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Discussion of Dr. Douglas's paper on the Copper Queen Mine, Arizona (see p. 511)Edward Keller, Baltimore, Md. (communication to the Secretary): When, at the New Pork meeting, February, 1899, Mr. Douglas gave an abstract of his highly interesting paper on the Copper Queen mine, he invited the members of the Institute, in his usual progressive spirit, to make a full scientific investigation of the region of that mine during the prospective excursion to Bisbee, Arizona. I volunteered to examine some of the metallurgical processes and products of the works, and obtained from Mr. Douglas a valuable series of samples. Upon the issue of his paper, however, I found that he had already a considerable volume of analyses of those products, and that little was left for me to do in that respect, except to duplicate his results, the importance of which work would not have been commensurate to the time and labor involved. I selected, therefore, only some points which he had not made entirely clear, or concerning which I was skeptical. The details of most of my work will appear in a future paper. From Mr. Douglas's figures I have calculated the values for the elimination of impurities in the so-called Leghorn converter, introduced by him at the Copper Queen works, and have found them to be as follows: Percentage of Elimination of Impurities in Pour Blows of a Converter. No of ' Selenium Sulph'r Iron. Zinc. I Nickel. Lead. Antimony Arsenic. and Blow- ! Tellurium .. 1.......... 99.4 99.6 88.0 92.6 94.4 81.6 83.8 40.3 2.......... 99.0 99.6 98.1 92.5 96.8 71.9 76.6 38.1 3.......... 98.8 99.5 93.5 91.4 96.3 63.8 80.6 25.3 4.......... 99.8 99.5 95.8 95.8 97.5 65.3 76.9 36.3 Average 99.2 99.6 93.8 93.1 . 96.2 70.6 ! 79.5 35.0
Jan 1, 1900
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Institute of Metals Division - On an Effect of Silicon on Recrystallization Textures in Cold-Rolled High-Purity Iron-Silicon AlloysBy C. G. Dunn
According to a recently suggested effect of silicon on the re recrystallization textures of high-purity Fe-Si alloys with (111)[112] type rolling textures, the recrystallization texture for a rolled (110)[001] oriented iron crystal probably should be entirely different from that of a (110)[001] oriented 3 pct Si-Fe crystal. Comparative studies of iron and 3 pct Si-Fe crystals, however, show that both have (110)[Ool] recrystallization textures when the rolling textures are the (111)[112] type after reductions in thickness of about 70 pct. Qualitatively the results from the iron crystal are like those of polycrystalline high-purity 3 pct Si-Fe and not like polycrys-talline high-purity iron. The large effect previously noted probably involves unknown impurities or processing variables rather than silicon itself. Some problems on experimental and analytical procedure for a spherical X-ray specimen, which was machined from a laminated composite of sheet specimens, are treated in the Appendix. A possible strong effect of silicon on the textures produced in cold-rolled high-purity Fe-Si (HPFe-Si) alloys during primary recrystallization and normal grain growth was suggested in a recent paper.' All the textures were far from the random-orientation type, but that of iron, or of Fe-Si alloys of low silicon composition, was entirely different from the texture of 3 pct Si-Fe. The same effect was noted for the textures obtained prior to normal grain growth, i.e., for primary recrystallization.2 It is the main purpose of the present paper to provide some clarification of this silicon effect. All the HPFe-Si alloys from zero to 3 pct Si, which were rolled by two or more stages separated by anneals, developed (111)[112] type rolling textures.2 Thus, there was no effect of silicon on the rolling textures. Earlier, Gensamer and Mehl3 also found no effect of silicon on the rolling textures of Fe-Si alloys; they obtained the Kurdjum.ow and Sachs (K-S) rolling texture for iron,4 which is characterized as the three ideal components: (100)[011], (112)[li0], and (111)[112]. There is a difference between the HPFe-Si multiple-stage rolling texture and the K-S single-stage rolling texture, but this is a variable processing effect. Of interest here is the fact that the recrystallization textures from (111) [llZ] type rolling textures were different depending on the amount of silicon in the alloy. There was a relatively strong (110) [001] component in the recrystallization texture of HP 3 pct Si-Fe5,8,2 but no such component in HP 0.6 pct Si-Fe, for example; the recrystallization texture for the latter was two (111) [110] type components and a (111) fiber component 1,2 Several publications have shown that a strong (110) [001] recrystallization texture is derivable from a (111) [112] type rolling texture for 3 pct Si-Fe crystals reduced in thickness by about 70 pct.7-10 Furthermore it appears that the strongest of these (110) [001] recrystallization textures occurred when the orientation of the crystal prior to rolling was (110) [001].7 Barrett and evensoon11 found that the rolling texture of a (110)[001] oriented iron crystal was (111) [llj]. Accordingly, it seemed desirable to determine whether a (110) [001] oriented iron crystal, upon rolling and annealing, would behave like the 3 pct Si-Fe crystal (or the polycrystalline HP 3 pct Si-Fe) and thus produce a (110) [001] recrystallization texture contrary to the suggested silicon effect, or would behave like the polycry stalline HP iron or HP 0.6 pct Si-Fe and thus produce (lll) [110] type components in agreement with a silicon effect. Briefly, the idea here involves the use of more precisely defined textures to obtain if possible better control of important variables that affect the recrystallization process. PROCEDURE A (110) oriented crystal of Ferrovac "E" iron (99.9 pct pure) was prepared in sheet form 0.080 in. thick with the [001] direction parallel to the long dimension of the specimen.'' This crystal was etched to 0.073 in. thickness (to remove some small included grains) and then was cold rolled in a 6-in.-diam mill to a final thickness of 0.022 in. The rolling was unidirectional except for an inadvertent reversal at 0.061 in. thickness. At this thickness, and also at 0.040 in., the rolling was interrupted for transmission Laue photographs. Molybdenum Ka-radiation filtered with zirconium was used in a transmission method1' to obtain the cold-rolled (110) pole figure. The sample was a 0.002-in.-thick section taken from the central region of the 0.022-in.-thick cold-rolled crystal. For the primary recrystallization study, cold-rolled samples were etched from 0.022 to 0.021 in. thick and annealed in hydrogen at 850°C. Primary recrystallization to a fine-grained structure, Fig. 1, was obtained in a 5-min anneal. Eleven sheets after
Jan 1, 1963
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PART IV - Papers - The Elastic Anisotropy of Rolled BerylliumBy R. L. Moment
The anisotropic elastic behavior of rolled beryllium sheet has been measured, using a pulse echo technique, and compared with X-ray diffraction data. Calculated elastic stiffness constants compared favorably with published values for beryllium single crystals which were attributed to the strong (0002) rolling plane texture. Variations of Young's modulus in the yolling plane could be associated with the velative distribution of (0002) planes out of their ideal position in the rollitzg pkule. WHEN a metal is subjected to cold working such as drawing, forming, or rolling, a crystallographic texture develops which can significantly alter its physical properties. One method for detecting this texture is X-ray diffraction, but Alers and Liu' have recently pointed out how the prediction of anisotropic physical properties from pole figures alone is not always accurate due to differences in interpretation. Variations in Young's modulus with orientation or, more completely, the values of the effective elastic constants of the worked metal, also serve to indicate the presence of a texture. In fact, as Alers and Liu' pointed out, calculated variations in Young's modulus for assumed orientations, when compared with experimental data, can be used to eliminate some of the uncertainty in interpretation of X-ray pole figures. Thus, elasticity measurements can serve not only to clarify any unusual elastic behavior of worked metal, but also to detect and in part determine the nature of its texture. X-ray determination of the texture of rolled beryllium has been reported by Smigelskas and Barrett,2 who found a strong texture of (0002) in the rolling plane with (1070) planes normal to the rolling direction. In the case of metal rolled at room temperature, they reported that [1010] directions also appeared at positions 60 and 120 deg from the rolling direction in the rolling plane, while in more recent work Keeler3 found these directions were also tilted towards the rolling plane. The texture for beryllium rolled at 80O0C, however, only showed (1010) planes normal to the rolling direction and the spread of (0002) planes out of the rolling plane was less. In looking for elastic anisotropy one might consider unidirectional rolling of a metal as introducing an or-thorhombic symmetry through reorientation of the grains, since the three deformations, compression, extension in the rolling direction, and extension in the cross direction, are orthogonal to each other and unequal in magnitude. Thus the rolled sheet could be treated like an orthorhombic single crystal and the nine stiffness constants of the elasticity tensor used to calculate the anisotropy of Young's modulus, the shear modulus and Poisson's ratio. In this case we could write: which is symmetric about its diagonal. Borik and Alers4 have recently used this approach on rolled die steel with very good results. They found, however, that instead of displaying orthorhombic elastic symmetry their specimens could be considered tetragonal in which case Cr1 = c22, c13 = Ca, and c44 =cjj. This conclusion was made solely on the basis of the measured tensor elements, and serves to point out the advantage of this method for studying the anisotropy of rolled metals. Their calculated values for Young's modulus as a function of angle in the rolling plane also checked very well with direct measurements made on different specimens using the resonance technique. In the present study, cross-rolled beryllium was used which had been unidirectionally rolled about 11 pct for the final reduction. This imparted a slight anisotropy in the rolling plane which was detected both by X-ray techniques and elasticity measurements. For purposes of discussion in this paper, the rolling direction is that direction in which the most reduction passes were made and cross direction is the normal to the rolling direction in the rolling plane. It was also decided to consider the rolled sheet as displaying orthorhombic symmetry for the purpose of obtaining elasticity samples with the direction defined as in Table I. Any change in the final symmetry attributed to the sheet would then be made on the basis of the measured elastic stiffnesses. The final data would then be compared with that expected from the X-ray study and that reported for beryllium single crystals. EXPERIMENTAL PROCEDURE Rolling Schedule. The samples used in this study were taken from a large sheet which, because of its size, had to be unidirectionally rolled for the final reduction. The resulting texture was that of cross-rolled metal with a slight unidirectional texture superimposed. A cast beryllium ingot, 9.500 in. sq by 3.325 in. thick, was cross-rolled to 81 pct reduction followed by unidirectional rolling for an additional 11 pct to give a total reduction of 92 pct. The thickness of the final sheet ranged from 0.265 to 0.280 in. Reduction up to 67 pct was done at 980°C and the final 25 pct at 870°C. Analysis for metallic impurities showed aluminum 0.06 pct, iron 0.19 pct, and silicon 0.11 pct, giving a beryllium purity of 99.64 pct.
