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By R. T. Hukki

This paper presents a preliminary analysis of the fundamental relationship between the net energy used and the respective product size throughout the entire range of sizes covered by crushing and grinding, and an attempt to find a sensible correlation between the existing theories. Walker, Lewis, McAdams, and Gilliland' have given the following differential equation of a general form for comminution: dE = -C§ [1] where E is the net energy required per unit weight in a certain process of comminution; x is the factor indicating the fineness of the product; n is the exponent indicating the order of the process, and C is a constant related with the material, units chosen, etc. H exponent n in the above equation is replaced by numerical figures 2, 1, and 1 1/2, the integrated form of the general equation leads to the well known fundamental theories represented by the law of von Rittinger,' law of Kick, and the third theory of comminution by Bond, respectively. The total net energies (E) from infinite feed size to a product of size x are as follows: The net energy required in a certain process of comminution is proportional to the new surface developed according to the law of von Rittinger, to the weight or size of the bodies treated according to the law of Kick, and to the length of the new cracks formed which initiate breakage according to the theory and explanation by Bond. On a logarithmic paper, where particle size is presented on the abscissa and energy consumption on the ordinate (see Fig. 21, all three relationships are represented by straight lines. The slope m of the line according to the law of von Rittinger is equal to -1.0; of Kick, 0; and of Bond, -0.5. Experimental evidence in favor of the law of Rittinger has been presented, e.g., by Gross and zimmerley5 on quartz crushed in a drop weight crusher and evaluated for surface by the method of dissolution, by Dean on magnetite crushed by a similar method and evaluated for surface by the determination of coersive force, by piret7 and co-workers on a group of minerals crushed again by a similar method as well as by compression and evaluated for surface by permeability and gas adsorption methods, and by schellinger8 on a group of minerals ground in a calorimetric ball mill and evaluated for surface by gas adsorption. Experimental evidence in favor of the law of Kick seems to be scant in the field of comminution. On the other hand, in the field of mechanical engineering Kick's law seems to be of fundamental nature in processes such as cutting, pressing, shaping, and rolling of metallic substances. Experimental evidence in favor of the third theory has been provided by Bond." To a large extent, data are based on the vast amount of grindability tests performed in the laboratories of Allis-Chalmers Manufacturing Co. In addition to the devoted proponents of one or the other of the basic theories listed above, certain investigators have indicated that one of the theories might be applied for a certain range of sizes, while another theory might be used for other sizes. In a discussion of a paper by Bond," Dobie" presented a statement at the International Mineral Dressing Congress in London (1952) indicating that 1) for large particles, the law of Kick was approximately correct; 2) for finer particles, von Rittinger's suggestion was nearer to the truth; and 3) Bond's new

Jan 1, 1961

By C. S. Land

Relative permeability functions are developed for both two- and three-phase systems with the saturation changes in the imbibition direction. An empirical relation between residual nonwetting-phase saturation after water imbibition and initial nonwetting-phase saturations is found from published data. From this empirical relation, expressions are obtained for trapped and mobile nonwetting-phase saturations which are used in connection with established theory relating relative permeability to pore-size distribution. The resulting equations yield relative permeability as a function of saturation having characteristics believed to be representative of real systems. The relative permeability of water - wet rocks for both two- and three - phase systems, with the saturation change in the imbibition direction, may be obtained by this method after properly selecting two rock properties: the residual nonwetting-phase saturation after the complete imbibition cycle, and the capillary pressure curve. INTRODUCTION Relative permeability is a function of saturation history as well as of saturation. This fact was first pointed out for two-phase flow by Geffen et al. 1 and by Osaba et a1.2 Hysteresis in the relative permeability-saturation relation also has been reported for three-phase systems.3 Since saturations may change simultaneously in two directions in a three-phase system, four possible relationships arise between relative permeability and saturation for a water-wet system. The four saturation histories of this system were given by snel14 as 11, ID, DI and DD. I and D refer to the direction of saturation change (imbibition and drainage), with the first letter of the symbol indicating the direction of change of the water phase. As used in this paper, the second letter of the symbol refers to the direction of saturation change of the gas phase, i.e., D and I indicate an increase and decrease, respectively, in gas saturation. Only a few three-phase relative permeability curves have been published. Leverett and Lewis5 published three-phase curves for unconsolidated sand, and Snell4 reported results of several English authors for both drairrage and imbibition three-phase relative permeability of unconsolidated sands. Three-phase relative permeability curves for a consolidated sand were published by Caudle et a1.3 for increasing water and gas saturations (ID). Corey et a1.6 reported drainage (DD) three-phase relative permeability for consolidated sands. Recently, Donaldson and Dean7 and Sarem8 calculated three-phase relative permeability curves from displacement data on consolidated sands, also for saturation changes in the drainage direction. The only published three-phase relative permeability curves for consolidated sands with saturation changes in the imbibition direction (11) are those of Naar and Wygal.9 These curves are based on a theoretical study of the model of Wyllie and Gardner 10 as modified by Naar and Henderson.11 Interest in three-phase relative permeability has increased recently due to the introduction of new recovery methods and refinements in calculation procedures brought about by the use of large-scale digital computers. The scarcity of empirical relations for three-phase flow, and the experimental difficulty encountered in obtaining such data, have made the theoretical approach to this problem attractive. RELATIVE PERMEABILITY AS A FUNCTION OF PORE-SIZE DISTRIBUTION Purcell used pore sizes obtained from mercury-injection capillary pressure data to calculate the permeability of porous solids.12 Burdine extended the theory by developing a relative permeability-pore size distribution relation containing the correct tortuosity term.13 The works of Purcell and Burdine were combined by Corey14 into a form that has

Jan 1, 1969

By D. F. Stoneburner

The thermoelectric power and electrical conductivity of a series of liquid alloys of thallium were determined in order to study the relation of chemical bonding to semiconduction in liquids. The results indicate metallic behavior for the alloys of thallium with arsenic, antimony, and bismuth, while the sulfides, selenides, and tellurides indicate semiconduction. The results are compared with the Properties of the same alloys in the solid state. This work supports the observation that long-range order is not a necessary requirement for semiconduction. PREVIOUS work1,5 has shown that some sulfides and oxides behave as semiconductors in the liquid state. Although the band theory has been of great help in understanding the properties of solid semiconductors, its quantitative application to liquids is difficult. The very existence of liquid electronic semiconductors shows that ascribing the discrete structure of the energy spectrum to strict lattice periodicity, or long-range order, is not always satisfactory. Rather, the short-range order determines the structure of energy levels and the width of the forbidden gap and, consequently, the concentration of free holes and electrons. This is borne out by the analysis of data accumulated by Regel and coworkers.6 The similarity of electronic structure of liquid and solid phases of certain liquid metals was pointed out by Knight et a1.,7 who examined nuclear resonance in solid and liquid Li, Na, Rb, Cs, Mg, Al, Ga, Sn, and Bi. They found noticeable changes in the electronic structure upon melting only in the cases of bismuth and gallium. They concluded that "a liquid metal possesses a band structure which is very like that of the solid, provided the short-range structure is not altered during melting." In semiconductors in which the near-neighbor arrangement remains the same on fusion, the material would be expected to retain its semiconducting properties. The quantum theory of semiconductors, with its band structure of energy levels, is linked exclusively to long-range order. Furthermore, it has limited usefulness in predicting new semiconductors. Many sulfide8-12 have made comparisons of properties on the basis of crystal structure or the position in the periodic table, both methods involving the same factors as chemical bonding. Mooser and Pearson8"10 have pointed out that crystal structure depends on chemical bonding, and that this bonding is a property of the atoms themselves. As the periodic arrangement of the atoms offers an easy comparison of such factors as atomic weight and number of valence electrons it provides clues to expected similarities of bonding for various elements or groups of elements. This approach has led Mooser and Pearson to formulate their valence-bond theory of semiconduction, in which they define a semiconducting bond. These authors state that "semiconductivity is the result of the presence in a solid of predominantly covalent bonds. These lead, through the process of electron sharing, to completely filled s and p orbi-tals in the valence shells of all atoms of elemental semiconductors while in semiconducting compounds only one atom of any two bonded together need acquire closed s and p orbitals. The presence of empty 'metallic' orbitals in some atoms of a compound does not destroy the semiconductivity provided that these atoms are not bonded together; it may, however, give rise to pivoting resonance in

