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Institute of Metals Division - A study of the {1011} and {1013} Twinning Modes in MagnesiumBy R. E. Reed-Hill
The lattice reorientations in (1011) and (1013) twins of pure magnesium have been investigated using polarized light. Both forms (Ire subject 20 almost complete second-order twinning on the (1012) plane of the first-order twin. The observed deviations of composition planes by 6 and 3 deg, respectively, from coherent twinning planes are caused by second-order twinning. The experimental data indicate that (1011) and (1013) are reciprocal twins with a twinning shear 0.136. In a previous paper1 it was shown that the primary fracture mechanism in single crystals of magnesium strained in tension parallel to the basal plane is parting or fracture inside twins. In the temperature interval 25oto286oC, the observed twinning form, dominant in fracture, was a very small twin which formed in bands. Because these twins were very small and appeared in extensively deformed regions they did not lend themselves to X-ray analysis. Lacking Cou-ling and Pearsall's2 recently reported polarized light technique for magnesium, the twinning plane indices (K1) were originally determined by two surface composition plane measurements. This plane fell in a major zone (axis < 1120>) at an angle of 55.75 deg to the parent crystal basal plane. Because its habit deviated by 6 deg from{l0ll), 61.9 deg, the experimental data per se were not consistent with simple (1011) twinning and, for expedience, the twin was designated with habit plane indices (30341, 54.5 deg, representing the lowest set of indices corresponding to measured angles. Couling, Pashak, and sturkey3 have also found bands of reoriented lattice with a similar habit in polycrystalline specimens of magnesium and certain dilute magnesium alloys. These bands are significant because their formation in large numbers during plastic flow permit specific magnesium alloys to undergo very extensive deformation by cold rolling. Using polarized light2 they showed that the basal plane in the reoriented material was nearly parallel to the band habit and, as a result, proposed a mechanism for band formation involving a double twinning process in which (1011) twins form and then retwin according to (1012). Because of the obvious similarity between the twin bands observed in single crystals and in polycrystalline specimens, it was decided to investigate if the two phenomena were not identical and, if possible, to verify the retwinning hypothesis. The present paper is a report of this investigation and shows that the twins with the (3034) habit correspond closely to retwinned (l011) twins. Evi- dence is also given for an analogous retwinning process in (1013) twins. EXPERIMENTAL PROCEDURE Rectangular single-crystal specimen deformed in tension (stress axis in the basal plane parallel to [1010], as previously described,4 were polished electrolytically by Jacquet's method5 and etched in acetic picral.2 All twins studied in this investigation belong to a major zone, whose axis, [1210], was perpendicular to both stress axis and two sides of each specimen [(1210) surfaces]. These latter contain the plane of shear of the twins and measurements of the basal plane trace of twins on these surfaces determines the lattice orientations of the twins. The position of the basal plane in each case was determined with a polarizing microscope using a modification of the technique of Couling and Pearsall.2 For each twin the four positions of maximum extinction were measured, the data averaged, and then the pair of extinctions corresponding to the basal plane was determined by rotating the microscope stage and observing the position at which the color changed from orange to blue with a gypsum red, first-order plate inserted between the crossed Nicol prisms. EXPERIMENTAL RESULTS (1013) Twins—In general, especially in speci-mens deformed at 150°C, (1073) twins appear in greater numbers and larger sizes than (1011) twins, and the lattice reorientation inside these twins is therefore easier to study and measure. Fig. 1 shows an area of an unetched and unpolished (1210) crystal surface containing a number of (1073) twins sloping upward to the right at about 29 deg with the basal plane of the original crystal (horizontal direction). Slip line segments may be seen in both the parent crystal (running horizontally) and in the twins (sloping downward to the right at approximately -22 deg with the horizontal). As may be seen in Fig. 2, the slip lines in the twin are not at the proper angle (64 deg from basal plane of the
Jan 1, 1961
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Extractive Metallurgy Division - The Use of Oxygen Enriched Air in the Metallurgical Operations of Cominco at Trail, B. C.By T. H. Weldon, L. V. Whiton, R. R. McNaughton, J. H. Hargrave
Oxygen enriched air is being used quite extensively in the metallurgical plants of The Consolidated Mining and Smelting Co. of Canada, Limited, at Trail, B.C. The oxygen used for this purpose is a by-product from the Company's chemical plants located in the area. Most of the ore treated in the Trail metallurgical plants comes from Com-inco's Sullivan Mine at Kimberley, B.C. At Kimberley the ore is milled to produce lead and zinc concentrates which are shipped to Trail for further treatment to metal. One section of this paper deals with the use of oxygen enriched air in the suspension roasting of the zinc concentrates. In this process the concentrate is calcined for leaching preparatory to electrolytic recovery of the zinc. A second section of the paper describes the use of oxygen enriched air in operations at the lead smelter. There oxygen enriched air is used in the blast to the lead blast furnaces and in the slag fuming furnace which recovers the lead and zinc contained in lead blast furnace slag. The final section of the paper outlines the precautions necessary for the safe use of oxygen enriched air in any plant operation. The Use of Oxygen Enriched Air in the Suspension Zinc Roasters The suspension roasting of zinc concentrate developed at Trail, B.C., has been described in AIME Vol. 121, "The Electrolytic Zinc Plant of The Consolidated Mining and Smelting Company of Canada, Limited" by B. A. Stimmel, W. 11. Hannay and K. D. McBean. Since the publication of that paper, the use of oxygen enriched air in suspension roasting has been introduced as regular practice with marked advantage. The relative importance of a specific advantage may vary with changing conditions, but, in general, it may be stated that improved operation has been achieved at increased capacities. Suspension roasting is carried out at Trail in converted standard 25 ft diam Wedge roasters. The 2nd, 3rd, 4th and 5th roasting hearths have been removed and the drying hearth covered over. Drying of the concentrate is done on the drying hearth and the 1st roasting hearth. The dried concentrate, after any lump's have been broken up in a ball mill, is fed to a single burner located in the upper part of the combustion chamber. Oxygen is introduced at the burner fan along with the gases from drying, returned combustion gases from the waste heat boiler outlet and the required amount of new air. Up to 60 pct of the concentrate settles out on the 6th roasting hearth, the rest passilig out of the roaster. The product collected in the waste heat boiler is finished calcine, but the dust collected in the cyclones after the boilers is returned to the base of the combustion chamber where the sulphate is decomposed. Gases from the c'yclones go to a Cottrell precipitator. The discharges from the 7th roasting hearth and the waste heat boiler are combined with the Cottrell dust to give the finished calcine. Following small scale tests started in 1933, oxygen enriched air has been used continuously in the suspension roasting of zinc concentrate in Trail, beginning in 1937. A significant factor in promoting its use in this operation was the availability of by-product oxygen from the Company's near-by Chemical and Fertilizer Division. To-day it is standard practice at Trail to use oxygen enriched air for zinc concentrate roasting. The most important requirement in roasting a zinc concentrate for an electrolytic plant is that the zinc in the calcine should have maximum solubility. It is also desirable at Trail that the gas produced for the manufacture of suhhuric acid should have a ~naximum concentration of SO2 and that a substantial recovery of waste heat from the gas be achieved. High solubility of zinc requires that the sulphide sulphur and zinc ferrite in the calcine be kept low. These are both functions of temperature and time, with formation of zinc ferrite also dependent on contact between the iron and zinc particles. One of the inherent advantages of suspension roasting is that minimum time and contact are achieved. The limit on temperature is imposed by the fusion point of the concentrate and not by the need to control zinc ferrite formation. Operating temperatures are normally maintained within the limits of 1725" and 1850°F. A relatively low zinc sulphate in the calcine is required at Trail, and this results from discharging the calcine from the high sulphur dioxide atmosphere at a temperature above 1600°F.
