was observed in the heat-treated steels. THE nitriding of steel has been a well-established commercial process for about 40 years, but in spite of this comparatively long period of use there have been few studies aimed at understanding the process. Most studies, like the early but very competent work of Jones and organ&apos; and nones.&apos; were concerned with establishing the pertinent engineering variables of steel composition, gas composition, temperature, and time. As far as the present authors are aware, there have been no studies of the composition, size, shape, or distribution of the nitrides formed in the nitriding of steel. Noren and Kindbom3 did, however, examine a few nitrided steels by surface replica electron microscopy, and were able to show the presence of car-bonitrides and AlN and TiN nitrides. pitsch4,5 and Hrivnak6 examined nitrided pure iron by transmission electron microscopy. Baird7 found manganese nitrides in Fe-1.6 pct Mn when nitrided at 650°C, using the same technique. In the present work, emphasis was placed on transmission electron microscopy because of its inherently better resolution, using principally binary alloys of iron containing 1 pct of alloying element. In addition, a few simple 0.4 pct C steel compositions were examined to investigate possible carbonitride formation. It was not anticipated that all of the added elements would form nitrides under the conditions used, but it was considered desirable to obtain direct experimental evidence on this point. It would be considerably easier to ascertain the presence of alloy nitrides by examining appropriate binary alloys in preference to relatively complex steels. The work reported here could have been done using orthodox ammonia-nitriding procedures, but an operating ion-nitriding equipment was available, and was therefore used for specimen preparation. EXPERIMENTAL DETAILS 1) Materials. Binary alloys were made up from vacuum-melted electrolytic iron with 1 wt pct additions of Cr, Ti, V, Al, Mn, Mo, and Si of about 99.9 pct purity. In addition, three steels were similarly made up—a basis steel with 1 wt pct Cr and 0.4 wt pct C and two steels with further additions of 1.2 wt pct A1 or 2.0 wt pct Ti, respectively. The materials were vacuum-melted and cast as 11-lb heats into tapered square molds of about 2 by 2 in. average cross section. The castings were forged and hot-rolled to 11/4 in. rounds. Discs of 4 in. thickness by about 1 in. diam were machined from the rods. Some of these discs were hot-forged and hot-rolled to about 0.020 in. thick, sand-blasted, and then cold-rolled to about 0.003 in. thick. At this point, the surface was cleaned by light etching with HC1, then washed, dried, and vapor-degreased prior to nitriding. 2) Ion-Nitriding Procedure. The type of ion-nitriding equipment used here is similar to that described by Jones and Martin.8 Briefly, a mixture of nitrogen and hydrogen at 5 mm total pressure is placed in a vacuum chamber with a dc potential of 450 to 500 v applied between the work (cathode) and the grounded metal vacuum enclosure (anode). Nitrogen ions are accelerated to the work where a thin layer of Fe4N forms on the surface and thus sets up a nitrogen concentration gradient. This causes nitrogen atoms to diffuse into the surface layers of the alloy forming a finely divided dispersion of alloy nitrides, causing hardening of the surface. In the work to be reported here. the nitriding was carried out at 550° to 600°C to be consistent with commercial nitriding practice. The temperatures cited are those measured by a thermocouple located under a platform on which the work was sitting. Except where otherwise stated, the mixture used in nitriding the binary alloys contained -2.0 pct N, balance hydrogen. The nitrogen concentration in the nitriding gas mixture used for the binary alloys was purposely kept lower than normally used in nitriding steels. 10 to 20 pct, in order to minimize Fe4N formation. In this way only the alloy nitrides would be present as a second phase. However, in the case of steels which would contain a- carbide phase along with as