Jan 1, 1965

By Noel Jarrett, Allen S. Russell, Bernard M. Starner, Stanley C. Jacobs

A process has been developed to refine high-grade commercial aluminum to 99.99 pct purity. This enzploys precipitating titanium, vanadium, and zirconiu~ as borides. The upgraded liquid is partially crystallized under conditions that prevent massive freezing. The resulting crystals are compacted and washed free of adhernig impure liquid aluminum by melting the top crystals while draining off the liquid. Finally, the bottorn portion of the crystal bed is melted and removed as the pure product. Leakage from the crystallizat~on vessel is prevented by a layer of alumina granules that are not wetted by the aluminum. ALUMINUM of 99.99 pct purity is desired in a variety of applications. These include electrolytic capacitors, catalyst carriers, decorative trim for automobiles, aluminum powder, and high-strength alloys. This market was for many years filled by refining commercial-purity aluminum in a three-liquid-layer electrolytic cell of the type originally proposed by Hoopes. To meet the expanding need for lower-cost high-purity aluminum, a refining process based on chemical precipitation and fractional crystallization was developed. The availability of this super-purity metal was announced in November 1961, and three patents1-3 relating to the process were issued in 1965. An alternate process, comprising continuous fractional crystallization of a portion of a liquid-aluminum feed stream under conditions of strong agitation at the surface of the growing crystals, was published by Dewey4 in 1965. Earlier proposals by Larsen 5 and by Regner6 also emphasized the advantage of rapid agitation of the melt in the region of the crystallization zone. johnson 7 more recently proposed extracting purified aluminum from an alloy by mixing crystals of pure aluminum into the molten alloy, allowing them to grow, and removing the pure aluminum as by casting. Aamot's 8 recent patent describes a freeze refining process that involves controlled partial freezing against cooled moving retort walls. The Alcoa process to produce high-purity aluminum is schematically described in Fig. 1. Relatively pure aluminum is treated with boron in a furnace (a) to precipitate high melting point impurities, the supernatant liquid is transferred to a crystallization vessel (b), the liquid is partially crystallized with mechanized "tamping" (c), the remaining impure liquid is tapped out and the crystal bed partially and directionally re-melted to wash the underlying crystals (d), and the balance of the crystals is melted and withdrawn as high-purity aluminum (e). PRINCIPLES OF FRACTIONAL CRYSTALLIZATION Commonly encountered impurity elements form two types of systems with aluminum. Titanium, vanadium, and some other transition elements in periodic groups IV, V, and VI are the high melting point impurities. Initial solidification of aluminum containing small percentages of these elements will produce solid markedly enriched in them at temperatures slightly above the freezing point of high-purity aluminum. Most other elements, such as silicon and iron, produce eutectic type reactions with aluminum. In this case the first solid formed on initial solidification at temperatures slightly below the freezing point for high-purity aluminum is markedly depleted while the remaining liquid is enriched in these elements. The equilibrium change in composition during solidification of aluminum contaminated with silicon, iron, or titanium is illustrated in Fig. 2. Here, for clarity, the temperature scale is expanded beyond the

Jan 1, 1968

By A. M. Adair

The effect of cathodically charging zone-refined iron with hydrogen and the resultant yield stress-grain size relationship has been investigated by tensile testing at -31°C. The resulting Petch plots (using a least-squares analysis) reveal a significant reduction in the slope and an increase in the intercept for specimens cathodically charged with hydrogen, regardless of whether the hydrogen is present during testing or is removed by evacuation. Other than surface blistering, the major effect of cathodically charging this material is to create occasional grain boundary cracks and thus presumably a large number of free dislocations at grain boundaries. These results are consistent with the hypothesis that the slope of the Petch plot is related to the stress required to activate dislocation sources at or near pain boundaries. While there is no significant effect of the presence of hydrogen on the lower yield stress of this material, the ductility is considerably reduced. After hydrogen removal by evacuation, the ductility recovers substantially and almost complete recovery of ductility is experienced by the smaller grain size specimens. THE influence of hydrogen on the mechanical properties of ferritic materials has received much attention throughout the history of the metallurgy profession. This interest has stemmed from the obvious importance of preventing the catastrophic failure of parts in service, and from the desire to determine what mechanism is responsible for the observed behavior. The various mechanisms proposed for hydrogen em-brittlement have been discussed in detail by Tetel-man,'who concludes that a combination of the applied stress and hydrogen pressure within voids best accounts for the many experimental observations reported. From a quite reasonable correlation of the strain aging and delayed-failure behavior of a variety of materials,2-7 Troiano and coworkers are of the opinion that the delayed-failure mechanism (slow strain rate embrittlement as well) is better explained as a lattice effect; solute elements diffuse to regions of high triaxial stress, form uncondensed atmospheres there, and effect a reduction in the cohesive strength of the lattice. Since hydrogen yield points8,9 have been observed in ferritic materials, and since the hydrogen embrittlement process may be related to strain aging, one further contribution to embrittlement could be hydrogen-dislocation interactions which make crack blunting by plastic deformation a more difficult process. The etch" relationship offers a means of comparing the relative ease of initiating and propagating plastic deformation in metals and alloys. In the present study, this relationship was used to compare the behavior of zone-refined iron in three conditions: uncharged, cathodically charged with hydrogen, and cathodically charged with hydrogen and evacuated. These Petch plots and the observed ductility parameters allowed a separation of the effects of the very presence of hydrogen and the act of cathodically charging hydrogen into this material. MATERIALS AND EXPERIMENTAL PROCEDURE An ingot of zone-refined iron was obtained from Battelle Memorial Institute which contained the following (typical) interstitial impurities in ppm: carbon, 10 * 5; nitrogen, 1; oxygen, 22; hydrogen, 0.9. The ingot was cold-reduced to a 1/2-in.-sq cross section, recrystallized 1 hr at 575°C, and then straight-rolled to a thickness of about 0.105 in. Tensile specimens were milled from the strip having a 1-in. gage length