Jan 1, 1968
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Institute of Metals Division - The Control of Annealing Texture by Precipitation in Cold-Rolled IronBy W. C. Leslie
The textures of cold-rolled and of annealed iron are compared with those of an iron-0.8 pct copper alloy in which the amount of precipitation after cold rolling was controlled. Previously published pole figures -for cold-rolled and for annealed iron are confirmed. The effects of precipztatiotz after cold rolling are to retain the cold-rolled texture after annealing, to inhibit the formation of the usual allnealing texture, and to produce elongated recrys-tallized ferrite grains. It is suggested that the inhibition of new textures by precipitation after cold rolling is a general phenomenon. A great deal of attention has been paid to the development of texture during the secondary or tertiary recrystallization of ferritic alloys, but very little work seems to have been done on the control of texture during primary recrystallization. If such control were attained, it might be possible to simplify the processing of oriented materials or to change the characteristics of current cold-rolled and an-nealed products. From previous experience, it seemed likely that texture could be controlled by recrystallizing a supersaturated solid solution. Green, Liebmann, and Yoshidal found that the formation of preferred orientation in aluminum (40 deg rotation about <111> relative to the deformed matrix) was inhibited when iron was retained in supersaturated solid solution in the strained aluminum. The authors attributed this inhibition to iron atoms in solid solution. There is, however, an alternative explanation. Green et al, took a highly supersaturated solution of iron in strained aluminum and heated it to an unspecified temperature for recrystallization. It is probable that precipitation occurred prior to and during recrystallization, and it is proposed that the inhibiting agent is this precipitate, rather than the iron atoms in solid solution. It is important to note that precipitation before cold work is ineffective; the effective precipitate is that formed after cold working and either before or during recrystallization. The location and distribution of the precipitate are critical. Precipitation in such a manner has been found to have profound effects upon kinetics of recrystallization and the microstruc-ture of the recrystallized alloys.2-4 It would be surprising, indeed, if this were accomplished with no change in texture. Because of the relative simplicity of the system, and because of previous experience,4-7 it was decided to determine the effect of precipitation on texture in an alloy of iron and copper. Bush and Lindsay5 found an unspecified change in texture in cold-rolled and annealed low-carbon rimmed steel sheets when the copper content exceeded 0.1 pct. MATERIALS In earlier work, the rate of recrystallization of a low-carbon steel was greatly decreased by 0.80 pct copper, and, after the proper treatment, the recrystallized ferrite grains were greatly elongated.4 Accordingly, it was decided to investigate the effect of precipitation on texture at this level of copper content. The iron and the iron-copper alloy were made from high-quality electrolytic iron and OFHC copper, vacuum-melted in MgO crucibles, cast, hot-rolled to 0.2 in., then machined to 0.150 in. The compositions are given in Table I. The plates were heated to 925°C and brine quenched, twice. This produced a ferrite grain size of ASTM 0 in the iron and ASTM 1 in the Fe-Cu alloy. Disk specimens were cut from the heat-treated plates, repeatedly polished and etched, then used to determine (110) and (200) pole figures by reflection. Despite the complication of large grain size, these pole figures strongly indicated a random texture. PROCEDURES The copper content in solid solution in ferrite before cold rolling and recrystallization, and hence, the amount that could precipitate during the recrys-tallization anneal, was controlled at three levels by heat treatment. The specimens as quenched from 925° C were presumed to have all the copper, 0.80 pct, in solid solution. Other samples of the quenched alloy were aged 5 hr at 700°C to retain about 0.5 pct Cu in solid solution.6 A third set of quenched specimens was reheated to 700°C, then slowly cooled in steps, to reduce the amount of copper in solid solution to a very low level. All specimens were cold-rolled 90 pct, from 0.150 to 0.015 in. thick. The rolling was done in one direction only, i.e., the strip was not reversed between passes, with a jig on the table of the mill to keep the short specimens at 90 deg to the rolls. The rolls were 5 in. in diameter and speed was 35 ft. per min. Machine oil was used as a lubricant. In a supersaturated alloy, the maximum effect of the copper precipitate on microstructure and on recrystallization can be developed by a treatment at 500°C, after cold rolling and before recrystallization.'
Jan 1, 1962
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Part IX - Papers - Computer Solutions of the Taylor Analysis for Axisymmetric FlowBy G. Y. Chin, W. L. Mammel
The problem of selection of the active slip systems for a crystal undergoing an arbitrary strain has been analyzed by Taylor and by Bishop and Hill. The Taylor analysis is based on a principle of' virtual work, and involves finding, among numerous cotnbinalions of slip systems that satisfy the imposed strain, the combination in which the sum of the glide shears is a minimum. Previously, Taylor has treated the case of axisymmetric flow when slip occurs on (111)(110) (or {110)(111)) systems only. His analysis has now been extended by computer methods to the cases of slip on {112}(111) and {123)(111) systerns and of mixed slip on {110), {1 12), and (123) planes with a common (111) slip direction, all of which are important in the deformation of bcc crystals. The results are computer-plotted as contours of the ratio of the floe strength to the critical resolved slzea-r stress for slip, for axial orientations distributed throughout the standard stereographic triangle. Implications of the computer results to texture develop,merit, texture hardening, and dislocation theories oj work hardening are discussed. WhEN a single crystal is extended in the usual tension test, the lateral dimensions can change relatively freely. In this case, the glide shear produced by slip on a single slip system is sufficient to accommodate the (tensile) deformation. Since slip is governed by a critical resolved shear stress law (the Schmid law'), the single active slip system is one for which the stress, resolved on the slip plane and in the slip direction, is the highest among the several equivalent slip systems. This amounts to saying that a value M = U/t = y/~ is a minimum among the equivalent systems, where M is the inverse of the familiar Schmid factor (a and E refer to tensile stress and strain, and T and y refer to resolved shear stress and shear strain). A grain embedded in a polycrystalline aggregate, on the other hand, cannot freely change its shape due to constraint from its neighbors. In this case, slip from five independent slip systems (to accommodate five independent strains) is generally required.' Based on the principle of virtual work and assuming that the critical resolved shear stress for slip is the same for all systems, Taylor hypothesized that, among all combinations of (five) slip systems which are capable of accommodating the imposed strain, the active combination is that one for which the sum of the absolute values of the glide shears is a minimum. Again, this is equivalent to saying that the value of M = CjlyjI/ is a minimum, in analogy to the single slip case. Taylor aminimum,analyzed the case of {111)(110) slip for fcc metals, and applied the analysis to crystals undergoing axisymmetric flow, that is, the same macroscopic shape change as the poly crystalline aggregate under uniaxial tension (or compression). For the twelve equivalent {111}( 110) slip systems, there are 384 independent combinations of selecting five systems to satisfy the five independent linear equations of imposed strain.4 Taylor calculated the value of M for each combination* and obtained the active com- *A number of the independent combinations were omitted from consideration in Taylor's original work (see Ref. 5). bination (minimum M) for a number of axial orientations distributed throughout the standard stereographic triangle. Later work by Bishop and Hill*'8 showed that Taylor's least-shear hypothesis was equivalent to a maximum work principle which they advanced. Using the simplified Bishop and Hill method for {111)(110) slip, Hosford and Backofen' obtained detailed contours of constant minimum M for the same axisymmetric flow case. In contrast to {111}(110) slip in fcc metals, slip in bcc metals is generally described as occurring on {ll~)(lll), {112)(111), {123) (111) systems as well as mixed slip composed of all three. Since the direction cosines of the slip plane normal and the slip direction enter as a product in the Taylor analysis, the Taylor solutions of ,M for {110)(111) slip are identical to those for { 111} 110) slip. The other three cases of slip, however, have not been solved. In view of the numerous combinations of slip systems involved in the calculations, the Taylor analysis is clearly oriented toward computerized solutions. THE TAYLOR ANALYSIS In order to obtain the active combination of (five) slip systems by solving for the minimum value of M = we first express the (small) strain components E,, with respect to the cubic axes 1, 2, 3 ([loo], [010], [001], respectively) of the crystal, in terms of the sum of the glide shears yj from slip systems j: where n, and n,j refer to direction cosines of the slip plane normal, and dri and dsi to direction cosines of the slip direction, of slip system j, all referred to the cubic axes. In practice, the strain components are given with respect to the specimen axes X, y, 2. These components are readily converted to ers through the tensor transformation where irk and 1,~ are the direction cosines between the two sets of coordinate axes.