Jan 1, 1950
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Iron and Steel Division - The Influence of Temperature on the Affinity of Sulphur for Copper, Manganese, and IronBy E. M. Cox, A. S. Skapski, N. H. Nachtrieb, M. C. Bachelder
As a result of using copper-containing scrap in the steelmaking process, the copper content of steels has been steadily increasing for years. Consequently the possible role copper may play in the steelmaking process and in the finished product begins to attract the metallurgists' attention. Some time ago one of the present authors forwarded the idea—based on the results of the analysis of nonmetallic inclusions extracted electrolytically from steels—that sulphur in plain carbon steels is distributed mainly between copper and manganese, the amount of iron sulphide being very small; and that, consequently, the problem of copper and that of sulphur in steel cannot be treated separately.' At the time of the publication of the quoted paper little was known about the relative affinities of copper and manganese for sulphur at high temperatures except that at moderate temperatures (below 1000°C) the affinity of manganese for sulphur is much greater. To gather more experimental data on this subject, the present authors undertook the investigation of the equilibrium constants of the reactions: 2Mn(8 or 1) + S2(g) = 2MnS(s) 4Cu(s or 1) + S2(g) = 2Cu2S (S or I)* 2Fe(s) + S2(g) = 2FeS (s or 1) over a range of temperatures wide enough to establish the dependence of these equilibrium constants on temperature. From the equilibrium constants (K = l/Ps2) the free energy of formation (affinity) can be calculated from F° = -RTln 1/PSt (1) where the standard conditions chosen are: 1 atm of sulphur pressure and the activities of condensed components equal one. The decomposition pressure, Ps2, of sulphur over the respective sulphides is too small to be measured directly, but there is a way of eliminating this difficulty by measuring the equilibrium constant of the reaction between the sulphide and hydrogen. From the latter and from the equilibrium constant of the thermal dissociation of H2S we then calculate Ps2 for the respective sulphide. 2Mn + 2H2S = 2MnS + 2H, 2H2 + S2 = 2H2S_________ 2Mn + S2 = 2MnS The numerical values of the equilibrium constant of the thermal dissociation of H2S at different temperatures were taken from Kelley's paper, "The Thermodynamic Properties of Sulfur and its Inorganic Compounds."² In previous experimental work published by Jellinek and Zakowski3 and by Britzke and Kapustinsky4 the equilibrium constants of the reactions Metal sulphide + H2 = H2S + metal were determined by passing hydrogen, at different rates of flow, over the sulphide, analyzing the resulting H2S + H2 mixture and then extrapolating the H2S/H2 ratio (which is a function of the rate of flow) to the zero speed of flow, a method necessarily involving considerable uncertainty. In the present work the equilibrium ratio was actually measured instead of being extrapolated. The apparatus is shown in Fig 1. Experimental Procedure The sulphides were prepared by the following methods: FeS Powdered iron which had been reduced with hydrogen (ferrum reduc-tum) was mixed in stoichiometric ratio with sublimed sulphur and carefully ground. The mixture was put into an alundum crucible, covered with pure sulphur, and the reaction started by touching the mixture with a glowing iron rod. After the reaction was completed the product (still containing some metallic iron) was again ground with sulphur, put into a Rose crucible, covered with sulphur, and heated in a strong current of pure hydrogen. Analysis of the final product showed 62.46 pct Fe and 36.59 pct S. Theoretical for FeS: 63.53 pct Fe and 36.47 pct S. MnS Manganese sulphide (precipitated and carefully washed with distilled water containing H2S) was dried in a Rose crucible in an atmosphere of H2S and heated in a current of hydrogen for 2 hr at red heat. The product was then ground and ignited for several hours at 1000°C in a current of hydrogen sulphide. Analysis showed 64.53 pct Mn and 36.63 pct S. Theoretical: 63.15 pct Mn and 36.85 pct S. Some MnS samples were prepared from metallic manganese and sublimed sulphur by mixing and grinding them and then heating in a current of hydrogen sulphide in an alundum tube.