Jan 1, 1967

By J. C. Scully, G. Sanderson

The electrolytic formation of y hydride in thin foils of Ti-5Al-Z.5Sn alloy and four Ti-A1 binary alloys has been studied by electron microscopy and electron diffraction. Two orientation relationships have been found: THE adsorption of hydrogen by titanium alloys from aqueous solutions has been widely reported. This can occur, for example, in both alkaline' and acidic2 pickling baths, in chemical polishing374 and electro-polishing Solutions,3,4 during cathodic polarization5" and under certain corrosion conditions,7,8 Etching reagents may also produce visible precipitates, sometimes after an aging period.9 During an investigation into the stress corrosion susceptibility of a titanium alloys by thin foil electron microscopy many observations have been made of hydride precipitation which has been deliberately promoted by techniques that are described below. The characteristics of hydride precipitation are reported and the observed crystallographic orientation relationships are discussed with reference to distortion in the titanium lattice created by the presence of the hydride. EXPERIMENTAL TECHNIQUE One grade of commercial titanium and five alloys were examined. Their composition and hardness values are shown in Table I. All the materials were in the form of thin sheet, 0.05 to 0.065 cm thick, which had been annealed after cold rolling. Foils suitable for transmission electron microscopy were made in two ways: a) by chemical polishing; and b) by elec-tropolishing. The solution used for chemical polishing was a mixture of 44 pct HF and 73 pct HNO3 in the volumetric ratio 2:3. During this polishing specimens were manually moved up and down in the solution. The reaction was veFy rapid, specimens thinning to foil thickness (2000A) in 5 min. Since chemical polishing solutions tend not to cause hydride contamination if they are kept cool3 no attempt was made to prevent the solution from becoming hot during the thinning operation. Electropolishing was performed at -30° C with a mixture3 composed of 295 cu cm methyl alcohol, 175 cu cm n-butyl alcohol, and 30 cu cm perchloric acid with an applied voltage of 40 v after chemically thinning specimens to approximately 0.017 cm thickness in a cool solution of 44 pct HF, 40 vol H2O2, and water in the volumetric ratio 1:6:3. EXPERIMENTAL RESULTS 1) Ti-5A1-2.5Sn Alloy. The Ti-5A1-2.5Sn alloy was severely contaminated by hydrogen during the chemical polishing. Foils obtained in this way contained large amounts of the y hydride phase. A typical micrograph is shown in Fig. l. The laths were identified as the hydride phase by selected-area diffraction of a large number of foils examined in a tilting stage that could be turned through 40 deg. Using the lattice spac-ings of the alloy obtained by X-ray diffraction as a standard the a value of the hydride was determined fromo the electron diffraction patterns to be 4.38 to 4.40A. The accuracy of this figure is only about ±2 pct. Further evidence of the identification was obtained by vacuum annealing chemically polished foils of the alloy at 500°C. This resulted in the dissociation of the hydride with the production of dislocations and possibly vacancy loops as shown in Fig. 2. The hydride

Jan 1, 1968

By E. H. Rennhack, J. F. Libsch

Definite transition behavior was found in unalloyed titanium at 0.13 pct 0 equivalent. The addition of 0.5 Sn, 1.0 Al, 0.5 Al, and 1.0 Sn lowers the tvansition temperature of titanium at oxygen equivalents exceeding 0.22, 0.29, 0.40, and 0.51, respectively. Metallographic evidence indicates that progressive amounts of oxygen restrict deformation at low temperatures resulting eventually in brittle fracture. The presence of tin or aluminum is thought to alter the atomic distribution of oxygen within the titanium lattice in such a manner as to facilitate some degree of slip and twinning. 1 ITANIUM-like iron and zinc experiences a transition from ductile to brittle fracture with decreasing temperature. The presence of sufficient quantities of the interstitial elements, carbon, oxygen, and nitrogen in solid solution, has been shown to progressively lower the room-temperature impact resistance of titanium with increasing interstitial content.1"1 Ogden,et al,2 reported finding no transition from ductile to brittle fracture with decreasing temperature in iodide titanium. However, a definite transition was found to occur at 0.36 pct 0 equivalent in an alloy containing 0.47 pct carbon in solid solution. The oxygen equivalent in this case was obtained by assuming the effects of carbon, oxygen, and nitrogen in combination on the impact properties of titanium to be additive on the same basis as their separate effects on tensile strength, namely: Oe = 2/3 (pct C) + pet 0 + 2 (pet N) They concluded that the tendency toward transition behavior is dependent on the total interstitial content in solid solution and not on any one particular interstitial element. Rennhack,4 however, recently found transition behavior in iodide titanium at an oxygen equivalent of 0.17 pct. Ogden, etal3, reported that the strengthening effects of carbon, oxygen, and nitrogen in titanium decrease with the addition of tin. They showed that tin additions increase the tolerance of titanium for the interstitials, that is, 10 pct Sn permitted individual additions of up to 0.4 wt pct of the interstitial elements without any significant loss in ductility. Aluminum tends to decrease ductility and impact strength of titanium for a given interstitial ~ontent.3 Van Thyne and Kessler5 found that the solid solubility of carbon in titanium doubled in the presence of 10 pct Al. The precise effects of tin and aluminum in the nrespncp of rorvfen nn the impact properties of titanium had previously not been determined. The high oxygen tolerance of titanium containing tin may provide a suitable means for improving the impact properties of titanium containing the interstitial elements, particularly oxygen. Unlike tin, however, aluminum has a high affinity for oxygen and will reduce rutile titanium dioxide (TiO2)by a thermit-type reaction.6 Thus, the atomic distribution of oxygen in titanium might be different in the presence of aluminum. The present work was undertaken to: 1) Determine the effect of oxygen on the transition behavior of unalloyed iodide titanium. 2) Determine the effect of small amounts of tin and aluminum on the transition behavior of iodide titanium in the presence of oxygen and other interstitial~. EXPERIMENTAL Three different lots of iodide titanium were employed to prepare the alloys studied in the present work. Their chemical composition is presented in Table I. The compositions of the tin and aluminum used for alloying are shown in Table 11. Oxygen additions were made using calcined rutile titanium dioxide (TiO2)of 99.7 pct purity. Alloy Preparation—Four titanium-base alloys containing separate additions of 0.5 and 1.0 pct each