Jan 1, 1968
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Part IX - Papers - Activity of Interstitial and Nonmetallic Solutes in Dilute Metallic Solutions: Lattice Ratio as a Concentration VariableBy John Chipman
The concentration of a solute in a dilute ),zetallic solution may be measured by any of several parame- ters including weight percent, atom fraction, atom ratio, and lattice ratio. The ratio of filled to unfilled interstitial sites is useful for interstitial solutes. A variable 2 proportional to this ratio is used as a measuve of concentration. For component 2 irz a bitzary solution z2 = n2/Ym - nz/b) where b is the numberber of interstitial sites per lattice atom. For a t~lul-ticortzporzent solution this becomes zz = n2/(nl + Cvjnj) in which Vj = - l/b for an interstial solute and +1 for a substitulional solute. In the infinitely dilute solution the activity of an interstitial solute 2 is proportional lo z2. At finile concentration the departure from this limiting law is expressed us an activity coefficient, his coefficient is a function of concentra1io)z expressed as tevactiolz coeffcient 8; is analogous to the jark~iliar e£ bul is found to be independent of concentvation in certain solutions for which data are available. It is found that the same equations may be used to express the activity of a nonmetallic solute, sulfur, in liquid solutions of iron containing other solutes, both metallic and nonmetallic. For a nonmetallic solute or for one which strongly increases the actiuity of sulfur, it is convenient to assign arbitvarily a value vj = — 1. When this is done the derivative is found to be constant in each of the ternary solutions studied. The activity coefficient of sulfur in a complex liquid iron solution may be expressed as where nk is a second-order cross product determined in the quaternary solution Fe-S-j-k. The equation is used to calculate tlze activity of sulfur i)z three sevetl- component solutions. IN thermodynamic calculations concerning dilute solutions it is unnecessary to invoke laws and relations which extend across the concentration range to include concentrated solutions. In most binary metallic systems, as arkeen' has recently pointed out, there exist two terminal composition regions of relatively simple behavior, connected by a central region of much greater complexity. When the solute is a nonmetal there is only one such region and in many systems the concentration range is extremely limited. It is the purpose of this paper to suggest a method for the calculation of activities in such a terminal region in which one or more solutes are dissolved in a single solvent of predominantly high concentration. HENRY'S LAW In the usual textbook statement of Henry's law, concentration is stated in mole fraction. This has the advantage that it makes Henry's law thermodynamically consistent with Raoult's law. Since all measures of concentration at infinite dilution are related by simple proportion it follows that mole fraction, molality, atom ratio, weight percent, or any other unit of concentration can be used with the appropriate constant. At finite concentrations, however, calculations based on the law depend upon the unit employed. Deviations from Henry's law at finite concentrations depend upon the composition variable employed. They are evaluated in terms of activity and interaction coefficients2 which have become familiar features of metallurgical thermodynamics. It is the purpose of this paper to propose a measure of concentration for metallic solutions containing interstitial or nonmetallic solutes by means of which the calculation of activities in complex solutions may be simplified. The discussion will be restricted to free-energy interaction coefficients3 typified by Wagner's c|a BINARY SOLUTIONS The several measures of concentration which are to be considered are shown in line a of Table I. The corresponding activity coefficients are in line b and the deviation coefficients, sometimes called self-interaction coefficients, are in line c. Henry's law simply states that the activity coefficient approaches a constant value at infinite dilution. By adoptihg the infinitely dilute solution as the reference state and defining the "Henrian" activity as equal to the concentration in this state, the activity coefficient is always unity at infinite dilution. This convention is far sim~ler and more useful in dilute solution than emploiment of the 'Raoultian" activities and it will be used in the following discussion. The several definitions and equations of Table I will be referred to by means of their coordinates in the table. Early observations of deviations from Henry's law in metallic solutions were shown graphically4 rather than analytically. For the case of sulfur in liquid iron5 the slope of a plot of logfs vs (%S) was constant in the range 0 to 4.8 pct S, indicating constancy of eh2' in Ic. He was proposed by wagnerz and has been widely adopted. The a function of IIIc recently employed by ~arkenl was designed specifically for dilute solutions. Darken has shown that the value of a12 remains essentially constant for many binary solutions within a substantial range of compositions. The atom ratio is directly proportional to the molalitv.<, a conventional measure of concentration. IVb and C served as the basis for smith's6 classic studies of
Jan 1, 1968
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PART IV - Papers - Phase Relations and Thermodynamic Properties for the Samarium-Zinc SystemBy P. Chiotti, J. T. Mason
Ther?nal, X-ray, metallographic, and vapor pressure data were obtained to establish the phase diagram and standard free energy, enthalpy, and entropy of formation for the compounds in the Sw-Zn system. Four compounds, SmZn, SmZn2 , SmZn4.s, and SmZn8.5, melt congruently at 960°, 94Z°, 908°, and 940°C, respectively. The cornpounds SlnZns, Sm3Znll, and SnzZn7.3 undergo peritectic decomposition at 855", 870°, and 890C, respectively. Another compound of uncertain stoichiometry, SmZn11, undergoes peritectic decomposition at 760°C. Four entectics were observed with the following compositions in weight percent zinc and eutectic tenzperatures in degrees Centigrade: 12 pct, 680°C; 36 pct, 890°C; 58 pct, 850°C; and 72 pct, 900°C. An allotropic transformation and a composition range were observed for the SmZnz compound. The transfor)nation varies from 905" to 865°C as the zinc content increases from 16.0 to 48.5 wt pct, respectively. The free energy of formation of the compounds at 50PC varies between -15.9 kcal per mole for SmZn to -51.1 kcal per mole for SmZn,.,. Corresponding enthalpies vary between -19.2 to -78.3 kcal per mole. The ther-modynamic properties for the liquid alloys are described by the relations: A search of the literature revealed very little information on the Sm-Zn system. Chao et al.' as well as Iandelli and palenzonai have reported the structure of SmZn to be cubic B2 type and Kuz'ma et al3. have reported the structure of -sm2zn17 to be of the Th2Ni17 type. The purpose of this work was to establish the phase diagram of this system, to determine the zinc vapor pressure over the solid two-phase regions of the SYstem, and to calculate the thermodynamic properties of the compounds. MATERIALS AND EXPERIMENTAL PROCEDURES The metals used in this investigation were Bunker Hill slab zinc 99.99 wt pct pure and Ames Laboratory samarium. Analysis of the samarium by chemical, spectrographic, and vacuum-fusion methods gave the following average impurities in ppm: Nd, <200; Eu, <100; Gd, <100; Y, <50;Ca, 225; Ta, 400; Mg, 10; Cu, ~50; 0, 175; H, 20; and N, 15. The elements Fe, Si, Cr, Ni, Al, and W were not detected. The samarium was received as sponge metal and was kept under argon except when being cut with shears and when being weighed. Tantalum was found to be a suitable container for alloys with zinc contents up to the Sm2Znl, stoichio-metry. At higher zinc contents the grain boundaries of the tantalum containers were penetrated by the alloy and the containers failed during prolonged annealing. About 25 g of massive zinc and samarium sponge were sealed in tantalum crucibles equipped with thermocouple wells. These crucibles were in turn sealed in stainless-steel jackets. All closures were made by arc welding under an argon atmosphere. The samples were equilibrated in an oscillating furnace and in some cases were given various heat treatments in a soaking furnace. After appropriate heat treatment the steel jackets were removed and the alloy subjected to differential thermal analysis. The apparatus was calibrated against pure zinc and pure copper and found to reproduce the accepted melting points within 1°C. Alloys were subsequently subjected to metallographic examination and those of appropriate compositions were used for X-ray diffraction analysis and for zinc vapor pressure determinations. The vapor pressures were determined by the dewpoint method. Both the differential analysis and dewpoint measuring apparatuses have been described in earlier papers.4, 5 All alloy samples were etched with Nital (0.5 to 3 pct nitric acid in alcohol) except the samarium-rich alloys. These more reactive alloys were electro-polished in a 1 to 6 pct HClO4 in methanol solution at -700c at a potential of 50 v. EXPERIMENTAL RESULTS Phase Diagram. The results of thermal analysis are indicated by the points on the phase diagram, Fig. 1. Eight compounds and four eutectics were observed. The composition of the compounds and their melting or peritectic temperatures are given on the phase diagram. The four eutectic compositions in wt pct zinc and eutectic temperatures in % are: 12 pct,- 680°C; 36 pct, 890°C; 58 pct, 850°C; and 72 pct, 900°C. The stoichiometry of the most zinc-rich compound is still uncertain, but is very likely either SmZnll or SmZnlz. However, to simplify the presentation which follows it will be referred to as SmZnll. As shown on the phase diagram the phase regions for some of the samarium-rich alloys have not been unambiguously established. A sample of pure samarium was observed to transform at 924°C and to melt at 1074"C, in good agreement with corresponding val-
Jan 1, 1968
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Part X - Thermal-Dilation Behavior of Titanium Alloys During Repeated Cycling Through the Alpha-Beta TransformationBy Jerome J. English, Gordon W. Powell
An experimental investigation and mathematical analysis of the thermal-dilation behavior of the titanium alloy Ti-7Al-3Cb have shown that the linear dimensional changes associated with the polymorphic transformation need not be isotropic. The absolute magnitude of the linear dimensional change, which may be either positiue or negative, associated with the cr-p transformation is dependent upon the relutzve volumes of different orientations of the transformation product. It is hypothesized that the dilation irregulati-ties that have been observed during the polymorphic transformation of pure, coarse-grained titanium and other titanium-base alloys can be explained in the same manner. When titanium is heated above about 165O°F, the hcp a structure transforms to bcc 0. Thermal-dilatioh measurements have shown that the transformation is accompanied by a decrease in length of 0.16 pct.' Such dilation behavior would be expected because the volume of the hcp unit cell is about 0.3 to 0.4 pct greater than that of the bcc unit cell. A recent investigation2 of the thermal-dilation behavior of an experimental a-p* titanium alloy, Ti- 7A1-3Cb, containing 0.06 wt pct 0 showed that its dilation behavior during the polymorphic transformation differed substantially from that reported for unalloyed titanium. The first time the alloy was cycled through the transformation, the dilation curve closely duplicated that of unalloyed titanium. However, upon repeated cycling through the transformation temperature range, both the magnitude and the sign of the dimensional change associated with the transformation were observed to vary with each cycle. This investigation was undertaken to obtain additional data on the dimensional changes associated with the polymorphic transformation in the Ti-7A1-3Cb alloy and to determine the cause of the dimensional irregularities. After testing, the specimens were examined metallo-graphically. In addition, Laue back-reflection patterns were obtained from selected sections taken