Jan 1, 1950
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Part IX – September 1968 - Papers - Convection Effects in the Capillary Reservoir Technique for Measuring Liquid Metal Diffusion CoefficientsBy J. D. Verhoeven
In the past 15 years a considerable amount of experimental and theoretical work has been done concerning the onset of convection in liquids as a result of interm1 density gradients. This work, which has been doue in many different fields, is reviewed here and extended slightly to give a rrlore quantitative understanding to the probletrz of conzection in liquid metal dlffusion experinletzts. In liquid metal systems the capillary reservoir technique is currently used, almost exclusively, to measure diffusion coefficients. In this technique it is necessary that the liquid be stagnant in order to avoid mixing by means of convection currents. Convective mixing may result from: 1) convection produced as a result of the initial immersion of the capillary; 2) convection produced in the region of the capillary mouth as the result of the stirring frequency used to avoid solute buildup in the reservoir near the capillary mouth; 3) convection produced during solidification as a result of the volume change; and 4) convection produced as a result of local density differences within the liquid in the capillary. The first three types of convection have been discussed elsewhere1-a and are only mentioned for completeness here. This work is concerned only with the fourth type of convection. Local density differences will arise within the liquid as a result of either a temperature gradient or a concentration gradient. It is usually, but not always, recognized by those employing the capillary reservoir technique that the top of the capillary should be kept slightly hotter than the bottom and that the light element should be made to migrate downward in order to avoid convection. In the past 15 years a considerable amount of work, both theoretical and experimental, has been done in a number of different fields which bear on this problem. This work is reviewed here and extended slightly in an effort to give a more quantitative understanding of the convective motion produced in vertical capillaries by local density differences. The Stokes-Navier equations for an incompressible fluid of constant viscosity in a gravitational field may be written as: %L + (v?)v = - ?£ + Wv - g£ [1] where F is the velocity, t the time, P the pressure, p the density, v the kinematic viscosity, g the gravitational acceleration, and k a unit vector in the vertical direction. A successful diffusion experiment requires the liquid to be motionless, and under this condition Eq. [I] becomes: where a is the thermal expansion coefficient [a =-(l/po)(dp/d)], a' is a solute expansion coefficient [a' = -(l/po)(dp/d)], and the solute is taken as that component which makes a' a positive number. Combining with Eq. [3] the following restriction is obtained: Since there is no fixed relation between VT and VC in a binary diffusion experiment, Eq. [5] shows that the condition of fluid motionlessness requires both the temperature gradient and the concentration gradient to be vertically directed. Given this condition of a density gradient in the vertical direction only, it is obvious that, as this vertical density gradient increases from negative to positive values, the motionless liquid will eventually become unstable and convective movement will begin. The classical treatment of this type of instability problem was given by aleih' in 1916 for the case of a thin fluid film of infinite horizontal extent; and a very comprehensive text has recently been written on the subject by handrasekhar.' It is found that convective motion does not begin until a dimensionless number involving the density gradient exceeds a certain critical value. This dimensionless number is generally referred to as the Rayleigh number, R, and it is equal to the product of the Prandtl and Grashof numbers. For the sake of clarity a distinction will be made between two types of free convection produced by internal density gradients. In the first case a density gradient is present in the vertical direction only, and, since the convection begins only after a critical gradient is attained, this case will be called threshold convection. In the second case a horizontal density gradient is present and in this case a finite convection velocity is produced by a finite density gradient so that it will be termed thresholdless convection. Some experimentalists have performed diffusion experiments using capillaries which were placed in a horizontal or inclined position in order to avoid convection. These positions do put the small capillary dimension in the vertical direction and, consequently, they would be less prone to threshold convection than the vertical position. However, if the diffusion process produced a density variation, as it usually does, it would not be theoretically possible to avoid thresh-
Jan 1, 1969
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Institute of Metals Division - The Yielding of Magnesium Studied with UltrasonicsBy W. F. Chiao, R. B. Gordon
Tile sharp-yield point found in magnesium crystals in the solulion-treated and aged condition is studied by dislocation internal-friction experiments. The results show that the sharp yield is not file to the sudden release of pinned dislocations hut is movc likely due to the rapid multiplication of an initially small number of dislocations. Recovery or the dislocation internal friction after deformation is also studied. This yecovery results from the re-pinning of dislocations by a solute, presumably nitrogen, which moves with a relatively small activation energy. SHARP-yield points, when they occur, are a striking feature of the stress-strain curve generated during a tensile test. Although commonly associated with steel, sharp yielding has been found in a variety of metallic and nonmetallic crystalline materials. In particular, sharp-yield points have been found in zinc"' and cadmium3 containing nitrogen. With this background, Geiselman and Guy4 investigated the tensile properties of magnesium single crystals containing nitrogen to see if sharp yielding also occurs in this system. They found that sharp yields did indeed occur in solution-treated and aged specimens tested at elevated temperature but were not able to give conclusive proof that the sharp yield was caused by nitrogen, a yield drop being observed even in their purest crystals. Sharp-yield points have also been found in various polycrystalline magnesium alloys.7'8 In the study of the sharp-yield phenomenon it is desired to observe the behavior of dislocations in the earliest stages of the deformation process. Internal-friction experiments are useful for this purpose because dislocation damping is sensitive to the mobility of free-dislocation segments. At low strain amplitudes the damping, A, due to the the forced vibration of dislocation segments of average length L is ? =KAL4 [1] where A is the dislocation density and K, if the applied frequency is well below the resonant frequency of the dislocation segments? is a constant for the sample under observation.5 Dislocation damping, because of the fourth-power dependence on L, is particularly sensitive to the creation of free-dislocation segments during deformation. Since sharp yielding is associated with the sudden release of pinned-dislocation segments, marked changes in the dislocation damping are expected at the yield point.6 The use of the dislocation-damping observations to help elucidate the incompletely understood mechanism of yielding in magnesium is the primary objective of the experiments reported here. PROCEDURE Many investigations have shown that very marked and rapid changes occur in the dislocation damping of of a deformed material as soon as the straining is stopped.5 It was quite essential, then, for the purpose of this investigation, to make the damping measurements during the deformation of the samples. This can only be accomplished through the use of the ultrasonic-pulse method. In this method traveling sound-wave pulses are used and, in contrast to resonating-bar methods, only the sample ends are set in vibration. Thus, the sample can be gripped along its sides in the tensile-test machine without disturbing the damping measurements. In the pulse method, the decrease in the amplitude of a sound pulse is measured as it travels back and forth through the sample. If A is the amplitude after traversing a distance x and A. is