Jan 1, 1960

By Robert T. MacMillan

Of all the mineral substances utilized by man, salt or sodium chloride has one of the longest and most varied histories. Because all animal life is descended from marine organisms, sodium and chlorine became necessary to life, and as sodium chloride meets requirements most readily, common salt has been essential to human and animal diets from earliest times. As civilization progressed, man learned to evaporate sea water and brines of saline lakes and springs to obtain salt, and gradually ceased to depend on the flesh of animals and the occasional salt outcrops or "salt licks" they frequented. He also learned that salt had a multitude of uses, particularly as a preservative of meat and other foods. The importance of salt in the minds of early men may be readily seen from many allusions in the Bible and other ancient writings. Expressions such as "not worth his salt," and "the salt of the earth" are deeply embedded in the English language. Salt has symbolized friendship, fidelity, purity, and hospitality. It has been used as currency; had religious significance; caused wars; and has been a favorite commodity for taxation. The English word "salary" stems from the Latin word for salt, in which Roman soldiers received part of their pay. Although salt today retains its dietary importance, it has thousands of other uses. Of each 100 pounds produced in the United States less than three pounds is for table use. The other 97 pounds goes for agricultural, industrial, and chemical uses. Fortunately, reserves of salt are enormous and reasonably well distributed on the face of the earth. The sea is an inexhaustible source of salt which may be had at prices which vary with climate and other factors. In addition, large underground salt deposits and many salt lakes, springs and playas are scattered throughout the world. Most countries have access to a salt supply, although some are more favored than others. Properties Crystallized sodium chloride or common salt is known as halite. Its molecular weight is 58.454 and it contains, by weight, 39.34 pct sodium and 60.66 pct chlorine. Alternate positions in the cubic lattice are occupied, respectively, by negative chloride and positive sodium ions; the crystal form is isometric. Crystallization from water produces concentric shells, and when broken, a crystal shows conchoidal fracture. Salt has a hardness of 2.5; its specific gravity ranges from 2.1 to 2.6 for rock salt and is 2.165 for the pure crystal. The refractive index is 1.554; it melts at 800.8 ± 0.5°C and boils at 1413°C. Its heat of fusion is 123.59 cal/ gram. Salt is transparent or translucent and highly diathermous. It is colorless when pure and has a vitreous luster. Salt containing traces of iron oxides has varying shades of yellow, orange, brown, pink, or red. The peculiar shade of red sometimes found in that produced by solar evaporation of sea water has been attributed to tiny organisms. Blue mottlings sometimes seen in halite crystals have been attributed to colloidal sodium. Salt is soluble in water to the extent of 35.7 parts per 100 parts of water at 0°C and 39.8 parts per 100 of water at 100°C. The small difference in solubility with increasing temperature is important in the economics of producing salt by evaporating brine. Salt has a negative heat of solution which is 1.281 kg-cal/ mole at 18°C in 200 moles of water.

Jan 1, 1960

By H. P. Stuwe

It is investigated whether a model of sphere packing permits the computation of the lattice parameters and their variation with concentration in various a phases; it does, except in phases containing silicon. Several observations indicate that a particular role is played by the "E-atoms" in the lattice. THE phase is formed by many alloys of the transition elements.'-' Its structure has been described by Bergman and Shoemaker,5,8 Dickins, Douglas, and Taylor,7 and Kasper, Decker, and elanger.' There are five kinds of crystallographically equivalent positions for the 30 atoms in the unit cell which have been designated by these authors I, 11, 111, IV, and V or, in the same sequence, A, B, C,D, and E, as shown in Fig, 1. For the purposes of the present paper two elements of the lattice will be discussed separately: The lattice planes perpendicular to the c-axis which are made up by the atoms A, B, C, and D and which determine the a-parameter; and the close-packed "vertical rows" of E-atoms which determine the c-parameter. asper,9 and Frank and kasper10 described the a phase and other complex structures as sphere packings. In these papers particular attention is paid to the coordination polyhedra. Lattice positions with an equal number of nearest neighbors are considered equivalent regardless of their crystallo-graphic description. This seems to work very well for the explanation of ordering phenomena in the a phase as far as information on this is available." If the description of the phase as a sphere packing is valid it should be possible to draw two further conclusions: 1) It should be possible to calculate the lattice parameters from the atomic radii of the components, and 2) It should be possible to predict the variation of the lattice parameters with concentration within one phase field. Both points are discussed in this paper. PROCEDURE Measurements of lattice constants were done with a symmetrical back-reflection X-ray camera. With Cr-radiation, about a dozen a1 lines could be observed with most samples. From the (550/710)- and 720-lines the a-value was computed. With this value the c-parameter was calculated from the (333)- and (413)-lines. Finally, the position of all the other lines was computed from the lattice parameters thus obtained. In this way the validity of the indexing could be checked and, at the same time, this proce- dure gave an estimate of the accuracy of the lattice parameters. A correction was made for film shrinkage. The atomic radii used in the computations are the Goldschmidt radii for coordination number 12. Actually, some of the atoms have a coordination number of 14 or 15, but the error thereby introduced is small. * For the computation of lattice constants from the atomic radii an "average atomic radius" of all components was used, i.e., complete disorder was assumed. Although this seems to be true for some systems like OS-Cr,4 it is not true in others.11,13,14 The ordering model, however, which has been suggested by Kasper on the basis of extensive research lets both kinds of atoms contribute to both the ''vertical rows" and the lattice planes perpendicular to them, so that even with ordering of this kind the assumption of complete disorder cannot introduce a very serious error in calculating lattice parameters. RESULTS Bergman and shoemaker6 gave a table of the interatomic distances in the Fe-Cr phase. If we disre-

Jan 1, 1960

By I. Tamura, J. O. Brittain, T. Mura

Plain carbon steel in the cold worked or marten-sitic conditions has an internal friction peak at about 250 oC at a frequency of I cps. The influence of substitutional alloying elements on this peak was examined experimentally. The alloys were vacuum melted Co-, Cr-, Mo-, Ni-, and Si-iron (about 3 pct alloying elements), and carburized Si-iron. The internal friction of the alloys in the temperature range 30o to 500 OC was determined by means of a torsion pendulum. The 250 oC peak of the cold-worked alloys was lower in height than that observed in plain C-iron and steel. Carburized Si-iron in the quenched condition had a peak which occurred at a slightly lower temperature than in quenched plain C-steel, but the height of the peak was substantially greater than that found for the same alloy in the cold-worked condition. The activation energy of this peak for martensitic Si-steel was about 35 kcal per mol. ANNEALED a iron has two internal friction peaks due to nitrogen and carbon at 20o and 40o C respectively, at a frequency of 1 cps. If a iron is cold worked, these diffusion peaks become smaller and a new peak appears at about 250o C. The activation energy for the 250o C peak is in the range of 32 to 44 kcal per mol and has an average value of 38 kcal per mo1. It has been experimentally verified that both interstitial solute atoms and dislocations are necessary for the 250o C peak. 3 Wert has also shown that an incubation period precedes the appearance of the 250 C peak.4 With regard to quenched martensitic steel, Ke et al.596 observed two peaks at around 130o and 250o C. They conjectured that the 250o C peak in martensite was due to the same mechanism as the 250°C peak in cold worked a iron, and the 130°C peak was due to the nature of tempered martensite. They did not report the activation energy for these peaks. Chernikova7 found only one peak at about 200° C in tempered martensite. In a previous paperS we reported an activation energy of approximately 40 kcal per mol for the 250° C peak in plain carbon martensitic steels. Ichiyama8 found the activation energy to be about 36 kcal per mol for the 250° C internal friction peak in steels in the martensitic condition. The present authors proposed a theory for the 250°C peak for cold worked and quenched iron and steel.= The theory for the peak is based upon the addition of a strain-energy term to the free energy for the formation of a carbide precipitate due to the presence of a disclocation. The model employed for the relaxation process consists of the growth and solution of a carbide precipitate of critical size as a consequence of an oscillating dislocation. In this report, the influence of substitutional alloy ing elements on the 250° C peak is examined and the experimental results are discussed in terms of our theory for the peak. Most of the experimental work on the alloy steels was confined to the Fe-Si-C alloys.