perpendicular to the specimen axes to determine the a orientations present in these sections. White radiation from a tungsten target and a 0.1-mm-diam collimator were used to produce the diffraction patterns. RESULTS Dilation Curves. Three types of thermal-dilation curves were obtained when the a-8 titanium alloy was heated and cooled through the transformation temperature range. These three types of curves are illustrated in Fig. 1. The type I curve represents what is considered normal behavior, because the dilation change is what would be expected on the basis of the volumes of the unit cells of a and p. The Type I1 curve is the inverse of Type I. Normal behavior is characterized by an expansion on cooling through the transformation, whereas a contraction takes place in the Type 11 curve. With Type ni behavior, no clearly distinguishable length change occurs during the transformation. No other anomalies that might be indicative of other phase transformations were observed in the dilation curves at lower temperatures. Apparently, the cooling rate was low enough for equilibrium to be reached during the 0 to a transformation. Table I lists the types of dilation curves observed during the polymorphic transformation as a function of the direction of measurement and cycle number. The A1 value was determined by extrapolating the low-temperature (a + 5 pct p) and high-temperature (100 pct p) segments of the dilation curves to a common temperature and measuring the difference in the or-dinates at that temperature, see Fig. 1. The transformation occurs over a temperature range in this alloy, so the magnitude of A1 is not an absolute value but depends on the choice of temperature. A mean temperature, T,, within the transformation temperature range was selected for the measurement. T, on cooling occurred about 100°C lower than T, on heating. The first time each of the three dilation specimens was heated to above the temperature, that is, Cycle 2, normal Type I behavior was observed. In Cycle 3, two deviations from normal behavior occurred. First, during cooling of the longitudinal specimen, a substantially larger expansion, +0.21 pct, was measured as 0 transformed to a compared with +0.03 pct in Cycle 2. Second, the thickness specimen was observed to undergo a contraction instead of the anticipated expansion on cooling. Continued cycling of the three specimens from room temperature to 2500°F produced additional changes in the dilation behavior. These changes did not seem to be related to the fabrication direction of the alloy because the values of a1 for the longitudinal, transverse, and thickness specimens varied unpredictably in magnitude and sign. Furthermore, both the longitudinal and transverse specimens showed all three types of dilation curves at least once during the six cycles that they received. Fig. 2 is a sketch of the transverse specimen after
Jan 1, 1967
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Coal - Increasing Coal Flotation-Cell Capacities. A Report on Semicommercial-Scale ExperimentsBy H. L. Riley, B. W. Gandrud
AS far as the present writers know, this system of flotation has not been used elsewhere in this country, but in the last couple of years it has been introduced, with minor variations, at one plant in England and one in Wales.' The system has been described and discussed in a number of publications.2-5 The following is quoted from an abstract of the latest of these,5 a paper presented at an International Conference on Industrial Combustion in 1952. On the basis of experience to date with the commercial plants, it is believed that the kerosene-flotation process incorporates all the necessary elements to make it greatly superior to anything else now available for treating of fines in wet processes of coal preparation. Additional study and investigation are still needed, however, to determine if certain phases of the process can be improved to such an extent as to make it generally satisfactory and acceptable to the industry. Further improvements will be needed with respect to the capacities of the flotation cells and the reagent consumption. The situation referred to above explains why an investigation is being made of the possibilities of achieving better cell capacities. Results obtained from this investigation, which is still in progress, are believed significant with regard to both cell capacity in general and the relation of cell design to cell capacity in particular. Commercial equipment now being used in a laboratory-type investigation should have performance characteristics similar to those of the larger machines. Equipment and Procedures: All flotation tests have been made in a standard Denver sub-A 24x24-in. unit cell of 12-cu ft volume. Cell modifications to make it more suitable for the tests were an adjustable front-wall section for varying cell depth and a perforated scraper-drag assembly for removal of the float product. There is also an apron dry-coal feeder, a gravity-feed water supply, reagent feeders, and a centrifugal pump that feeds the mixture of coal, water, and reagents into the flotation cell. A wattmeter connected into the drive-motor circuit records the power requirements of the impeller throughout each run. Dry coal, water, and reagents are all fed through a pan-type intake to the feed pump. A Sturtevant blower was set up to furnish air for supercharging. A centrifugal pump with a garbage-can intake provides for disposal of refuse flow to an outside settling tank. Figs. 1 and 2 show the flotation cell; Fig. 2 also illustrates the blower for supercharging. For purposes of this investigation, the percentage by weight of the feed coal recovered in the float product under a standard set of conditions has been considered as the criterion of cell capacity. The authors realize that such a criterion may be somewhat unorthodox, as the term cell capacity is usually understood to refer to feed input and ordinarily takes into account the ash analyses of the float product and refuse. However, the word capacity is flexible enough so that Webster gives one definition as maximum output, a definition which seems to justify, at least partly, acceptance of the above criterion. It has been the authors' experience in the Birmingham district that the ash-reduction efficiency of the coal-flotation process is generally satisfactory and that the only real problem is to increase the rate of float recovery so that the feed rate to any given bank of cells can be increased without undue loss of coal in the refuse. Originally it was planned to operate the flotation cell to simulate continuous operation during sampling periods. It was assumed that operating for reasonable time with feed coal, water, and reagents turned on would stabilize conditions so that the weight of float coal discharged during a fixed time interval would be an accurate measure of the rate at which the coal was being floated. It developed, however, that this supposition was erroneous. The float coal, caught for fixed time intervals and weighed, gave widely varying results in duplicate runs. Efforts to correct this trouble failed, and it was decided to try to operate on a batch-test basis, whereby all the float coal produced during a run on a known weight of feed coal would be caught in tubs, dewatered, and weighed. This method gives consistent and reproducible results, with total float product weight rarely varying by more than 3 or 4 pct on duplicate runs. The standard test procedure is as follows: A 132-lb sample of dry feed coal is weighed and placed in the feed hopper. The feeder is adjusted for a rate of 800 lb per hr. Feed water and reagents are turned on, and the feed and refuse pumps are started. One minute later the impeller is started. Six minutes are allowed for the cell to fill up with the water-reagent mixture. The feed of dry coal is started at the end of this 6-min period. One minute later the float-coal removal drag is started. The float coal is caught in one tub for the first 6 min after the flow of feed coal starts. Tubs are then changed, and the float coal is caught in a second tub until the feed coal runs out, when the tubs are again interchanged to catch the float coal for the remainder of the run in the first tub. The cell is kept running for 3 min with the water and reagents on after the feed stops to allow residual float coal to be removed. At the end of a test the wet float coal in both tubs is weighed and the total weight recorded. The product in the second tub is used for moisture determination and screen-size analyses. When the
Jan 1, 1956
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Institute of Metals Division - Alloys of Titanium with Carbon, Oxygen and NitrogenBy R. I. Jaffee, H. R. Ogden, D. J. Maykuth
IN THE past year, Jaffee and Campbell' and Finlay and Snyder2 reported on the mechanical properties of titanium-base alloys, some of which were in the same ranges of composition as are covered in this paper. In this paper, evidence confirming that given by Finlay and Snyder on the effects of carbon, oxygen, and nitrogen on titanium will be presented; and, in addition, new data will be given on the effects of these elements on the flow properties and phase transformation of titanium. Materials and Preparation of Alloys The preparation and general properties of iodide titanium have been adequately described elsewhere.' , As-deposited iodide titanium rod, prepared at Battelle, of Vickers hardness less than 90 was employed as the base metal in the present work. This was the same material as that used by Finlay and Snyder.2 The probable analysis reported by them for standard quality metal holds here also: N 0.005 pct, 0 0.01 pct, C 0.03 pct, Fe <0.04 pct, A1 <0.05 pct, Si <0.03 pct, and Ti 99.85 pct. Carbon was added in the form of flake graphite supplied by the Joseph Dixon Crucible Co. Oxygen was added in the form of c.p. grade TiO, powder, produced by J. T. Baker Chemical Co. Nitrogen was added in Ti3N4 powder, supplied by the Remington Arms Co. Individual ingots weighed 7 or 8 g. Carbon, oxygen, or nitrogen was added by placing the corresponding powder in a capsule made from as-deposited iodide titanium rods and melting the capsule with the balance of the charge. The charge was are-melted with a tungsten electrode on a water-cooled copper hearth under a partial vacuum of very pure argon (99.92 pct minimum). Melting was practically contamination free. Vick-ers hardness increases of less than 10 points were normal for unalloyed iodide titanium control melts. Nitrogen analyses of are-melted iodide titanium showed a nitrogen content of 0.005 pct, about the same as is present in the as-deposited rod. No tungsten pickup was found in a melt of iodide titanium analyzed for tungsten. Weight losses in melting nitrogen-free alloys were very small and varied consistently from nil to 0.015 g (0 to 0.2 pct). This permitted the use of nominal composition for these alloys. Chemical analyses made for carbon, which can be analyzed conveniently by combustion methods, justified this procedure. Where nitrogen was added, considerable splattering took place. Here it was necessary to analyze for nitrogen by the Kjeldahl method. The ingots were hot rolled at 850°C to about 0.045 in. thick. After hot rolling, the strips were descaled by mechanical grinding, and then given a cold reduction of 5 to 10 pct to insure a uniform thickness throughout the length of the specimen. The edge strips and the tensile strips were annealed in a vacuum of 1x10-4 mm Hg pressure for 3 1/2 hr at 850°C and furnace cooled. Methods of Investigation Hardness Measurements: At least five Vickers hardness measurements were taken using a 10-kg load on each sample in the following conditions: (1) top and bottom of each ingot, (2) top and bottom surface of as-rolled and annealed sheet, and (3) on cross-section of annealed sheet and all quenched specimens. Tensile Tests: Tensile tests were conducted on Baldwin-Southwark testing machines having load ranges of 600 or 2000 lb. Tests were made on 1-in. gauge-length specimens, 3 1/4-in. overall length, 1/2 in. wide, 0.040 in. thick, with a reduced section 1 1/4 in. long and 0.250 in. wide. Two SR-4, A-7 strain gauges, one mounted on each side of the specimen, were used to measure the strain over a limited range to determine the modulus of elasticity. After the modulus of elasticity readings had been taken, load vs. strain readings were taken, using only one strain gauge, at increments of 0.0001 in. until the yield points were passed and then at 0.001-in. increments to the limit of the strain-gauge indicator (0.02 in.). Strain readings above 0.02 in. per in. were taken every 0.01 in., using dividers to measure the strain between the 1-in. gauge marks until the maximum load had been reached. Crosshead speed, when using the SR-4 gauges, was 0.005 in. per min, and, when using dividers, 0.01 in. per min. Flow Curves: Flow curves were determined using the true stress-true strain data obtained during the tension test. The usefulness of this type of information has been dealt with very adequately elsewhere by L. R. Jackson,' J. H. Hollomon,6 and many others. Flow curves of true stress vs. true strain could be converted to the more conventional cold-work curve of 0.2 pct offset yield strength vs. percentage of cold reduction by means of the transformation, 1/1 = 1/1-R, where R is the fraction reduction in cold working. Thus, the true strains corresponding to percentage reduction can be calculated, and the 0.2 pct offset yield strengths scaled off the — 6 curve by taking the true stresses corresponding to the values of 6 + 0.002 strain. Heat Treatment: For the transformation studies, the alloys were heat treated in a horizontal-tube furnace using a dried 99.92 pct argon atmosphere, and quenched into water. Essentially no contamination was found after several hours of heat treatment at temperatures up to 1050°C. Metallography: Specimens were prepared in the