the initial amplitude, A=Aoe-ax [2] and a is called the attenuation. It is commonly measured either in units of cm-I or as db per µ sec. The observed attenuation in a metal sample is due to a number of causes. These include scattering by grain boundaries and impurity particles, thermo-elastic damping, diffraction effects, stress-induced ordering of solute atoms, and dislocation damping. The total observed attenuation in a given sample usually cannot be resolved into these various components, but changes in a due solely to changes in dislocation damping can be accurately determined, provided the experiment is arranged so that all other sources of damping are held constant. It is desired to reduce the extraneous sources of attenuation to a minimum and for this reason the experiments are done on single crystals of high purity. Magnesium crystals offer the further advantage that, when properly oriented, only a single set of slip planes is active during deformation. Crystal Preparation. The method of sample preparation is similar to that of Geiselman and Guy.4 The starting material was high-purity, sublimed magnesium rod supplied by the Dow Chemical Co. Melting under Dow 310 flux was used to reduce the nitrogen content of the starting material: the fluxing was done under an argon atmosphere and the
Jan 1, 1965
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Health Physics for the Aboveground Uranium Miner and ProducerBy Joe O. Ledbetter
INTRODUCTION Health physics as a profession really got a significant start during the Manhattan Project of World War 11. The Health Physics Society has recently published its 25th anniversary issue of the journal (June 1980). There was concern over radiation exposures during and after uranium production, especially about radium and its daughter products [Jackson 19401 and, as evidenced by the frequency of articles in the literature, there still is. The reason for this concern was expressed by Harley as "Workers engaged in the mining and pro- cessing of radium-bearing materials are exposed to dusts of the parent, to radon, and to the radon daughter products. In- haled radioactive particulates may be retained in the lung or redistributed to other organs of the body. Relatively minute de- posits of radioactive substances, particularly alpha emitters, have been clearly shown to be the etiological factor in a variety of injuries to industrial and re- search workers. " [Harley 1953] Emphasis in measurements has been placed on radium in water and radon in air, since these are the principal mobilized phases; however, it should be kept in mind that radium-containing particles do become suspended in air as aerosols and radon absorbs in liquids. Much of the uranium mining and production is being carried out aboveground. The principal difference between underground and surface (pit or leach) mining of uranium is the reversal in the relative importance of roles for the types of radiation dose. For aboveground the major radiation exposure is external gamma ray, whereas for underground it is internal alpha; for aboveground, the whole body penetrating is of greater importance than the lung alpha dose. AS a result of the politics involved and the law- suits for any and all diseases as being occupationally- caused, today , more than ever before, the successful performance of the activities connected with uranium production--before-, during-, and after-the-fact-- must include the provision of first class radiation protection. Such protection can be achieved by good measurements, thorough risk evaluations, and adequate controls. Meeting the ALARA (As Low As Reasonably Achievable) philosophy necessarily entails the determination of what is reasonable exposure. The necessary and sufficient elements of radiation safety under the ALARA dictum require a hard look at the dose versus effects data. There are times when the health physicist needs to make decisions of judgement rather than compliance with a well-defined regulation value. In order to facilitate such decisions, the real world must be separated from opinions that are merely artifacts of statistical variation and from the unprovable "what ifs" that are slanted to question the morality of any non-Luddite. UNITS VOCABULARY FOR DOSIMETRY There have been many radiation quantifying and dosimetric units introduced in the past. Fortunately, most of them did not catch on enough to become required knowledge for reading the health physics literature. The unit definitions necessary for our purposes here are the following: -curie (Ci)--unit of radioactivity equal to 3.7 x 10 10 disintegrations per second Webster's 19711 or the quantity of radionuclide that undergoes 3.7 x 10 nuclear transformations per second. Environmental levels of radioactivity are usually measured in picocuries (10-l2 Ci) per cubic meter for air and in picocuries per liter (pCi/~) for water and sometimes for air. .roentgen (R)--exposure dose of x or gamma rays that gives 1 esu of charge (either sign) to 1 cc of dry air @ STP. The roentgen is equivalent to an energy absorption of 86.7 ergs/g of air [Gloyna and Ledbetter 19691. .rad--radiation absorbed dose of 100 ergs per gram of absorber. The SI unit for absorbed radiation dose is the Gray; 1 Gy = 100 rads. orem--radiation absorbed dose of 1 rad times the quality factor (QF) for that radiation. The QF is 1 for x rays, gamma rays, beta rays, and posi- trons. For heavy ionizing particulate radiation, QF is a function of the amount of energy trans- ferred per unit length of travel, i.e. , the linear energy transfer (LET); the values of QF:LET in keV/um are as follows: 1:<3.5; 1-2:3.5-7; 2-5:7-23; 5-10:23-53; and 10-20:53-175 [Morgan and Turner 19 671 . For radiobiology, relative biological effectiveness (RBE) is recommended for use instead of the quality factor above that is for radiation protection: the RBE is the ratio of the dose of 200 kVp x rays to the dose of radia- tion in question (both in rads) to cause the same
Jan 1, 1980
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Part VII – July 1969 - Papers - The Mechanical Properties of Some Unidirectionally Solidified Aluminum Alloys Part I: Room Temperature PropertiesBy J. R. Cahoon, H. W. Paxton
The mechanical properties of unidirectionally solidified A1(rich)-Mg and A1(rich)-Cu castings containing up to 15 wt pct solute have been determined with re -spect to the volume fraction of interdendritic eutectic. Pioperties were determined in the directions pumllel and Perpendicular to that of solidification; the volume fraction of eutectic was varied between the "as-cast" and equilibrizcm amounts by approperiate heat treatment following solidification. The principles of fiber strengthened composites and dispersion strengthened materials are adapted to explain the mechanical properties of these castings. It is generally accepted that castings often have inferior mechanical properties when con~pared to wrought products. However, there is little quantitative data available concerning the factors which make apparently sound castings weak and/or brittle. The relative ease and inexpensiveness of the casting process have always been attractive and, therefore, an understanding of the factors which contribute to the mechanical properties of castings would seem desirable. Such an understanding may lead to an improvement in the mechanical properties to an extent where castings would become competitive in applications where presently only wrought products are considered to have the requisite properties. Such an understanding could also improve the reliability of present cast products. Much of the recent research on castings has centered about determining the extent of segregation in cast alloys. Macrosegregation, particularly inverse segregation, has been studied in some detail 1-8 and a considerable understanding of microsegregation has been obtained.9'10 The effect of solidification rate on dendrite spacing and on the amount of interdendritic eutectic in binary alloys has been established, particularly for Al(rich)-Cu alloys.""0 However, the extension of these ideas to relate the amount of interdendritic eutectic, concentration gradients, micro-segregation, dendrite spacings, and so forth, to the rnechanical properties has been limited. Dean and spear" have related the mechanical properties of an Al-Si-Mg alloy, A356-T62, to the dendrite spacing and have shown that the mechanical properties improve with decreasing dendrite spacing. Passmore et al.12 have shown that annealing at high temperature improves the mechanical