Jan 1, 1962

By M. Garfinkle, W. D. Klopp, W. R. Witzke

The tensile properties of binary W-Re alloys containing up to 33 at. pct Re were determined at temperatures from 78" to 3630°F. Elongations as high as 260 pct were observed in electron-beam-melted tungsten containing 23 at. pct Re when tensile-tested at 3630°F after a 1-hr anneal at 3090°F. All alloys tested under these conditions with rhenium contents between 20 and 28 at. pct exhibited elongations of at least 200 pct. These alloys also showed enhanced grain growth rates. The values of strain-rate sensitivity ranged between 0.2 and 0.3 for the alloys exhibiting high elongations. Houlezler, for swaged alloys tested just above the re-crystallization temperature, strain-rate sensitivities as high as 0.8 were observed. The high-temperature strengths of the high-rhenium-content alloys were also less than those of alloys with intermediate rhenium contents. ALLOYING with rhenium has two distinct effects on the mechanical properties of tungsten. One effect occurs in dilute solid solutions and is most clearly seen in the lowering of the hardness and of the ductile-brittle transition temperature at about 5 at. pct Re.1-3 The second effect occurs in the concentrated solid solution at about 25 at. pct Re, and is characterized by twinning and a larger decrease in the ductile-brittle transition temperature. An aspect of the high-rhenium-content alloy which has received little attention is the higher-than-usual tensile ductility at 3500°F.3 Anomalous high ductility has been observed in several other alloy systems. usually associated with a phase transformation or a solid-solubility limit.4'5 The phenomenon is now commonly termed superplasticity. High-strain-rate sensitivities6 and grain boundary sliding7 have been reported for materials that undergo superplastic deformation. Also, it has been found that superplastic materials usually have a very fine grain structure (less than 10 pm).8 and it has been proposedg that such a structure alone is sufficient for superplasticity. The purpose of the present study was to further characterize the high-temperature tensile properties of W-Re alloys to determine the conditions under which they might be superplastic. Tensile and selected strain-rate sensitivity tests were conducted on alloys containing 0 to 33.3 at. pct Re at temperatures from 78" to 3630°F. Grain-growth rates were also determined on most alloys at 3630°F. Fig. 1 indicates the compositions evaluated and their locations relative to the solvus line in the tungsten-rich end of the W-Re phase diagram. Twelve binary W-Re alloys containing up to 33.3 at pct Re were double electron-beam-melted and subsequently fabricated to 0.3-in. rod by extrusion and swaging. The starting materials were commercial powders of tungsten and rhenium with impurity levels as listed in Table I. The various blended W-Re compositions were hydrostatically pressed at 70 ksi. The pressed bars were drip-melted into 1.5-in.-diam ingots and then remelted into 2-in.-diam ingots at a chamber pressure of 10~5 torr. The ingots were canned in molybdenum and extruded to round bar at a reduction ratio of 6:l. The alloy extrusions were swaged to about an 80 pct reduction at 2100" to 2900°F. Buttonhead tensile specimens with a reduced section diameter of 0.16 in. and a gage length of 1.0 in. were centerless-ground from the swaged bars

Jan 1, 1970

By Harry L. Brown, Philip E. Armstrong

Young's modulus doto ore presented for W, Mo. Ta. V, Cr. Ni, Ti, and Zr as a function of temperature up to about 0.7 of the melting points. A plot of reduced temperature us reduced modulus produces a general correlation except for titanium and zirconium. Young's modudlus data for some representatiue commercial graphites are given up to 2400°C. All results were obtained from longitudinal resonance-frequency measzrrements of 4-in. long samples, corrected for simultaneously measured thermal expansion. Comparison of poly crystalline and single-crystal tungsten behavior indicates that all the observed modulus values are frequencv -dependent at the higher temperatures. STATIC measurements of elastic properties of materials at elevated temperatures are extremely difficult to make since the elastic behavior is obscured by relatively large first-stage creep effects. Dynamic methods which avoid this difficulty by utilizing the measurement of the resonance frequency of a simple vibrational mode have been described in the 1iterature.l-3 The authors have extended the operating temperature range of this type of measurement to above 2000°C and have described the equipment elsewhere.~ The Young's modulus data presented here were obtained with this equipment, using samples about 4 in. long and 1/4 in. diam, supported horizontally at the center and excited to the fundamental longitudinal resonance frequency. Young's modulus was calculated by the formula: E = 4f2f2p where E = Young's modulus, / = frequency, 1 = length, and p = density. Dilatometric data were obtained simultaneously by optical measurements of the change of length of the sample. For the metals tested, an attempt was made to obtain modulus values that would be representative of the pure, strain-free, randomly oriented material. All of the graphites studied exhibited a high degree of elastic anisotropy, while the method assumes an isotropic homogeneous material. However , when the values for Young's modulus obtained for AUC graphite were compared with those taken from static measurements at room temperature they were found to be only about 4 pet higher. This is excellent agreement considering the low precision of modulus calculations from stress-strain curves. The difficulty in using data of apparent Young's modulus for anisotropic materials arises when the attempt is made to use these data and shear-modulus data to obtain Poisson's ratio. The results are usually meaningless and sometimes absurd.' RESULTS Table I lists the sources, impurity content, thermal history, and dilatometric constants of the metal samples that were investigated. All the metal samples were tested under a vacuum of 1 to 5 x 10-5 Torr. Where our dilatometric data agreed with previously published data, the table lists the previous values and the literature reference. Where no reference is given, the constants were determined from our dilatometric data. Table II presents the modulus data in units of millions of psi as a function of temperature in degrees centigrade. The numbers were obtained from curves fitted to the experimental data. For some types of calculations, such as those attempting to correlate creep data, the slope of the modulus curve is of interest, and this information also is reported in Table 11. It is always tempting to try to fit physical-property data into some general pattern and then use this pattern to predict the behavior of other similar materials. The general pattern for an elastic modulus of a metal seems to be a linear deoro- with increasing temperature Over the range between 0.1 and 0.4 of the melting temperature, then a progressive1y decreasing value up to the melting point. Metals appear to retain finite moduli