Jan 1, 1951
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Mining - Change to Rotary Blasthole Drilling in Limestone Increases Footage, Cuts Time, Saves ManpowerBy D. T. Van Zandt
IN the late 1920's rotary drills began to replace the churn drills in the petroleum industry, but until the middle 1940's the churn drill was the only widely accepted means of drilling large-diameter blastholes for quarry operations. The Calcite plant of the Michigan Limestone Div., U. S. Steel Corp., was one of the first to experiment with rotary drills for quarry blasthole drilling, and the first to employ compressed air on a fully rotary rig to cool the bit and raise the cuttings to the collar of the blasthole. The Calcite plant operates a limestone quarry near Rogers City, Mich., in the northern part of the lower Michigan peninsula. The formation quarried, a portion of the middle Devonian series, is the Dundee limestone, which is uniform, seldom massive, and characterized by definite bedding planes. The dip is southeast, 40 ft to the mile. Quarry faces vary from 20 to 116 ft in height. Vertical blastholes are used entirely, from three to five rows of holes being drilled parallel to the working face, spaced 18 ft apart with 18-ft burden and drilled 6 to 8 ft below shovel grade. Quarry operations coincide with the navigation season on the Great Lakes, as the bulk of the stone is transported by lake carrier. The normal operating season runs from April to December, the remaining time being devoted to stripping operations and plant and equipment maintenance. In the followirig discussion drilling rates mentioned refer to overall drilling time and include all operations such as moving from hole to hole, penetration and extraction of tools, and routine maintenance. Time consumed by such factors as power delays and major machine repair is not included in drilling time unless otherwise stated. Figures cover only operations at this one plant in the formation mentioned. Needless to say, a very different set of figures could be obtained in a different formation. However, the comparison of footage obtained with churn drills and rotary rigs in this particular formation has been used as an indication of what might be the expected performance of rotary rigs in other formations. Prior to 1950 the bulk of the blasthole drilling at the Calcite plant was done by electrically powered churn drills. Both crawler and wheel-mounted rigs were used. These machines, which mounted a 22-ft drill stem of 4½ in. diam and a spudding type of bit 2 to 4 ft long, drilled a hole of 5 ?-in. diam. Average drilling rate of these rigs in the Rogers City formation was 8 % ft per hr. In 1946 one of the first rotary blasthole drills offered to the quarry industry was put into use on an experimental basis. This machine, known as the Sullivan Model 56 blasthole drill, Fig. 1, was on 16-in. crawler pads and electrically powered at 440 v. The drill bit, a Hughes Tri-Cone roller bit of 5?-in. diam, Type OSC, was threaded into the end of the 4-in. square hollow drill rod or stem. These drill rods were 20 ft long with female threads on one end and male on the other to allow for addition of the desired number of rods for drilling holes of various depth. Rods were handled by a single drum hoist geared to the main drive motor and racked by a 30-ft derrick or mast when not in use. The cable from the hoist drum fed through a crown block on the top of the derrick back to the water swivel mounted in the top end of the drill stem in use. This cable remained attached during drilling operations and was used to hoist the tool string from the hole. Down pressure was applied to the tool string by means of a pair of 4-in. diam hydraulic cylinders acting on the drill chuck holding the drill rod. The first chuck consisted of flat jaws which gripped the flat sides of the stem. These jaws were controlled by set screws forcing them into contact with the drill stem. As these set screws had to be loosened and tightened by hand with each stroke of the hydraulic feed cylinders, there was great delay. For this reason the semi-automatic chuck was developed which automatically gripped the stem on the downward stroke but released for retraction of the hydraulic feed cylinders. Rotation was imparted to the tool string by a rotary table acting on the chuck and geared to the main drive motor through a separate gear train and clutch. A positive displacement water pump, mounted on the drill, fed water through a system of pipes and hose into the water swivel mounted on the top of the drill rod and through the rod and bit, washing the drill cuttings to the collar of the hole. Where water was scarce, provision was made to settle out the cuttings coming from the collar of the hole and re-use the water. Where water was abundant the stream coming from the hole was wasted. Drilling rate with this machine was about 20 ft per hr and bit life 1600 ft of hole. While this rate was more than twice that obtained with the churn drills employed, the problem of water supply and drill cuttings disposal rendered the machine impractical from an operating standpoint. Consequently it was used only in that part of the operation for which water was easily supplied, when the character of the formation made it least difficult to wash cuttings away from the collar of the hole. In October 1949 it was suggested that drill cuttings be removed by compressed air, long used for this purpose on pneumatic drills, and collected at the collar by suction. Thereafter, the water pump on the Sullivan 56 was replaced by a 500-cfm air compressor and a trial run made. Air pressure at
Jan 1, 1955
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Logging and Log Interpretation - Computer Evaluation of LogsBy E. A. Breitenbach
A computer program has been developed to afford rapid and complete quantitative log analysis for exploration and production decisions. The computation consists of automatic selection of tops and bottoms of porous intervals from the digitized data, and then point-by-point calculations within each selected interval. Nearly all log types can be analyzed. This paper presents the calculation techniques found to be appticable to machine evaluation and gives examples of their use. INTRODUCTION As the quantitative interpretation of well logs entails repetitive use of charts and equations, it is natural that digital computer programs would be written. A Universal Log Interpretation Computer Program (ULICP) has been developed to afiord rapid and complete analysis for exploration and production decisions. Application of this program enables the log analyst to: (I) apply rapid quantitative log analysis for exploration and production decisions on either a field, a well or on a single zone basis; (2) apply concepts of interpretation requiring detailed numerical analysis; (3) analyze all porous intervals on each log, rather than a few selected zones, and complete the analysis in less time than previously required. Computations are reported for every digitized point in each zone; (4) use empirical techniques applicable to a given area as an integral part of the computation; (5) experiment with the empirical coefficients and exponents in the interpretation equations to find the best possible solution; and (6) automatically plot both the original and computed data to scales analogous to the field prints. The primary utility of a log interpretation program stems from its ability to do an overwhelming amount of work with very little man-power. If a calculation procedure or thought process can be formalized to the extent that step-by-step logic can be written, a computer program can be developed that follows this logic. The major question is one of economics. A feasibility study of the costs for such a program indicates that digital processing is economical primarily as a means of increasing the productivity of the log analyst. In effect, the probability of missing productive intervals in any well, because of a lack of time to do detailed calculations, is greatly reduced. The nucleus of ULICP is programmed to compute large sections of a suite of logs by selecting zones automatically and then performing all pertinent computations on a data point by data point basis within each zone.'.' An entire suite of logs can be processed in this manner with very little manual intervention. Sufficient programming logic is available so that each log analyst can request computations pertinent to his area. These requests are made by simple additions or deletions of information on the input header cards. Hence, the log analyst is always in complete control of the computation process. The evaluation of a suite of logs requires pre-editing, digitization, computation, presentation of results and interpretation. Work by the log analyst is reqilired only in pre-editing and interpretation. Thus, he is allowed more time for comprehensive interpretation, rather than calculation. For continuity, the discussion of ULICP is organized sequentially: pre-editing, digitization, computation and presentation of results. DISCUSSION PRE-EDITING The extent of pre-editing prior to computation is dependent on the format of the original data. For analog prints, it requires inspection, correlation and editing of the logs, plus the entering of required data an special forms. For digitized data such as magnetic tape field recordings, only the special forms are necessary. The process for analog prints will be given here. The inspection and correlation process involves the selection of sections for digitization and the correlation of the traces to a common depth. To decrease the cost of digitization, traces that exhibit large variations in shale formations can be redrawn to a non-zero baseline. The next step is to enter all pertinent data on the input header cards. The header cards presently used for ULICP are presented as Figs. 1 through 6. Cards 1, 2, 3 and 4 (Fig. 1) are defined as the Main Header Cards. They describe the particular well for output identification and give basic information. Cards 5 through 15 (Figs. 2 through 6) are defined as the Block Header Cards. As such, they define the log types and the interpretation parameters for the block of data immediately following. Cards 1 through 10 are required for every computer run. Cards 11 through 14 pertain only to nuclear logs. Card 11 is required if any nuclear log is supplied, and cards 12 through 14 are required only when gamma-ray, density or neutron log data, respectively, are supplied. Card 15 (Fig. 6) must be supplied when cross-plot calculations are required. Either two- or three-component
Jan 1, 1967
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Natural Gas Technology - The Importance of Water Influx in Gas ReservoirsBy R. G. Agarwal, Ramey Jr. H. J., Al-Hussainy R.