Jan 1, 1969

By E. E. Underwood, L. L. Marsh

Aluminum single crystals, alloyed with 0.042 atomic pet Cu and 0.11 and 1.1 atomic pct Mg, were subjected to constant stress creep tests, tensile tests, and hot hardness measurements within a temperature range of 300° to 866OK. Calculations based on Dorn&apos;s temperature-compensated time parameter, 6, gave a value of DH, = 27,000 cal per mol for the activation energy of early creep in aluminum single crystals. Correlations have been obtained for aluminum alloy single crystals with the parameter E for solid solution strengthening, as well as with the parameter F for solid solution hardening, by using a valence of three for aluminum. Limited measurements on tensile specimens show that the slip band density tends to decrease with increasing temperature and with decreasing solute concentration. INCREASING interest is being shown in the mechanisms of plastic deformation in single crystals during tensile and creep testing. The complexity of deformational processes in polycrystalline materials has led to a search for simpler experimental conditions. Numerous creep and tensile investigations have been conducted with pure, metallic single crystals. To a lesser degree, the effects of alloying elements on the tensile properties of single crystals have been determined. However: the literature dealing with the effects of alloying additions in single crystals under creep conditions is vanishingly small. This paper represents an attempt to narrow this gap in the knowledge of the subject. Previous investigations of creep behavior at the Battelle Memorial Institute1-1 have been of great value in the analysis of the present single crystal data. It is equally desirable, however, to ascertain the extent of correspondence between the behavior of single crystal and polycrystalline materials. For this purpose, correlations, similar to those developed for polycrystalline aluminum alloys by Dorn and co-workers, have been made with the single crystal data. The results from this study have tended to confirm and extend those correlations to the case of alloyed single crystals. Materials and Procedures Three dilute binary aluminum alloys were prepared for this investigation from 99.99 + wt pct Al, 99.8 wt pct Mg, and 99.92 wt pct (electrolytic) Cu. The nominal compositions of the alloys were 0.042 atomic pct Cu, and 0.11 and 1.1 atomic pet Mg. Precautions were taken to avoid contamination of the stock during melting and casting of the alloys. After a heat treatment of 8 hr at 925°F the alloys were extruded, then machined into) threaded tensile specimens with a 3 in. reduced section and a 0.505 in. diam. Spectrographic examination showed less than 47 ppm metallic impurities in each alloy. The single crystals were grown by the strain-anneal method, with a critical strain of about 11/4 pet giving the optimum results. In general, 3 in. crystals were obtained with the Al-Cu alloy, but smaller crystals in the magnesium alloys necessitated the use of 2 in. and 1 in. gage lengths with the low and high magnesium alloy specimens, respectively. After an electrolytic polish, the orientation of that portion of the specimen containing the largest single crystal was determined from Laue back-reflection photographs. Tensile tests were conducted at a constant load rate of about 2 lb per min. Creep runs were made in a constant temperature room, under constant stress at the higher creep temperatures, and constant load at the lower temperatures. The eloneation was measured to within ±5 microin. by a specially designed capacitance extensometer. The ex-tensometer arms were attached to the 3 in. specimens at the shoulders of the test piece or, where the crystals were smaller than 3 in., by knife-edge grips.