Jan 1, 1964

By R. H. Hiltz, R. W. Douglass

Large-grain specimens of iodide titanium prepared metal-lographically were stain etched using the technique of New York University as modified by Watertown Arsenal Laboratories. Orientations of grains showing an abnormal response to stain etching were determined by back-reflection X-ray techniques. X-ray results showed that a-titanium grains, oriented such that their basal planes were parallel to the polished surface, have a slower reactivity to stain etching than any other orientation. Grains oriented such that their basal planes made small angles with the polished surface exhibited reaction rates between that of the true basal orientation and the normal rate. As the angle with the surface increases the reactivity increases up to a maximum angle of 14 deg. Basal planes making an angle with the surface of greater than 14 deg show normal reactivity to stain etching. These data, plus work on polycrystalline specimens, indicate that the oxidation rate of titanium might be reduced by correct alignment of crystal planes. ThE earliest observed phenomenon in the micrography of titanium was the occurrence of a grains which exhibited no birefringency. Even though a titanium possesses a hexagonal-close-packed structure and should be optically anisotropic, it can appear optically isotropic, when the crystal is so oriented that its intersection with the polished surface is perpendicular to the axis of symmetry. During the develoment of color staining techniques for titanium: it was noted that the a phase did not stain uniformly. Staining of specimens of commercially pure titanium resulted in a micro-structure of blue-colored grains, among which were randomly oriented a few grains exhibiting colors between the initial yellow and the final blue color. Under polarized light, these off-colored grains appeared to be optically isotropic. More intense study with polarized light, however, showed only the yellow grains to be isotropic. The intermediate colored grains exhibited weak birefringency, which at first glance is not detectable due to the strong birefringency of the surrounding structure. Aminoff2 and Straumanis3 have previously shown that in zinc the basal orientation is less reactive than other orientations. Leidheiser4 showed the same thing to be true for the hexagonal-close -packed configuration of cobalt. Thus, it would appear that the basal-plane orientation is responsible for the abnormality in stained titanium. Later work by Leidheiser5 on cobalt has shown that other planes besides the basal plane exhibited reaction rates slower than the normal rate. Reported planes were the (100), the (1011) and several planes making small angles with the basal plane. The last observance appears not to be due to the reactivity of the reported plane but due to the reactivity of the basal plane which is very close to being parallel to the surface. There are, then, two possible explanations for the range of colors observed in stain-etched a titanium. Since extensive research on the effect of orientation on surface reaction has failed to provide any definite trend, these two explanations are not adequate in themselves. Planes showing the retarded reactivity differ not only for different crystal structures but for metals of the same crystal structure and even for different reactions of the same metal. Tragert,6 Leidheiser,7 Tammann,6 and wagner9 have shown copper to exhibit retarded reactivity on the (111) plane. However, Leidheiser10 has shown that under other conditions the retarded reactivity of copper is associated with the (100)

Jan 1, 1960

By R. A. Swalin, L. A. Neimark

The research work presented in this paper had initially a two-fold goal. First, further data concerning the low-temperature recovery of cold work was desired. Recovery phenomena have been extensively studied in face-centered-cubic metals but at the time of initiation of this research, no investigation concerning the low-temperature recovery in body-centered-cubic metals had been made. During the course of the investigation a paper by Martin on the recovery of point defects in molybdenum appeared.&apos; Comparison of our results on tungsten with Martin&apos;s results on molybdenum will be made. Secondly, knowledge concerning the influence of a particular type of impurity addition on the recovery kinetics was desired. It has been known for a long time that extremely small amounts of certain impurity additions exert a profound influence on the recrystallization behavior and the resulting microstructure of tungsten. Small amounts of potassium silicate and aluminum chloride added prior to the reduction of tungsten oxide to the metal have been found by Smithells to raise the recrystallization temperature markedly,2 and yield an ultimate microstructure in which grains several millimeters long are produced in fine wires of say 10 mil diam. If the impurities are added singly, ordinary secondary recrystallization results with none of the spectacular properties of the wire to which special additions were made. Swalin and Geisler3 and Rieck4 have studied the recrystallization behavior of such doped wire in some detail. The former workers found that small amounts of these impurities raised the recrystallization temperature over 400°C and electron microscopic examination revealed no obvious inclusions in the microstructures. In fact. chemical analysis showed that there was <0.001 pct K, <0.002 pct Al, trace of Si, and <0.0003 pct 0 in the wire studied. The possibility that the role of the special impurities is to keep the structure open by void formation and that submicroscopic porosity acts as the inhibiting agent has been discussed.2&apos;3 Meijering and Rieck5 have suggested that the impurities are strung out as second-phase particles in a direction parallel to the drawing direction. It was thought that a kinetic study of recovery could perhaps elucidate the role of the impurities to some extent. When a metal is deformed by cold work three basic types of defects are thought to be introduced into the crystal lattice, namely, interstitials, vacancies, and dislocations. Van Bueren6 has proposed that recovery of cold-worked metal is a four-stage process, each step being the result of the annealing of a primary defect or a combination of defects and having a unique activation energy. The steps in order of increasing activation energy are attributed to a) the diffusion of interstitials recombining with vacancies, b) diffusion of vacancy pairs, c) the diffusion of single vacancies, and d) climb of dislocations. In metals with relatively low- or medium-range melting points the temperatures for recovery are low enough so that the first three steps may occur during room-temperature deformation. For tungsten, because of the high melting point and subsequently high recovery temperature, it was calculated, using Nowick&apos;s approach7 that this recovery would occur in the temperature range 200" to 600°C. It is also known that recovery of X-ray line broadening, presumably due to dislocation climb, occurs at about 600°C.8 EXPERIMENTAL METHOD Two types of cold-rolled 10-mil-diam tungsten wire were used in the investigation; a) pure tungsten, (called undoped) and b) G. E. No. 218 wire (called

Jan 1, 1961

By W. A. Ver Wiebe

Under the impetus of new demands caused by the war, the oil and gas industries of Kansas established new records during the year 1942. In all, 1513 test wells were drilled, which is somewhat of a drop from the figure of 2113 for 1941. The 1513 tests yielded 800 new oil wells, 85 new gas wells, and 628 dry holes. Thus there was an increase in two categories, the gas wells and the dry holes. Considering that last year only 592 dry holes were completed out of a much larger total, the figure of 628 dry holes causes some concern among local operators. The increase in unsuccessful tests illustrates once more the fact that each year it is becoming harder to find the remaining oil pools. When the figures are broken down, it appears that western Kansas accounted for 1177 tests, of which 689 were oil wells, 33 gas wells, and 455 dry holes. The total potential daily initial production uncovered by the successful wells amounted to 753,178 bbl. of oil and 619,734,000 cu. it. of gas. The figures for new initial production indicate a substantial drop from last year&apos;s figure of 1,691,000 bbl., and the figures on gas are slightly higher. In 1941 the new gas as based on a daily potential was 508,000,-000 cu. ft. In eastern Kansas, 336 wells were drilled. Among these in were oil wells, accounting for a daily initial potential production of 16,199 bbl. The new gas wells numbered 52 and added 253,725,000 cu. ft. per day to the gas potential production of the state. The remaining tests, 173 in number, were dry. It is interesting and perhaps significant that about half (630) of the wells drilled in western Kansas were drilled by the independent operators. Among the large companies, the Cities Service Oil Co. drilled 163 wells; the Stanolind Oil and Gas Co., 52; the Skelly Oil Co., 39; the Continental Oil Co., 48; and the Shell Petroleum Co., 21 wells. In eastern Kansas the independent operators drilled 297 out of the total of 336 wells. Among the major oil companies the Cities Service Oil Co. drilled 19; the Phillips Petroleum Co. 7; and the Sinclair-Prairie Oil Co., 6 wells. The figures based on relative percentages of dry holes to successful oil or gas wells are revealing. In western Kansas almost one half of all wells drilled by the independent operators were dry holes. The major oil companies drilled approximately 547 wells in western Kansas, of which 379 were successful in finding either oil or gas. It thus appears that the major companies fared better than the independents. In eastern Kansas the major companies drilled 39 wells, of which 29 were successful in finding commercial quantities of oil or of gas. No less than 329 wildcat test holes were put down in western Kansas and 105 in eastern Kansas, or 434 in all, during 1942. Considerably more than half of these were drilled by independent operators; 223 in western and 99 in eastern Kansas. An exploratory hole 56 mile or more from production is regarded as a wildcat well in Kansas. On a percentage basis, about 80 per cent of wildcat wells were failures. In western Kansas only 20 per cent found either oil or gas. The failures were about equally distributed among the major