Although it has long been realized that gas recovery from a water-drive gas reservoir may be poor because of high residual saturations under water drive, it appears that only limited infomlation on the subject has been available until recently. This study was performed to show the qiiantitative potential importance of water influx. Results indicate that gas recovery may be very low in some cases: perhaps as low as 45 per cent of the initial gas in place. Gas recovery under water drive appear to depend in an important was on: (I) the prodirction rate and manner of production; (2) the residual gas saturation; (3) aquifer propertie.); and (4) the volumetric displacement effciency of water invading the gas reservoir. The manner of estimating water-drive gas reservoir recovery can vary considerably. Examples are: the steady-state tnethorl. the Hurst modified steady-state method, and various unsteady-state methods such ac. those of van Ever-dingen-Hurst, Hurst, and Carter-Tracy. The Carter-Tracy water influx expression was used in this study. In certain cases, it appears that gas recovery can be increased significantly by controlling the production rate and manner of production. For this reason, the potential importance of water influx in particular gas reservoirs should he investigated early to permit adequtrtr planning lo optirtize the pay reserves. INTRODUCTION In recent years, the economic importance of natural gas production has become increasingly apparent. This has been evidenced by more intensive exploration efforts aimed at gas production, and exploitation of both deep, as well as low-permeability gas reservoirs. Technical developments such as deep-penetration fracturing have made development of such formations economically feasible. Unfortunately, water influx has forced abandonment of a number of gas reservoirs at extraordinarily high pressures. Although reservoir engineering methods for estimating water influx have long been available, it appears that application of these methods to the water-drive gas reservoir has been sporadic.'a Available methods for estimating water influx which can be applied to the water-drive gas reservoir problem include the steady-state method,1 the Hurst modified steady-state method and various unsteady-state methods such as those of van Everdingen-Hurst. Hurst, and Carter-Tracy. Interesting applications of these solu- tions to gas reservoir and the aquifer gas-storage problems have appeared recently.3,12,14 The experimental study of residual gas saturations under water drive by Geffen et al. in 1952 indicated that residual gas saturations could be extremely high. A value of 35 per cent of pore volume is often used in field practice when specific information is not available. The study of Geffen et al. showed that residual gas saturation might be much higher in some cases. Naar and Henderson concluded that the residual non-wetting phase saturation under imbibition should be about half of the initial non-wetting phase saturation. The Naar and Henderson result that residual gas saturation under water influx should be about half the original gas saturation is recommended as an estimate if laboratory measurements are not available. Thus, it is clear that a considerable portion of the initial gas in place might be trapped in a water-drive gas reservoir as residual gas at high pressure. A full water-drive would result in loss of residual gas trapped at initial reser.voir pressure. Consideration of transient aquifer behavior leads to the conclusion that high-rate production of water-drive gas reservoirs could result in improved gas recovery by reduction of the abandonment pressure. However, there appears to be little quantitative information on this possibility. One of the few advantages of water-drive gas production appears to be improved deliverability through water-drive support of the reservoir pressure. There may also be an advantage in higher condensate recovery caused by pressure maintenance for gas-condensate water-drive reservoirs. In view of the preceding, this study was made to assess the potential importance of water-drive in gas reservoir engineering. The Carter-Tracy approximate water-influx expression was used because this equation offers some advantages in hand-calculation which do not appear to have been generally recognized.' However, calculations were performed in the main with a high-speed digital computer to permit evaluation of the effect of water-drive under a large variety of conditions. CALCULATION METHOD Water-drive gas reservoir performance can be estimated in a manner completely analogous to oil reservoir calculations: a materials balance is written for the reservoir, and a water influx equation is written for the aquifer. Siniltaneous solution provides the cun~ulative water influx and the reservoir pressure. When reservoir performance data (gas produced and reservoir pressures) are available, it is usually possible to match performance data to determine the initial gas in place and the water influx parameters —
Jan 1, 1966
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Drilling-Equipment, Methods and Materials - Horizontal Fracture Design Based on Propped Fracture AreaBy Harry A. Wahl
Precent fracture design procedures are bared on the total fracture area created. A method to distinguish beI,,.ecn total area and [he propped or effective fracture area has not been available. This paper presents a solution to this problem, applicable to horizontal fractures. The difierences between effective fracture area and torn] area are demonstrared in example calculations. This work is hayed on experimentally determined transport efficiencier of solids in sand-liquid slurries. Newtonian and non-Ne~vtoninn systems are considered. INTRODUCTION Fifteen years after commercial introduction, hydraulic fracturing remains the most successful stimulation technique in the oil field. This success is primarily due to ability of induced fractures to penetrate and alter permeabilities deep within formations. Many fields producing today could not have been developed without the hydraulic fracturing process. Because of wide usage, fracture-treatment design has received a great deal of engineering and research effort. This work, resulting in improved equipment and materials, has increased the benefits from fracture treatments as well as the applicability of the process. A major contribution was the development of fluid-loss additives. Necessarily, the number of parameters to be considered in treatment design has steadily increased, resulting in more complicated design techniques. Almost all present design procedures are based on the precepts set forth by Howard and Fast. Relating the fluid volume lost into the formation, the volume required in extending the fracture, and the total slurry volume injected, they developed an expression for the total fracture area created in terms of pertinent treatment parameters. Fluid loss during treatment was expressed as a function of time for three flow mechanisms. Although modifications of fluid loss equations have been made, the total fracture area concept has remained unaltered. A vast amount of field data indicate that induced fractures must be propped and held open to be effective. A notable exception is the Mesa Verde formation in the San Juan basin. However, analysis of these treatments shows that improved well productivities are obtained when propping agents are incorporated in the treating fluid. Although propped fracture area has been recognized as an important design parameter, a method to distinguish between total area and effective fracture area has not been available. The necessary information on slurry-sand transport in fractures has been lacking. Interest in the propped region of induced fractures is not restricted to areal extent alone. The distribution of sand within fractures is important from the standpoint of fracture flow capacities. Flow capacity affects the increase in well productivity after stimulation. The work of Huitt and Darin4 hows that partial monolayers of sand have large flow capacities compared to thick* dense sand packs. It has been postulated that gelled fluids have the ability to transport sand within the fractures at the deired low concentrations. An early contribution in the area of sand placement in fractures was made by Kern et al.' They studied sand movement in a transparent vertical fracture model. It was observed that the sand tended to settle out in the bottom of the model before moving very far. When the fluid velocity exceeded a certain critical value, all of the sand injected began moving through the crack even though it settled to the bottom. This critical velocity was determined under several flow conditions. Some work on sand movement in horizontal fractures has been reported in Russian publications. Sand movement was studied by Izyumova and Shan'gin' using a transparent "pie-shaped" flow model to simulate a horizontal radial flow system. However, the data were limited, especially in a quantitative sense. Dorozhkin, Zheltov and Zheltow studied the behavior of sand-liquid slurries in a horizontal linear flow model. The quantitative data were restricted primarily to the thickness of sand deposits formed at the bottom of the fracture. An earlier paper provided basic data on the flow of sand in horizontal fractures. This study was designed to yield specific quantitative information on rate of advance of sand particles and pressure behavior under various flow conditions. A comprehensive photographic study was undertaken in a 10-ft windowed flow cell to provide the necessary qualitative and quantitative data. Since the number of potential variables far exceeded the capacity of the initial study, emphasis was placed on the effects of sand concentration, oil viscosity and oil flow rate. A detailed description of these experiments and the results are described in Ref. 9. However. the implications of this work on the fracture design calculations were not discussed. An analysis of these data as well as new data is provided in the following sections. EXPERIMENTAL RESULTS The primary objective of the experimental investigation was to provide information on the rate of advance of the solids in sand-liquid sturries. A 10%-ft long transparent
Jan 1, 1966
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Drilling-Equipment, Methods and Materials - Bit-Tooth Penetration Under Simulated Borehole ConditionsBy W. C. Maurer
A study of bit-tooth penetration, or crater forniation. under simulated borehole condirions has been made. Pressure conditions existing when drilling with air, water and mud have been sirnulated for depths of 0 to 20.000 ft. These crater tests showed that a threshold bit-tooth force must he exceeded before a crater is .formed. This thresh old force increased with both tooth dullness and diflerenrial pressure between the borehole and formalion fluids. At low differential pressures, the craters formed in a brittle manner and the cuttings were easily removed. At high differenlial pressures, the cunings were firmly held in the craters and the craters were formed by a pseudoplas-tic mechanism. With constant farce of 6,500 16 applied to the bit reeth, an increase in differential pressure (sitnulated mud drilling) from 0 to 5,000 psi reduced the crater volumes by 90 per cent. A comparable increase in hydrostatic fluid pressure (simulated water drilling) produced only a 50 per cent decrease in volutne while changes in overburden pressure (simulated air drilling) had no detectable effect on crater volume. Crater tests in unconsolidated sand subjected to differential pressure showed that high friction was present in the sand at high pressures. Similar friction belween the cuttings in craters produces the transition from brittle to pseudo plastic craters. INTRODUCTION The number of wells drilled below 15,000 ft increased from 5 in 1950 to 308 in 1964. Associated with these deep wells are low drilling rates and high costs. High bottom-hole pressures produce low drilling rates by increasing rock strength and by creating bottom-hole cleaning problems. This paper describes an experimental investigation of crater formation under bottom-hole conditions simulating air, water and mud drilling. Although numerous investigators have studied bit-tooth penetration (cratering) at atmospheric pressure conditions, only limited work has been done on cratering in rocks subjected to pressures existing in oil wells. Payne and Chippendale2 have studied cratering in rocks subjected to hydrostatic pressure using spherical penetrators. Garner et aLJ conducted crater tests in dry limestone by varying overburden pressure and borehole fluid pressure independently and using atmospheric formation-fluid pressure Gnirk and Cheathem4,5 have studied crater formation in several dry rocks subjected to equal overburden and borehole pressure and atmospheric formotion pressure. Podio and Gray studied the effect of pore fluid viscosity on crater formation using atmospheric borehole and formation-fluid pressurc and varying overburden pressure. Although these studies have provided useful information on crater formation under pressure, they were limited in that the three bottom-hole pressures could not be varied independently and, therefore, that many drilling conditions could not be simulated. The prersure chamber used in this study allowed visual observation of the cratering mechanism and independent control of the borehole, formation and confining pressures. By using different fluids in the chamber, pressure conditions existing in air, water and mud drilling to depths of 20,000 ft were simulated. The mechanisms involved in cratering at these different pressure conditions were studied for teeth of varying dullness and at different loadins rates. High-speed movies (8,000 frames/sec) and closed-circuit television were used to visually study the crater mechanism under pressure. EXPERIMENTAT PROCEDURE PRESSURE CHAMBER The Pressure chamber in Fig. I was used to simulate bottom-hole pressure conditions. This chamber has been pressure-tested to 22,500 psi and is normally operated at pressures up to 15,000 psi. The chamber contains four lucite windows' used for illuminating and observing the crater mechanism under pressurc. A closed-circuit television and a Fastax camera (8,000 frames/sec) have been used in these studies. Cylindrical rock specimens (8-in. diameter X 6-in. long) were subjected to three independently controlled pressures simulating overburden, borehole fluid and formation-fluid pressures. Overburden pressure, which corresponds to the stress induced by the overlying earth mass, was applied by exerting fluid pressure against a rubber sleeve surrounding the rock. Borehole pressure, which is the pressure exerted by the column of mud in the wellbore, was simulated by applying pressure to the fluid overlying the rock in the chamber. Formation pressure was simulated by applying pressure to the water saturating the rock. The borehole and formation pressures were equal except when mud was used in the chamber, in which case the differential pressure between these fluids acted across the mud filter cake.