Jan 1, 1957

R,. P. JaRvis,* El Oro, Estado de México, México.—The practical problem raised by Mr. Wisser—that is, the determination of the lower limit of ore deposition, below which it is useless to look for ore shoots—is one of the most important in economic geology. He asks: "Can we learn to determine the position of such a line?" For individual districts, yes; but its determination has always been by empirical methods; that is by actually exploring the veins to such depths that the values drop below the economic limits. Usually the signs are plain enough that values have been bottomed without confirmation by the chemist or assayer. Most veins, when approaching their limit, begin to split into branches or stringers; the vein matter itself undergoes a change from "lively looking" rock to one that is dull and unpromising, the quartz, instead of having segregated into clean vein matter, has simply spread itself into the country rock, rendering this more siliceous but no richer—these, together with inclusions of the country rock in the vein, are all positive indications of the limit. Mr. Wisser seems disposed not to accept the law of cause and effect, which he calls "empiricism." He says: "Empiricism embodies an assumption perhaps not evident at first glance. It is this: that like effects spring from like causes and therefore necessarily have a common meaning." There can be no doubt as to the validity of this law, since it is the foundation stone upon which are built all inductive sciences, including economic geology. When demonstrable, proved facts become confused with inferences, as they seem to be generally in the paper under examination, no sound conclusions can be reached. Mr. Wisser has failed to give sufficient data covering the two vein systems which he cites as examples. Presumably they are situated in the Pachuca District of Mexico, but not everybody is familiar with the vein systems there in spite of the fact that it is world famous as a silver producer. Are these two systems separated some distance horizontally from one another and how far? He has given no estimate of the amount and kind of rock that has been eroded from over the present veins. His description of the two systems appears on page 100, beginning: "1. East-west veins," and ends on page 101, "they would lack spaces there in which to deposit." On page 101, with the paragraph beginning "On the other hand," he gives a picture of what he believes takes place in class 2 veins. The sum of this seems to be, according to Mr. Wisser&apos;s observations, that, in the east-west veins, class 1, there has been an invasion of an "altering solution," which I judge has been responsible for the formation of extensive "alteration haloes"; that these alteration solutions have followed along pre-existing fractures or fissures; and that after these alteration solutions finished their work the mineralizing solutions deposited the vein matter and metallic values. Mr. Wisser does not specify clearly what the "alteration haloes" consist of; in other words, what change the original rock has suffered, whether oxidizing, carbonating, or sulphidizing. If they came from depth they could not be oxidizing or carbonating, and in this case it is a bit

Jan 1, 1941

R,. P. JaRvis,* El Oro, Estado de México, México.—The practical problem raised by Mr. Wisser—that is, the determination of the lower limit of ore deposition, below which it is useless to look for ore shoots—is one of the most important in economic geology. He asks: "Can we learn to determine the position of such a line?" For individual districts, yes; but its determination has always been by empirical methods; that is by actually exploring the veins to such depths that the values drop below the economic limits. Usually the signs are plain enough that values have been bottomed without confirmation by the chemist or assayer. Most veins, when approaching their limit, begin to split into branches or stringers; the vein matter itself undergoes a change from "lively looking" rock to one that is dull and unpromising, the quartz, instead of having segregated into clean vein matter, has simply spread itself into the country rock, rendering this more siliceous but no richer—these, together with inclusions of the country rock in the vein, are all positive indications of the limit. Mr. Wisser seems disposed not to accept the law of cause and effect, which he calls "empiricism." He says: "Empiricism embodies an assumption perhaps not evident at first glance. It is this: that like effects spring from like causes and therefore necessarily have a common meaning." There can be no doubt as to the validity of this law, since it is the foundation stone upon which are built all inductive sciences, including economic geology. When demonstrable, proved facts become confused with inferences, as they seem to be generally in the paper under examination, no sound conclusions can be reached. Mr. Wisser has failed to give sufficient data covering the two vein systems which he cites as examples. Presumably they are situated in the Pachuca District of Mexico, but not everybody is familiar with the vein systems there in spite of the fact that it is world famous as a silver producer. Are these two systems separated some distance horizontally from one another and how far? He has given no estimate of the amount and kind of rock that has been eroded from over the present veins. His description of the two systems appears on page 100, beginning: "1. East-west veins," and ends on page 101, "they would lack spaces there in which to deposit." On page 101, with the paragraph beginning "On the other hand," he gives a picture of what he believes takes place in class 2 veins. The sum of this seems to be, according to Mr. Wisser&apos;s observations, that, in the east-west veins, class 1, there has been an invasion of an "altering solution," which I judge has been responsible for the formation of extensive "alteration haloes"; that these alteration solutions have followed along pre-existing fractures or fissures; and that after these alteration solutions finished their work the mineralizing solutions deposited the vein matter and metallic values. Mr. Wisser does not specify clearly what the "alteration haloes" consist of; in other words, what change the original rock has suffered, whether oxidizing, carbonating, or sulphidizing. If they came from depth they could not be oxidizing or carbonating, and in this case it is a bit

Jan 1, 1941