properties of Al(rich)-Cu al- loys and Archer and Kempf 13 have shown that an Al-1 pct Mg-1.75 pct Si alloy behaves in a similar manner. Ahearn and Quigley 14 have shown that high temperature homogenization also enhances the mechanical properties of an SAE 4330 steel. However, in the above investigations, no underlying reasons were suggested for the improvement in mechanical properties. The purpose of the present investigation is to relate the mechanical properties of castings to some of the solichfication variables and to derive some equations by which calculations of the mechanical properties may be attempted. In particular, the effect of the amount of interdendritic eutectic and the effect of stress direction with respect to that of solidification on the mechanical properties will be considered. The Al(rich)-Mg and Al(rich)-Cu binary alloy systems were chosen for study. The A1-Mg system was chosen because its constitutional relationships are such that large volunles of eutectic (up to 24 vol pct) may be obtained in the as-cast condition and then be completely dissolved by subsequent heat treatment at about 440°C. This allows a comprehensive study relating the mechanical properties of castings to the amount of interdendritic eutectic. Also the Al(rich)-Mg eutectic is almost a single phase 15 which should make the experimental results more amenable to theoretical interpretation and calculation. The A1-Cu system was chosen for study because of the large amount of related information available concerning segregation, dendrite spacing, and so forth. Unidirectionally solidified castings were used throughout the investigation so that the effect of solidification direction with respect to the direction of applied stress could be determined. THEORETICAL It is well known that upon solidification of binary alloy castings, the nonequilibrium amount of eutectic which forms is given by 10 where fe o is the weight fraction of eutectic, Cs is the solid solubility of solute at the eutectic temperature, k is the equilibrium partition coefficient, and C, is the average composition of the alloy. In the development of Eq. [I], it is assumed that the effects of inverse segregation and diffusion in the solid are negligible, and that no porosity is present. If the casting is homogenized at a high temperature for a long period of time, some (or all) of the eutectic is dissolved and the amount of eutectic for this "equilibrium" condition may be calculated directly from the constitutional diagram. By appropriate intermediate annealing, the
Jan 1, 1970
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Institute of Metals Division - A Constitution Diagram for the Molybdenum-Iridium SystemBy J. H. Brophy, S. J. Michalik
A constitution diagram for the system Mo-Ir has been determined. The maximum solubility of iridium in molybdenum is 16 at. pct at 2110ºC and decreases to less than 5 at. pct at 1500°C. The solubility of molybdenum in iridium is 22 at. pct. Three intermediate phases appear in the system: 8 MoJr, having the p-tungsten structure; a phase, a cornplex tetragonal structure; and the hcp ? phase. Metallography, melting point determinations, X-ray diffraction and fluorescence, and electron micro-probe unalyses were employed in establishing the diagram. PREVIOUS to the present investigation, the intermediate phases in the Mo-Ir system were identified, but no detailed account of the phase diagram has been reported in the literature. Raub1 investigated alloys of Mo-Ir over an extensive range of composition between the temperatures of 800º and 1600°C. The in-termetallic compound MosIr was found to exist with nearly pure molybdenum, as the solubility of iridium in molybdenum was not detectable parametrically in this temperature range. MO3Ir was found to be iso-morphic with a ß-tungsten type structure, having a parameter of 4.959Å. An intermediate hcp phase, designated as the ? phase, ranged in composition from 52 to 78.5 at. pct at 800ºC, and from 41 to 78.5 at. pct Ir at 1200°C. Parameters noted for the ? phase were as follows: at 42.7 at. pct Ir, a = 2.771i0, c = 4.4366, c/a = 1.601; at 78.5 at. pct Ir, a = 2.736A, c = 4.378A, c/a = 1.600. Molybdenum was found to be soluble in iridium up to 16.5 at. pct Mo (83.5 at. pct Irj, with the parameter of iridium increasing to 3.845A at the solubility limit. Knapton,2 who investigated alloys between 15 and 85 at. pct Ir, essentially agreed with Raub's data, but, in addition, found a a phase in as-melted alloys near 25 at. pcto Ir. The oaphase lattice parameters were a = 9.64Å, c = 4.96Å, c/a = 0.515. The a phase was replaced by the 8 -tungsten phase on annealing at 1600°C. Knapton concluded that the a was stable only at elevated temperatures, and placed the composition of the a phase at approximately 30 at. pct Ir. The intermetallic compound Mo3Ir, with a lattice parameter of 4.965A, was included among the 8-tungsten structures reported by ~eller.' Matthias and Corenzwit,4 and Bucke15 studied the superconducting nature of MosIr, and reported a superconducting transition temperature of 8.$K. The present investigation describes the phase relationships in the Mo-Ir alloy system determined by melting point measurements, X-ray diffraction and fluorescence, and metallography. EXPERIMENTAL PROCEDURES Alloys for the determination of the phase diagram were prepared from powders. Commercial 99.9 pct Mo from Fansteel Metallurgical Corp. and 99.9 pct Ir powder from J. Bishop and Co. Platinum Works were used. The powders were weighed to nominal compositions, mixed, and then pressed, without binder, into compacts weighing 4 to 6 g. These were presintered in uacuo between 1200' and 1400°C for 1 hr, to reduce the degree of spattering during subsequent arc-melting. The compacts were arc-melted in a nonconsumable tungsten electrode furnace six times on alternate sides on a water-cooled copper hearth in an atmosphere of zirconium-getter ed argon at 500 mm of mercury pressure. In almost all cases, this procedure yielded buttons of satisfactory homogeneity. The composition of all melted buttons were confirmed by X-ray fluorescent analysis using the experimentally determined ratio of the iridium La1 line intensity to that of the molybdenum Ka1 line as a function of composition. In this determination four alloys analyzed by wet chemical methods were used as standards. An uncertainty range of ±1 at. pct has been attributed to all indicated compositions. All heat treatments and solidus measurements were carried out in tantalum resistance heating elements in vacuum conditions of 10-4 to 10-5 mm of mercury. A detailed account of this procedure has been reported by Schwarzkopf and Brophy.8 In the heat treatment and solidus measurements of iridium-rich alloys (50 at. pct Ir or greater), a tungsten lining was inserted into the tantalum resistance heating element because of a eutectic reaction which occurs between iridium and tantalum at 1948ºc.7 Heat treatments and solidus measurements carried out at compositions less than 40 at. pct Ir both with and without tungsten linings within the resistance
Jan 1, 1963
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Extractive Metallurgy Division - Self-Fluxing Lead SmeltingBy Werner Schwartz, Wolfgang Haase
Lead sulfide concentrates, which may include other lead concentrates, are sintered on an up-draught sintering machine without the addition of any diluting agents or fluxes. Subsequently they are melted in an oil- or gas-fired rotary furnace. The sintering and melting processes are based upon the following roast-reaction: PbS + 2 PbO = 3 Pb + SO, PbS + PbSO, =2 Pb + 2 SO, For obtaining a lead bullion free from sulfur, the sintering process is carried out in such a way that the sinter product contains a small amount of excess oxygen above that to react with the sulfides. At the end of the melting process, when the reactions are finished, the remaining small amount of oxide residues is reduced with coal to which a certain percentage of soda ash (about 1 pct of the lead bullion) is added. For the lead smelting process described neither coke nor fluxes—except soda ash—are required. This process is being utilized by a European smelter successfully and with a high lead recovery. The consumption figures for the smelting of 100 tons per day of lead concentrates are indicated. The lead content of the lead concentrates from modern ore dressing plants ranges from 65 pct to above 80 pct. In most lead smelters of the world these concentrates are smelted in a blast furnace. For blast-furnace smelting the concentrates