Jan 1, 1966
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Institute of Metals Division - Recrystallization Textures in Cold-Rolled Electrolytic IronBy C. A. Stickels
The preferred crystallographic orientations developed during recrystallization of polycrystalline electrolytic iron sheet, cold-rolled 90 pct, were ivestigated. Recrystallization at 500° or 565° C for relatively short limes produces a texture which is similar to the rolling texture. A duplex partial fiber texture, significantly different from the rolling texture, is found when the annealing time is increased. Recrystallization at 700°C also produces a sequence of textures with increasing annealing time. In order of their appearance, these textures are: 1) the duplex partial fiber texture found at lower temperatures, 2) a four-component texture "near {322}(296)", 3) a {112)(110) +(111)(110) texture, and 4) a two-component "near {554)(225)" texture. Secondary recrystallization, or discontinuous grain growth, accompanies the development of the latter texture. However, the "near {554} (225)" texture was nol observed when secondary recrystallization occurred under other conditions. All of the ideal orientations found in recrystallization textures can be accounted for by the growth of minor components of the deformation texture. IN recent years there has been increased interest in improving the drawability of metals by controlling the preferred crystallographic orientation of the sheet.1-l3 Since more low-carbon steel is drawn than any other material, considerable attention has been focused on the properties of sheet steel. Efforts to improve drawability through texture control have been hampered by the lack of any published systematic study of the recrystallization textures developed in iron annealed below Acl. The purpose of the present work was to supply some of this missing information, specifically, the recrystallization textures obtained by isothermal anneals of polycrystalline iron, cold-rolled 90 pct. LITERATURE REVIEW—DEFORMATION TEXTURES Barrett14 reviewed and summarized the investigations of rolling textures in iron and low-carbon steel prior to 1952. The texture of heavily deformed iron (rolled 90 pct or more) is described as consisting of two partial fiber textures. The dominant fiber texture (designated here as fiber texture A) has a (110) fiber axis in the rolling direction and includes the orientations (001)[110], {112}( 110), and {111}(110). The secondary texture (designated here as fiber texture B) is described as having a (111) fiber axis in the sheet normal direction, and includes the orientations {111)( 110) and (111)(112). Since the publication of Barrett's book, there have been two detailed studies of the deformation texture in polycrystalline iron. In both instances, the more sensitive diffractometer methods of pole-figure determination were used. Bennewitz15 studied the cold-rolling textures developed in polycrystalline low-carbon steel and a 3 pct Si steel. He determined (110), (2OO), and (222) pole figures for specimens reduced 30, 50, 60, and 90 pct and analyzed his results in terms of partial fiber textures. He distinguished three stages in the development of the final deformation texture. 1) Grains rotate to form two incomplete fiber textures, with (110) fiber axes inclined 30 deg to the sheet normal toward the rolling direction (fiber texture B). After 50 pct reduction, the highest density of poles is near an ideal orientation {554}(225), the two components of which are members of this duplex fiber texture. 2) With increasing amounts of reduction, grains rotate about the former fiber axes toward ideal orientations of the type {112)( 110) (common to fiber textures A and B). 3) Finally, grains rotate about their ( 110) axis in the rolling direction, clockwise and counterclockwise from the orientations {112}(110). This produces the range of orientations from (111)(110) to (001)(110) commonly found in the rolling texture of heavily deformed iron (fiber texture A). No significant difference was found between the deformation textures of low-carbon and silicon steels. A few years earlier, Haessner and weik16 had determined (110) pole figures for carbonyl iron rolled to 30, 60, 80, and 90 pct reduction in thickness. heir data agree quite well with the more complete data of Bennewitz, but a somewhat different description of the evolution of the deformation texture was given. The appearance of (110) poles in the transverse direction is ascribed to a (100)[011] component rather than "near {554}( 225) " components, and the (110) fiber axes of fiber texture B are described as located 35 deg rather than 30 deg from the sheet normal. Both of these studies agree that the secondary texture present in heavily rolled iron, the duplex fiber texture B, has (110) fiber axes and not a single ( 111) fiber axis normal to the sheet, as
Jan 1, 1965
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Institute of Metals Division - The Effect of Surface Removal on the Plastic Flow Characteristics of Metals Part II: Size Effects, Gold, Zinc and Polycrystalline AluminumBy I. R. Kramer
Studies of the effect of size of the specimen on the change of slopes of Stages I and 11 by surface removal showed that the change of Stage I was independent of size with respect to the polishing rate; however, the change in the slope of Stage 11 with polishing rate increased directly in proportion to the surface area. The removal of the surface during the test affected the plastic deformation characteristics of gold, aluminum, and zinc single crystals and polycrystalline aluminum. The apparent activation energy of aluminum was found to be decreased markedly by removing the surface during the deformation process. In previous papers1-3 it was shown that the surface played an important role in the plastic deformation of metals. By removing the surface layers of a crystal of aluminum by electrolytic polishing during tensile deformation, it was found that the slopes of Stages I, II, and III were decreased and the extents of Stages I and II were increased when the rate of metal removal was increased. By removing a sufficient amount of the surface layer after a specimen had been deformed into the Stage I region, upon reloading, the flow stress was the same as the original critical resolved shear stress and the extent of Stage I was the same as if the specimen had not been deformed previously. The slope of Stage I was decreased 50 pct and that of Stage 11 decreased 25 pct when the rate of metal removal was 50 X 10"5 ipm. These data show that in Stage I the work hardening is controlled almost entirely by the surface conditions, while in Stages 11 and III both surface conditions and internal obstacles to dislocation motion are important. It appears that during the egress of dislocations from the crystal, a fraction of them becomes stuck or trapped in the surface regions and a layer of a high dislocation concentration is formed. This layer would not only impede the motion of dislocations, but would provide a barrier against which dislocations may pile up. In this case, there will be a stress, opposite to that of the applied stress, imposed on the dislocation source and dislocations moving in the region beyond this layer. It has been found convenient to refer to this layer as a "debris" layer. The "debris" layer may be similar to the dislocation tangle observed by thin-film electron microscope techniques.4 Reported in this paper are the results of studies on the effects of removing the surface during plastic deformation on aluminum crystals of various sizes. The effects of the surface on the yield point behavior of gold and high-purity aluminum crystals as well as the creep behavior were also determined. The effects of surface removal on polycrystalline aluminum (1100-0 and 7075-T6) are also reported. EXPERIMENTAL PROCEDURE For those portions of the investigation involving creep and tensile specimens, single crystals, having a 3-in. gage length and a nominal 1/8-in. sq cross section, were prepared by a modified Bridgman technique using a multiple-cavity graphite mold. The single crystals were prepared from materials which had initial purities of 99.997, 99.999, 99.999, and 99.999 pct for Al, Cu, Zn, and Au, respectively. The aluminum specimens for the size effect studies were prepared through the use of a three-tier mold in which crystals having a cross section of 1/8, 1/4, and 1/2 in. were grown from a common seed. The mold design was arranged so that one 1/2-in. crystal, two 1/4-in. crystals, and four 1/8-in, crystals of the same orientation could be cast. With this technique, it was possible to obtain only one set of crystals with the same orientation. Because of this limitation, it was not possible to determine both the changes of extent and slope of the various stages since a large number of crystals of the same orientation would have been required. Instead, only the change of slope as a function of the rate of metal removal was studied by abruptly altering the current density of the electrolytic polishing bath at various strains within the regions of Stages I and 11. The experimental techniques used for the tensile studies were essentially the same as those used previously.1,3 The specimens were deformed in a 200-lb Instron tensile machine, usually at a rate of 10-5 sec-5. A methyl alcohol-nitric acid solution was used as the polishing bath for aluminum. The temperature was maintained constant within ±0.l°C by means of a water bath. The tensile machine was
Jan 1, 1963
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Institute of Metals Division - The Effect of Neutron Irradiation on the Tensile Properties of the Zr-2.5 Wt Pct Nb (Cb)-0.5 Wt Pct Cu AlloyBy C. E. Ells, A. Sawatzky
The effect of neutron irradiation on tensile properties of the Zr-2.5 wt pet Nb-0.5 wt pet Cu alloy has been evaluated for integrated neutron fluxes up to 3 x 1020 n per sq cm (E > 1 Mev). Specimen temperature during irradiation was normally 300°C. The material was studied both in annealed and in quenched and aged conditions. When the alloy (fab-ricatedfrom sponge zirconium) is quenched from a temperature =40°C below the a + ß/ß transformation and aged 6 hr at 535oC, neutron irradiation up to the maximum studied has little effect 071 reduction in area, although there is a drop in uniform elongation and the yield strength is increased by = 25 pct. Conversely, irradiation of the alloy in an annealed condition can result in much greater changes in properties, with yield-strength increases of up to 200 pet. The dose dependence of irradiation hardening obeys the saturation equntion proposed by Makin and Minter to explain hardening in copper and nickel: Act = C[1 - exp(-Døt)/1/2 A rnodel is proposed to explain the effect of niobium content and metallurgical condition on irradiatiotz behavior. THE Zr-Nb alloys form a class of material susceptible to marked strengthening by quench and age heat treatment. With niobium concentrations as low as 2.5 wt pet, strengths can be developed which are double those of annealed zircaloy-2.1 Since the neutron-capture cross section of the Zr-2.5 wt pet Nb alloy is nearly identical to that of Zircaloy-2, significant gains in power-reactor neutron economy could be obtained by replacing stressed in-reactor components of Zircaloy-2 with the heat-treated Zr-Nb alloy. When the solution heat-treatment temperature is in the high (a + ß) phase, then the tensile properties of the quenched (and aged at 500°C) material have been shown to be relatively insensitive to neutron irradiation.1-3 Addition of small quantities of copper to the binary Zr-2.5 wt pet Nb alloy gives a useful reduction to the corrosion rate in air and carbon di- oxide,' and a ternary alloy of composition Zr-2.5 wt pet Nb-0.5 wt pet Cu was chosen for one component in the Douglas Point Reactor. This application utilizes both the corrosion resistance to a moist air-carbon dioxide environment and the strength developed by a quench and age heat treatment. By suitable choice of solution heat treatment and aging temperatures, tensile properties of the ternary alloy can be made nearly identical to those considered as optimum for the binary alloy. One effect of the copper addition, however, is to give marked changes in the aging kinetics of the alloy.' For this reason, it appeared that neutron irradiation might promote overaging in the ternary alloy, particularly at the elevated service temperature (=300°C). This paper describes the effect of neutron irradiation on the tensile behavior of the Zr-2.5 wt pet Nb-0.5 wt pet Cu alloy in several metallurgical conditions pertinent to its use as a reactor material. The metallurgical conditions included those for which aging occurs in the unirradiated material, and fully annealed conditions for which a higher degree of thermal stability could be expected. 