Jan 1, 1943

By W. A. Ver Wiebe

Under the impetus of new demands caused by the war, the oil and gas industries of Kansas established new records during the year 1942. In all, 1513 test wells were drilled, which is somewhat of a drop from the figure of 2113 for 1941. The 1513 tests yielded 800 new oil wells, 85 new gas wells, and 628 dry holes. Thus there was an increase in two categories, the gas wells and the dry holes. Considering that last year only 592 dry holes were completed out of a much larger total, the figure of 628 dry holes causes some concern among local operators. The increase in unsuccessful tests illustrates once more the fact that each year it is becoming harder to find the remaining oil pools. When the figures are broken down, it appears that western Kansas accounted for 1177 tests, of which 689 were oil wells, 33 gas wells, and 455 dry holes. The total potential daily initial production uncovered by the successful wells amounted to 753,178 bbl. of oil and 619,734,000 cu. it. of gas. The figures for new initial production indicate a substantial drop from last year&apos;s figure of 1,691,000 bbl., and the figures on gas are slightly higher. In 1941 the new gas as based on a daily potential was 508,000,-000 cu. ft. In eastern Kansas, 336 wells were drilled. Among these in were oil wells, accounting for a daily initial potential production of 16,199 bbl. The new gas wells numbered 52 and added 253,725,000 cu. ft. per day to the gas potential production of the state. The remaining tests, 173 in number, were dry. It is interesting and perhaps significant that about half (630) of the wells drilled in western Kansas were drilled by the independent operators. Among the large companies, the Cities Service Oil Co. drilled 163 wells; the Stanolind Oil and Gas Co., 52; the Skelly Oil Co., 39; the Continental Oil Co., 48; and the Shell Petroleum Co., 21 wells. In eastern Kansas the independent operators drilled 297 out of the total of 336 wells. Among the major oil companies the Cities Service Oil Co. drilled 19; the Phillips Petroleum Co. 7; and the Sinclair-Prairie Oil Co., 6 wells. The figures based on relative percentages of dry holes to successful oil or gas wells are revealing. In western Kansas almost one half of all wells drilled by the independent operators were dry holes. The major oil companies drilled approximately 547 wells in western Kansas, of which 379 were successful in finding either oil or gas. It thus appears that the major companies fared better than the independents. In eastern Kansas the major companies drilled 39 wells, of which 29 were successful in finding commercial quantities of oil or of gas. No less than 329 wildcat test holes were put down in western Kansas and 105 in eastern Kansas, or 434 in all, during 1942. Considerably more than half of these were drilled by independent operators; 223 in western and 99 in eastern Kansas. An exploratory hole 56 mile or more from production is regarded as a wildcat well in Kansas. On a percentage basis, about 80 per cent of wildcat wells were failures. In western Kansas only 20 per cent found either oil or gas. The failures were about equally distributed among the major

Jan 1, 1943

By Oscar M. Wicken

The mineral magnesite (MgCO3) if pure would consist of 47.7 pct MgO and 52.3 pct CO2. It is one of the calcite group of rhombohedral carbonates which includes calcite (CaCO3), siderite (FeCO3), rhodocrosite (MnCO3), and smithsonite (ZnCO3) among others. The members of this group enter into a wide range of substitutional solid solutions, whose range is still imperfectly known.* MgCO3 and FeCO3 appear to form a complete series of which breunnerite (ferroan magnesite) is a well known variety. Because of the considerable difference in size of the Ca and Mg ions, there is only a limited range in substitution in the MgCO3-CaCO3 series. (Dolomite, not strictly a member of the calcite group, may be regarded as an ordered structure developed when Ca: Mg is approximately 1:1.) The practical consequence of these relationships is that the lime carbonates (calcite and dolomite) are commonly present in magnesite deposits chiefly as mechanical mixtures. Magnesite may be either crystalline or "amorphous" (cryptocrystalline). The crystalline form has a hardness of 3.5 to 4.0. The color may range from white to black through shades of yellow, blue, red or gray. It is rarely found pure but generally contains variable amounts of iron, lime, and silicate minerals. Color cannot be used as an index of purity except under specific local conditions in a single quarry. In a given quarry an experienced man may be able roughly to grade magnesite by intuitively assessing such features as crystallinity and color. Crystalline magnesite occurs in larger deposits, but the cryptocrystalline variety is more common. The latter is fine-grained and compact and shows no cleavage; often it is descriptively called "bone magnesite." The fracture is usually conchoidal, and hardness is 3.5 to 5.0. It is normally white, but sometimes it is light yellow to orange or buff because of included impurities. In addition to lime and iron, which may be present in small amounts, silica may be present as inclusions of serpentine, quartz, chalcedony, or other minerals. In general, commercial deposits of "amorphous" magnesite have lesser amounts of accessory minerals than does crystalline magnesite. The specific gravity of "amorphous" magnesite is 2.90 to 3.0. Pure, crystalline magnesite has a specific gravity of 3.02, but iron carbonate, commonly present, raises the specific gravity to somewhat higher values. Magnesite dissociates, when sufficiently heated, into magnesia (MgO) and carbon dioxide. Either simultaneously or upon further heating the magnesia develops a crystalline structure identical with that of the natural mineral, periclase, which occurs sparingly in nature but not normally in workable deposits. Brucite is another magnesium mineral capable of being directly reduced to magnesia by heat alone. Brucite (Mg(OH)2) has been mined for the production of various grades of magnesia. It theoretically contains 69.1 pct MgO and 30.9 pct H2O. It may be white, but is generally blue or green with a gray cast. It has a translucent appearance. The mineral is soft (hardness, 2.5), and has a specific gravity of about 2.4. Nomenclature of Products The word "magnesite" literally refers to the natural mineral, but common usage has applied it plus a prefatory word to two other