have to be desulfurized and agglomerated by sintering. A requirement for the perfect operation of a down-draught sintering machine and of a blast furnace is a maximum lead content in the feed of 40 to 45 pct. For this reason, some lead concentrates have to be diluted by adding return slags, limestone, and possibly iron oxide and sand. As an example, 100 tons of lead concentrate with 72 pct Pb would contain 13.5 tons of gangue (including the zinc). To produce a perfect sinter with 42 pct Pb it would be necessary to add 70 tons of flux and return slag, more than five times the original weight of the gangue, to the sinter mix and blast-furnace charge. A correspondingly large amount of coke would be required in order that all of these materials reach the heat of formation and the melting temperatures of the slag (1200" to 1400°C) inside the blast furnace. The roast-reaction process presents a possibility for lead recovery without dilution of the concentrates. In this process the concentrate mixed with coal is placed upon a Newnam-hearth and air is blown through nozzles into the heated mix. AS a result metalllic lead and a relatively great amount of so-called .'Grey Slag" with a lead content of 25 to 35 pct are formed. The slag is sintered to eliminate sulfur and, after addition of the requisite fluxes, treatt:d in a blast furnace. Owing to the poor recovery of lead from the hearths and to the unavoidable heavy hand-work plus the risk of poisoning this process is utilized in very few 112ad smelters today. Since in mxny countries of the world coke is expensive and difficult to obtain, it appeared feasible to use the principle of the roast-reaction by modern sintering and melting methods with recovery of the lead in electric, or oil, gas, or coal-fired furnaces. Two processes are utilized on an industrial scale: A) Lead smelting in the electric furnace of the Bolidens Gruv A/B in Sweden, as described by S. J. Walldcn, N. E. Lindvall, K.G. Gorling, and S. Lundquist. B) The self-fluxing lead smelting of Lurgi Gesell-schaft fiir Chemie und Huttenwesen m.b. H., Frankfurt a M, Germany, which is described in this paper. In the Boliden process referred to above the sinter mix is pelletized by enveloping return fines with layers of flue dust, limestone powder, and dried galena concentrate. The roasting and agglomeration are carried out on a down-draught machine, and a slight excess of sulfur is left in the sinter product. During the smelting in the electric furnance the roast-reactions occur and a slag poor in lead and a sulfur bearing lead are formed. This latter is subsequently oxidized in a converter to obtain lead bullion and dross. The Lurgi-process achieves the maximum possible extent of the roasting reaction on the sintering machine. The wet flotation concentrates are blended with return fines (lead content 70 to 80 pet), any existing flue dusts and lead slimes—but without the
Jan 1, 1962
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Miscellaneous - Relaxation Methods Applied to Oilfield ResearchBy Herman Dykstra, R. L. Parsons
A numerical method for solving partial differential equations in steady state fluid flow is described. This method, known as the "relaxation method," has two advantages over analytical methods: (1) practically any problem can be solved, and (2) a solution can be obtained quickly. A disadvautage is that the solution is not general. The method is applied to core analysis and relative permeability measurement to calculate constriction effects and to calculate the true pressure drop measured by a center tap in a Hassler type relative permeability apparatus. Further applications are suggested. INTRODUCTION Many problems in fluid flow cannot be solved analytically because of the nature of the boundary conditions. For many problems, however. an exact answer is not necessary because boundary conditions are not exactly defined or the parameters describing the porous medium are not accurately known. The relaxation method can be used to obtain an approximate answer easily and quickly for the flow of incompressible fluids in porous media. The method can also be used for other types of problems, such as determining the stress in a shaft under load. or the temperature distribution during steady state heat flow. In this discussion only calculations concerned with the flow of fluids in porous media will be considered. The method was introduced by R. V. Southwell in 1935.' THEORY The treatment given here follows that given by Enimons.2 Consider a porous medium to be replaced entirely by a net of tubes of equal length and uniform cross-sectional area as shown in part in Fig. 1. Assume that the net of tubes behaves exactly like the porous medium which it replaces; that is, the net can be made fine enough to reproduce exactly the porous medium. Assume also that Darcy's Law can be used to calculate the flow from one point to another point through these tubes. The flow from point 1 to point 0 is KA . ------ P-P) .......(11 where a is the distance between points: K is the "permeability" of a tube; A is the cross-sectional area of a tube; is the viscosity of the liquid in the porous medium; and (P1 — P0) is the pressure difference between point 1 and point 0. In like manner the flow can be calculated from points 2, 3, and 4 to point 0. The net flow into point 0 is Qo = KA/µa (P1 + P2 + P33 + P4-4P0) . . (2) MB For an incompressible fluid the net flow into point 0 will be zero or, Q. = 0. This says that at point 0 fluid is neither being accumulated nor depleted. 'Therefore. P1 + P2 + P3 + P4 - 4P0 = 0 .... (3) . If. now. with specified boundary conditions. the pressure i.; known at a finite number of points in a given region, as at the points shown in Fig. 1, Equation (3) will be satisfied at every point. If, on the other hand, the pressure is not known, the pressure can be guessed at these points. Then. unless the guess is perfect. Equation (3) will not be satisfied at all of the points. When Equatiol~ (3,) is not satisfietl. let d = P1 + I?, + P, + P, - If' .,....(4) where 6 is an apparent error and is called the residual at point 0. Equation (4) shows how much the pressure guess is in error at point 0 with respect to the surrounding points. A positive residual means that the pressure is too low, and a negative residual means that the pressure is too high. To bring the residual, 6. to zero in order to satisfy Equation (3). it is necessary to make changes in the pressure guesses. Equation (4) shows that a +1 change in Po will change the residual at point 0 by -4. A +1 change in the pressure at any of the four surrounding points will change the residual at point 0 by +l. Thus it can be seen that a change at any point will affect the residual at that point and the four surrounding points. By changing the pressure from point to point, all of the residuals can eventually be brought nearly to zero and the problem will be solved. This procedure is the essence of relaxation methods and is used to relax the residuals so that Equation (3) is satisfied at every point. The procedure can be most easily explained in detail by solving a simple problem. as Southwell says, "To explain every detail of a practical technique is to risk an appearance of complexity and difficulty which may repel the reader. A
Jan 1, 1951
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Iron and Steel Division - Reduction Kinetics of Magnetite in Hydrogen at High PressuresBy W. M. McKewan