1) EXPERIMENTAL Two batches of alloy were used, both made from sponge zirconium. The fabricator's analysis of principle constituents showed no significant difference between the two batches, Table I. The rod material was rolled to 1.5 in. diam, and then swaged to final sizes of 0.5 to 0.375 in. diam at nominal temperatures of 785" and 625°C for the AM and AS batches, respectively. Subsequent hydrogen analyses at CRNL confirmed that the hydrogen concentration of the as-received rod was indeed <20 ppm. However, it was found that the (a + ß)/ß transus for the AM material was approximately 25°C lower than that of the AS material, indicating rather more difference in oxygen concentration than given in Table I. Except for a small difference in yield-point behavior, the tensile prop-
Jan 1, 1965
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Natural Gas Technology - Gas Well Testing With Turbulence, Damage and Wellbore StorageBy R. A. Wattenbarger, H. J. Ramey
A systematic study has been made of the application of the real gas pseudo-pressure m(p) to short-time gas well testing. The m(p) function can be used in real gas flow problems to account for the variation of viscosity and z-factor with pressure. A mathematical model was solved numerically to generate solutions of various real gas flow problems. The effects of turbulence, formation damage and wellbore storage were included in the model. The analysis of simulated well tests showed that the interpretation methods normally used for liquid flow are generally accurate when the m(p) is used. For practical rates without turbulence, the solutions are not rate-sensifive, and the flow capacity.. kh and skin effect can be determined accurately from either a buildup or a drawdown test. However, the kh calculated from a drawdown test can be significantly low when turbulence is present. A case was simulated in which this error wa.s 36 percent. Turbulence does not affect the determination of kh from buildup tests. The proper determination of kh from p and pa buildup and drawdown plots is developed by analyzing their relationship to the m(p) method. A simple equation is given that can be used for long-range gas well performance forecasting. This expression is compared with a method pre-sended by Russell et al." Introduction The formation flow capacity and wellbore damage condition can be determined for liquid-producing tests by means of buildup and drawdown tests. These tests make use of short-time pressure transient data rather than stabilized flow tests that are often used for gas well testing. Tracy' presented a method of gas well testing that was based on ideal gas equations and utilized p2 buildup plots. This method was shown to be good for low pressure wells. MatthewsZ suggested plotting p and using an average slope and average gas properties. This method was more successful on high pressure wells. Al-Hussainy, Ramey and Crawfordh howed that variation in gas properties could be simplified by using the real gas pseu do-pressure m(p). Some cases showed that the use of the m(p) function Original manuscript received in Society of Petroleum Engineers office Aug. 8. 1967. Revised manuscript received June 11, 1968. Paper (SPE 1835) was presented at SPE 42nd Annual Fall Meeting held in Houston Tex., Oct. 1-4. 1967, and at SPE 4th Annual Eastern Regional ~eetin$ held in Pittsburgh. Pa., Nov. 2-3. 1967. 0 Copyright 1968 American Institute of Mining, Metallurgical, and Petroleum Engineers, Inc. 'References given at end of paper. provided an accurate method of interpreting buildup and drawdown tests. Because the work of Al-Hussainy et al. included only a few actual cases, there was a need to explore the use of the m(p) method for a greater variety of flow conditions. The occurrence of turbulent flow around the wellbore often is an important factor in gas well testing. Swift and Kiel,' and Carter et a1.' treated turbulence in gas well testing, but did not consider the variation of viscosity and z-factor with pressure. This paper presents the results of an investigation of the application of the m(p) method to buildup and drawdown testing. Vhe investigation included the effects of turbulence, formation damage and wellbore storage. Gas Flow Equations To formulate the mathematical model, many of the assumptions usually used in well testing theory are applied. The system has radial geometry with a closed outer boundary and is composed of a horizontal porous formation that has uniform and isotropic rock properties and uniform thickness. Allowance is made, however, for a radial region of reduced permeability near the wellbore. This region represents formation damage. The geometry of the system is shown in Fig. 1. Darcy's law does not always apply to gas flow. A more general expression is needed for non-Darcy, or "turbulent" REGION OF DAMAGED PERMEABILITY SEALED BOUNDARIES ClRCULAR WELL BORE Fig. 1—Radial flow model. AUGUST, BT7
Jan 1, 1969
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Institute of Metals Division - Dislocation Blocking in Face-Centered-Cubic MetalsBy I. R. Kramer
A delay time for yielding in cold-worked face-centered-cubic metals was found. Slip on (123) planes was observed. Glide on these planes occurred during the delay-time period before slip starts on the (111) planes. AN important approach to the study of the anchoring and blocking of dislocations is available through the delayed-yield phenomenon which has been observed in body-centered and hexagonal close-packed metal by several investigators. Clark and his associate1-5 showed that a delay time for yielding is present in mild steels and fine-grain molybdenum. Type 302 stainless, SAE 4130 normalized, SAE 4130 quenched and tempered, and 24s-T aluminum aid not have a delay time. Kramer and Maddin6 studied the delay-yield effect. in metal single crystals. While they found a delay time in body-centered-cubic metals none could be found in the face-centered-cubic metals. Later7 a delay time was found in hexagonal close-packed metals. cottrell8 has proposed an explanation for the difference in the yield phenomena of b.c.c. and f.c.c. metals based upon the anchoring of edge dislocations by the proper types of impurity atoms (C and N). In the body-centered-cubic lattice the interstitial atoms are near a cube edge and can interact with an edge dislocation, while in a face-centered-cubic lattice the distortion around an interstitial atom is of spherical symmetry and cannot anchor a screw dislocation which has practically no hydrostatic component. Cottrell's theory seems to account rather well for the behavior of body-centered-cubic . metals. EXPERIMENTAL PROCEDURE The apparatus used in these experiments is essentially of the same design as described previously.' Single crystals 1 in. long and having a diameter of % in. were placed in a pendulum which consisted of a bar 8 ft long designed with a crystal holder to accommodate the specimen at low temperatures. This portion of the apparatus was supported on fine molybdenum wires. A bar of the same diameter and length comprised the other portion of the apparatus. This bar was supported on a set of roller bearings arranged around the periphery of the bar to allow accurate alignment. This bar was propelled by means of a spring-loaded gun and allowed to strike the lead bar in front of the single-crystal specimen. SR-4 type A-8 resistance strain gages were cemented to the specimen and the strain measurements were obtained by amplifying the strain-gage output by means of a high-gain preamplifier. A tektronix 545 oscilloscope was used together with a polaroid camera to record the strain and time sweep. An Ellis Associate Bridge was used to calibrate the strain gages and calibration readings were obtained before each test. The sweep of the time signal was initiated by means of a miniature thyraton which was fired when the two bars came into contact. The single-crystal specimens were cut from single-crystal bars about 12 in. long, grown by a modified Bridgman technique. The aluminum crystals were made with material of 99.99 pct purity while the purity of the copper was 99.999 pct. A cut-off wheel was used to prepare the specimens which were then machined to the desired length. The two opposite faces of the specimen were parallel to each other and perpendicular to the axis of the specimen. The specimens were compressed 1 pct. No machining followed thereafter. In some cases prestraining was carried out in liquid nitrogen by impacting the specimens directly in the apparatus so that subsequent observations could be made without allowing the specimen to warm up to room temperature. The single crystals were compressed 1 pct at room temperature in a hand press without much control of the rate of deformation. In some cases specimens were recompressed to obtain the desired length change. As far as could be determined in these experiments this factor did not seem to influence the results. The SR-4 strain gages were glued with a cellulose type cement onto the specimen surface and baked at 45°C for 12 hr. As a check on the baking treatment gages were allowed to dry at room temperature. All delay time tests in this paper were conducted in a liquid nitrogen bath at -195°C. A schematic delay time oscilloscope trace is shown in Fig. 1. At point B the elastic stress wave caused by the impact reaches the strain gage on the specimen. The portion BC is the elastic strain. In this investigation the strain at point C was used to calculate the critical resolved shear stress by multiplying by the proper modulus depending upon the orientation of the single-crystal specimen. The time between C and D is the delay time portion of the curve. This portion of the curve is fairly flat but does have a definite microstrain associated with it. After the point D is reached the specimen deforms rapidly and the strain reaches a maximum at E. Following this, depending upon the length of the bar behind the specimen, the strain remains constant for a period and then decreases when the reflected elastic wave returns from the end of the pendulum bar. A permanent plastic strain is recorded on the oscilloscope trace and also measured by a strain-measuring bridge. The strain, E p,
Jan 1, 1960