Jan 1, 1960

By L. K. Jetter, J. C. Ogle, C. L. McHargue

The preferred orientation developed in extruded aluminum rods has been studied as a function of extrusion temperature, extrusion speed, and position in the rod. Duplex <111> - <001> textures were developed for slow extrusion speeds at temperatures of 75° to 850° F and for fast extrusion speeds at temperatures of 75° to 450°F. The <001> texture component was shown to be primarily due to re crystallization occurring during fabrication. At fast speeds and billet temperatures of 650° to 850°F, complete recrystallization occurred and <115>or<118> textures were found. The nature of the structure has proved to be an important variable in the production and use of extruded products. Data on the flow of aluminum and aluminum alloys summarized by Smith,&apos; Hardy,&apos; and Locke3 show that the extruded product may possess a deformed, a partially recrystallized, or a completely recrystallized structure, and there may be important variations in the structure from surface to center and from front end to back end of an extrusion. This inhomogeneity in grain structure and preferred orientation affects both the mechanical properties of the extruded section and its response to subsequent heat treatment. Among the fabrication variables causing these differences are temperature, extrusion ratio, and extrusion speed. Preferred orientation which develops during the extrusion of rods is of the fiber-type and, in general, has been assumed to be similar to that developed in rods or wires fabricated by drawing through dies, rolling, or swaging.4 Because of the nature of the flow of metal being extruded, this assumption may be valid for material near the center of the rod but probably is not valid for the outer layers. In most face-centered-cubic metals a duplex fiber texture has commonly been reported in which the grains have either <Ill> or <001> directions parallel to the longitudinal axis. Sachs and fichiebold5 reported cold-drawn aluminum (99.6 pct pure) to have a single <Ill> fiber texture, and this observation was confirmed by Schmid and Wassermann.6 Hibbard, on the other hand, observed a minor <001> and a major <111> texture in 99.994 pct A1 cold drawn to 98 pct reduction in diam.7 He concluded that the <001> component resulted from a small amount of room-temperature recrystallization. Dayal8 concluded that the <001> component was an intermediate component which disappeared at high reductions in 99.5 pct pure Al. Kostron and schippers9 found duplex <111> — <001> textures in extruded 99.5 pct Al, as did Gow and cahnl0 and GOW11 for extruded rods of commercial and superpure aluminum. Similar duplex fiber textures have been reported for aluminum alloys by Kostron,= Unckel,13 and Van Horn.14 The present paper is concerned with the variation in texture with fabricating conditions and with the nature of the texture components in extruded aluminum rod (99.99 pct pure). EXPERIMENTAL PROCEDURE Ingots were chill-cast in cast-iron molds and machined to 3-in. diam by 6-in. long extrusion billets. These billets were upset to 3.125 in. diam and extruded through a flat-face 0.690-in. diam die. Quenching of the rods was accomplished by a water spray at the die face. The combinations of fabricat-

Jan 1, 1960

By A. Heim, M. Gondouin

Invasion experiments were run on Berea sandstone cores to get laboratory measurements of resistivity and saturation profiles characteristic of water and oil sands invaded by mud filtrate. Injection rates were as low as 1.13 cm/D, and the cores were 30 to 36 in. long, cut parallel to the bedding planes. In the water-sand case, the resistivity profiles revealed the existence of an extensive transition zone between flushed and uncontaminated zones. In the linear geometry of the experiment, the width of the transition zone increased as the square root of the injected fluid volume. For the oil-sand case the core was prepared by displacing the formation water with kerosene to minimum water saturation. During the subsequent invasion experiment. oil saturation was measured directly by means of an oil-soluble radioactive tracer, and resistivity profiles along the core were taken at the same time. These data were interpreted in terms of an oil-water front, followed by a formation water bank, a zone of mixed waters, and finally, invaded mud filtrate near the borehole. Micro-fingering and capillarity seemed to affect considerably the resistivity profiles observed in the invaded oil-sand experiment. Beyond the regular conductive annulus or "low zone", it was found that a resistive "anti-annulus" could also be formed. As a result of these experiments, some simplified invasion profiles have been accepted and are being used in Grand Slam* interpretations. INTRODUCTION The importance of the mud filtrate-invaded zone in interpreting electrical logs has long been recognized.&apos;,* In trying to account for its effect, only very simple models of the resistivity profiles in the radial direction from the borehole have been used. In fact, most log interpretation charts have been based on resistivity models consisiting of two media of uniform resistivity (R, and R,) abruptly separated at the diameter of invasion. Such a clean separation of the media of different resistivities seems unrealistic, since flushing may not be perfect and may vary with radial distance into the formation.3** The nature of the transition zone, when it is within the radius of investigation of the surveying devices, may affect the log readings. Campbell and Martin&apos; verified that a conductive annulus containing a high percentage of formation water may be formed when mud filtrate invades an oil-bearing sand. Interpretations which are to include the effect of such an annulus require the addition to the model of a conductive zone located at the outer rim of the invaded zone.&apos; Using the Buckley-Leverett relations,6 aturation profiles may be derived, from which resistivity profiles can be calculated. Results of such computations by K. S. Kunz and J. H. Moran were given in a paper by Dumanoir. Tixier and Martin,7 and led to the construction of log interpretation charts which were based on a representation with three media of resistivities R, R0 and R1. Fig. 1 shows a schematic representation of a resistivity profile which includes an annulus. Campbell and Martin realized that, during the invasion of an oil sand, both capillarity and mixing would contribute to rounding of the profile shown in Fig. 1. Capillarity tends to draw some of the formation water from the annulus into the uncontaminated (Rt) zone, whereas mixing of the mud filtrate with formation water of the

Jan 1, 1965

By M. C. Miller, M. R. Tek, D. L. Katz

Previous studies have shown the influence of geometric variations on the drawdown and buildup behavior of a well completed in a homogeneous, porous medium containing a single-phase fluid. Other papers have shown the influence of leakage across caprocks on drawdown tests on water wells and aquifers. This paper presents two additional cases: the influence of an adjacent, expansible source of fluid, and the effect of caprock leakage on the measured in situ permeability and compressibility. Methods are developed for evaluating the influence of these two deviations from a uniform aquifer upon the in situ permeability and compre.ssibility indicated by pump tests. INTRODUCTION In relatively uniform porous media, saturated with a single-phase fluid, the effective reservoir permeability and compressibility of the water porous bed system may be obtained from drawdown and build-up data on wells, such as the initial wells drilled in aquifer storage reservoirs (Homers and Katz et al.7). In considering the drawdown and build-up behavior of wells adjacent to storage reservoirs, or of wells in an aquifer adjacent to an unknown gas field, questions arise as to the quantitative effect of the presence of compressible fluid on the measured permeability and compressibility of the formation. The solution to this problem is presented, using a constant pressure line source at some distance from two wells, one of which is pumped and the other used as the pressure observation well. The solution is presented in terms of the geometry of the wells and their relationship to the constant pressure line. It is known that caprock leakage can interfere with the determination of an aquifer in situ permeability and compressibility (Mantush4, Hantush and Jacob3 and Witherspoon and Muellerll). This paper presents an added case of the effect of leakage through a caprock of known thickness and permeability on well tests starting with a reservoir of constant pressure above the caprock and contributing to the aquifer as a result of the pump test. Again, both a pumping well and an observation well are postulated. These two cases are presented together since both a compressible fluid nearby and. caprock leakage show similar deviations from expected in situ permeability and compressibility results, and the solutions are similar in form. EFFECT OF A NEIGHBORING CONSTANT PRESSURE SOURCE ON IN SITU MEASUREMENTS Bixel, Larkin and van Poollenl presented a paper showing the influence of a discontinuity of the properties of a fluid formation system on drawdown and build-up performance. Their case is related to the present study but may be distinguished from it in that their numerical work and resulting graphs relate only to the performance of the pumping well itself. Incorrect values for in situ reservoir properties may be obtained from pump test data if the skin effect of the well and after-flow are not considered. Analysis of this problem by the authors indicated that the more reliable method of evaluating the influence of an adjacent gas field or expansible source was to use one well for pumping and another well at some distance from it for observing the aquifer pressure performance. An expansible source of hydrocarbon near a pumping well may be approximated by a line of constant pressure for a pump test. Fig. 1 illustrates a pumping well and an observation well near a line of constant pressure. Pressure behavior of an observation well during a drawdown pump test near a line of constant pressure is given by the diffusivity equation:

Jan 1, 1967