Magnetite pellets were reduced in flowing hydrogen at pressures up to 40 atm over a temperature range of 350° to 500°C. The rate of weight loss of oxygen per unit area of the reaction surface was found to be constant with time at each temperature and pressure. The reaction rate was found to be directly proportional to hydrogen pressure up to 1 atm and to approach a maximum rate at high pressures. The results can be explained by considering the reaction surface to be sparsely occupied by adsorbed hydrogen at low pressures and saturated at high pressures. PREVIOUS investigation1,2 have shown that the reduction of iron oxides in hydrogen is controlled at the reaction interface. Under fixed conditions of temperature, hydrogen pressure, and gas composition, the reduction rate is constant with time, per unit surface area of residual oxide, and is directly proportional to the hydrogen pressure up to one atmosphere. The reduction rate of a sphere of iron oxide can be described3 by the following equation which takes into account the changing reaction surface area: where ro and do are the initial radius and density of the sphere; t is time; R is the fractional reduction; and R, is the reduction rate constant with units mass per area per time. The quantityis actually the fractional thickness of the reduced layer in terms of fractional reduction R. It was found in a previous investigation2 of the reduction of magnetite pellets in H2-H,O-N, mixtures, that the reaction rate was directly proportional to the hydrogen partial pressure up to 1 atm at a constant ratio of water vapor to hydrogen. Water vapor poisoned the oxide surface by an oxidizing reaction and markedly slowed the reduction. The enthalpy of activation was found to be + 13,600 cal per mole. It was also found that the magnetite reduced to meta-stable wüstite before proceeding to iron metal. The following equation was derived from absolute reaction-rate theory4,8 to expfain the experimental data: where Ro is the reduction rate in mg cm-2 min-'; KO contains the conversion units; Ph2 and PH2O are the hydrogen and water vapor partial pressures in atmospheres; Ke is the equilibrium constant for the Fe,O,/FeO equilibrium; Kp is the equilibrium constant for the poisoning reaction of water vapor; L is the total number of active sites; k and h are Boltzmann's and Planck's constants; and AF is the free energy of activation. Tenenbaum zind Joseph5 studied the reduction of iron ore by hydrogen at pressures over 1 atm. They showed that increasing the hydrogen pressure materially increased the rate of reduction. This is in accordance with the work of Diepschlag,6 who found that the rate of reduction of iron ores by either carbon monoxide or hydrogen was much greater at higher pressures. He used pressures as high as 7 atm. In order to further understand the mechanism of the reduction of iron oxide by hydrogen it was decided to study the effect of increasing the hydrogen pressure on rebduction rates of magnetite pellets. EXPERIMENTAL PROCEDURE The dense magnetite pellets used in these experiments were made in the following manner. Reagent-grade ferric oxide was moistened with water and hand-rolled into spherical pellets. The pellets were heated slowly to 550°C in an atmosphere of 10 pct H2-90 pct CO, and held for 1 hr. They were then heated slowly to 1370°C in an atmosphere of 2 pct H2-98 pct CO, then cooled slowly in the same atmosphere. The sintered pellets were crystalline magnetite with an apparent density of about 4.9 gm per cm3. They were about 0.9 cm in diam. The porosity of the pellets, which was discontinuous in nature, was akrout 6 pct. The pellets were suspended from a quartz spring balance in a vertical tube furnace. The equipment is shown in Fig. 1. Essentially the furnace consists of a 12-in. OD stainless steel outer shell and a 3-in. ID inconel inner shell. The kanthal wound 22 in. long, 1 1/2, in. ID alumina reaction tube is inside the inconel inner shell. Prepurified hydrogen sweeps the reaction tube to remove the water vapor formed during the reaction. The hydrogen is static in the rest of the furnace. The sample is placed at the bottom of the furnace in a nickel wire mesh basket suspended by nickel wire from the quartz spring. The furnace is then sealed, evacuated, and refilled with argon several times to remove all traces of oxygen. It is then evacuated, filled with
Jan 1, 1962
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Miscellaneous - Relaxation Methods Applied to Oilfield ResearchBy R. L. Parsons, Herman Dykstra
A numerical method for solving partial differential equations in steady state fluid flow is described. This method, known as the "relaxation method," has two advantages over analytical methods: (1) practically any problem can be solved, and (2) a solution can be obtained quickly. A disadvautage is that the solution is not general. The method is applied to core analysis and relative permeability measurement to calculate constriction effects and to calculate the true pressure drop measured by a center tap in a Hassler type relative permeability apparatus. Further applications are suggested. INTRODUCTION Many problems in fluid flow cannot be solved analytically because of the nature of the boundary conditions. For many problems, however. an exact answer is not necessary because boundary conditions are not exactly defined or the parameters describing the porous medium are not accurately known. The relaxation method can be used to obtain an approximate answer easily and quickly for the flow of incompressible fluids in porous media. The method can also be used for other types of problems, such as determining the stress in a shaft under load. or the temperature distribution during steady state heat flow. In this discussion only calculations concerned with the flow of fluids in porous media will be considered. The method was introduced by R. V. Southwell in 1935.' THEORY The treatment given here follows that given by Enimons.2 Consider a porous medium to be replaced entirely by a net of tubes of equal length and uniform cross-sectional area as shown in part in Fig. 1. Assume that the net of tubes behaves exactly like the porous medium which it replaces; that is, the net can be made fine enough to reproduce exactly the porous medium. Assume also that Darcy's Law can be used to calculate the flow from one point to another point through these tubes. The flow from point 1 to point 0 is KA . ------ P-P) .......(11 where a is the distance between points: K is the "permeability" of a tube; A is the cross-sectional area of a tube; is the viscosity of the liquid in the porous medium; and (P1 — P0) is the pressure difference between point 1 and point 0. In like manner the flow can be calculated from points 2, 3, and 4 to point 0. The net flow into point 0 is Qo = KA/µa (P1 + P2 + P33 + P4-4P0) . . (2) MB For an incompressible fluid the net flow into point 0 will be zero or, Q. = 0. This says that at point 0 fluid is neither being accumulated nor depleted. 'Therefore. P1 + P2 + P3 + P4 - 4P0 = 0 .... (3) . If. now. with specified boundary conditions. the pressure i.; known at a finite number of points in a given region, as at the points shown in Fig. 1, Equation (3) will be satisfied at every point. If, on the other hand, the pressure is not known, the pressure can be guessed at these points. Then. unless the guess is perfect. Equation (3) will not be satisfied at all of the points. When Equatiol~ (3,) is not satisfietl. let d = P1 + I?, + P, + P, - If' .,....(4) where 6 is an apparent error and is called the residual at point 0. Equation (4) shows how much the pressure guess is in error at point 0 with respect to the surrounding points. A positive residual means that the pressure is too low, and a negative residual means that the pressure is too high. To bring the residual, 6. to zero in order to satisfy Equation (3). it is necessary to make changes in the pressure guesses. Equation (4) shows that a +1 change in Po will change the residual at point 0 by -4. A +1 change in the pressure at any of the four surrounding points will change the residual at point 0 by +l. Thus it can be seen that a change at any point will affect the residual at that point and the four surrounding points. By changing the pressure from point to point, all of the residuals can eventually be brought nearly to zero and the problem will be solved. This procedure is the essence of relaxation methods and is used to relax the residuals so that Equation (3) is satisfied at every point. The procedure can be most easily explained in detail by solving a simple problem. as Southwell says, "To explain every detail of a practical technique is to risk an appearance of complexity and difficulty which may repel the reader. A
Jan 1, 1951
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Part IX – September 1969 – Papers - Critical Current Enhancement by Precipitation in Tantalum-Rich Zirconium AlloysBy H. C. Gatos, J. T. A. Pollock
It is well known that the superconducting critical current densities of many alloy superconductors may be increased by cold working and in some cases further enhanced by a short heat treatment. This latter enhancement has been attributed to the redistribution of dislocations into cell-like networks' and to the precipitation of second phase particles,2'3 which act as flux pinning centers. In a manner analogous to dislocation pinning in precipitation hardening alloys,4 it is expected that here also a critical distribution of the pinning centers should result in maximum pinning effect. Concentration inhomogeneities exist in most or all commercial alloys yet there have been only a few attempts made to determine their effect on critical current capacity in the absence of cold working. Sutton and Baker,5 and Kramer and Rhodes6 have found that the complex precipitation processes occurring during the aging of Ti-Nb alloys can result in critical current density enhancement. Livingston7-10 has clearly shown, for lead and indium based alloys, that the distribution of precipitated second phase particles is of critical importance in determining magnetization characteristics. However, these '(soft" alloys age at room temperature and the time involved in specimen preparation prevents metallographic examination in the state in which the superconducting measurements are made. Thus results with such alloys are expected to be biased towards larger precipitates and interpar-ticle spacing. The present study of Ta-Zr alloys was undertaken to examine the influence of second phase precipitation, as controlled by heat treatment, on the critical current capacity of well annealed polycrystalline material. A study of the published phase diagram11 indicated that annealing supersaturated samples containing up to 9 at. pct Zr at suitable temperatures would result in the precipitation of a zirconium-rich second phase. It was MATERIALS AND PROCEDURE The alloys were prepared from spectrochemically pure tantalum and zirconium. Analysis was carried out by the supplier. Major impurities in the tantalum were: 12 pprn of 02, 17 pprn of N2, 19 pprn of C, and less than 10 ppm each of Mo, Nb, Al, Cr, Ni, Si, Ti. The crystal bar zirconium was pure except for the following concentrations: 15 pprn of 02, 17 ppm of C, 23 ppm of Fe, 11 ppm of Cu, and less than 10 pprn each of Al, Ca, N2, Ti, and Sn. Samples were prepared in the form of 8 to 10 g but-tons by arc melting using a nonconsumable electrode on a water-cooled copper hearth in a high purity ar-gon atmosphere. Each button was inverted and re-melted three times to ensure an even distribution of the component elements. The samples were then homogenized at temperatures close to their melting points for 3 days in a vacuum furnace maintained at 5 x 10-7 mm Hg. After this treatment the buttons were cold rolled to sheets approximately 0.020 in. thick from which specimens were cut, 0.040 in, wide and 1 in. long suitable for critical current density (J,) and critical temperature (T,) measurements. These strips were then recrystallized and further grain growth was allowed by an additional vacuum heat treatment at 1800°C for 60 hr. Some second phase precipitation occurred during cooling of the furnace and a solution treatment was necessary to produce single phase supersaturated samples. This treatment was successfully carried out by sealing the samples together with some zirconium chips in quartz tubes under a vacuum of 5 x 10-7 mm Hg, heating at 1000°C for 5 hr and then quenching into water or liquid nitrogen. The samples were then heat treated at either 350" or 550°C and quenched into water or liquid nitrogen. All samples which were heat treated at 350°C were quenched in both cases by cracking the capsules in liquid nitrogen. The samples treated at 550°C were quenched by dropping the capsules into water. Analysis for oxygen in randomly selected samples indicated that the oxygen content was in the range of 175 to 225 ppm. Values of Tc were determined by employing a self-inductance technique. Jc measurements were made at 4.2oK by increasing the direct current through the wire in a perpendicularly applied field until a voltage of 1 pv was detected with a null meter. The risk of resistive heating at the soldered joints during these latter measurements was reduced by first plating the ends of the wires with indium and then soldering to the copper current leads using tin. Metallographic examinations were performed after mechanical polishing of the same samples and etching in a 4H20:3HN03 (conc):lHF(conc) solution.
Jan 1, 1970
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Part VIII – August 1968 - Papers - Deformation and Transformation Twinning Modes in Fe-Ni and Fe-Ni-C MartensitesBy M. Bevis, A. F. Acton, P. C. Rowlands
Defor~nation twinning and transformation twinning modes most likely to be operative in Fe-Ni and Fe-Ni-C martensites have been determined using a new theory of the crystallography of deformation t~inning.~ This analysis shows that potentially important conventional and nonconventional twinning modes1 have been omitted in previous analyses. Discussion is given on the relevance of the predicted twinning modes to the lattice invariant shear associated with the martensite transformation in steels and to anomalous deformation twinning in Fe-Ni-C martensites. THE two most important criteria which appear to govern operative twinning modes in metallic structures1 are that the magnitude of the twinning shear should be small and that the twinning shear should restore the lattice or a multiple lattice in a twin orientation. The latter criterion ensures that the shuffle mechanism required to restore the structure in a twin orientation is simple. These criteria have been adhered to in the prediction of twinning modes2"6 in bcc and bct single-lattice structures with axial ratios in the range y = 1 to 1.09 as, for example, encountered in martensite occurring in steels. Refs. 2 and 3 in particular consider the martensite transformation in steels and the twinning modes in these cases relate to transformation twinning, and hence the lattice invariant shear associated with the martensite transformation. The list of twinning modes which can be compiled from these sources is incomplete and the ranges of magnitude of shear considered could be unrealistically small, particularly in the case of deformation twinning. The latter consideration is supported by the fact that twinning modes with magnitudes of shear large compared with the smallest shear consistent with a simple shuffle mechanism have been established in, for example, the single-lattice structure mercury7 and the multiple-lattice structure zirconium.' In addition the anomalous deformation twins reported by Ftichrnan4 to occur in a range of Fe-Ni-C martensites still remain unexplained. It is clear that a comprehensive analysis of twinning modes likely to be operative in martensite In steels is required. The results of the application of a new theory of the crystallography of deformation twinningg to these structures are presented in this paper. The theory has been used to determine all shears which restore the lattice or a multiple lattice in a new orientation with magnitude of shear up to a required maximum. The orientation relationships between parent and twinned lattices are not restricted to the classical orientation relationships of reflection in the twin plane or a rotation of 180 deg about the shear direction. PREDICTED TWINNING MODES Twinning modes which restore all or one half of lattice points to their correct twin positions will be referred to as m = 1 and m = 2 modes, respectively. These modes are the most likely to describe operative modes in single lattice structures. The bcc m = 1 and m = 2 modes which have magnitudes of shear s in the range s < 2 and s < 1, respectively, have been given10 and are reproduced here in Tables I and 11. Detailed discussion of the crystallography of these modes and cubic modes in general will be discussed elsewhere (~evis and rocker, to be published). The four twinning elements Kl, &,ql,7)2 as well as the magnitude of shear s are given for each twinning mode, and the twinning modes are given in order of increasing shear. Two twinning modes are given in each row of the tables, the twinning mode Kl, Kz, ql, q2 and the reciprocal twinning mode with elements Kl = K,, Ki = Kl, q: = q2, and 17; = ql. The m = 1 and m = 2 twinning modes which describe twinning shears with small magnitudes of shear and simple shuffle mechanisms in bct crystals with -y = 1 to 1.09 are given in Tables I11 and IV, respectively. On increasing the symmetry of the tetragonal lattice to cubic, that is making y = 1, all modes listed in Tables 111 and IV must reduce to crystallographically equivalent variants of the modes given in Tables I and 11, respectively, or become twinning modes with both shear planes as symmetry planes in the cubic lattice and hence not considered in Tables I and 11. With the exception of this last type of mode only those tetragonal twinning modes which reduce to modes 1.1, 1.2, 2.1, and 2.2 of Tables I and I1 are considered in Tables 111 and IV. For values of y in the range -y = 1 to 1.09 the tetragonal modes and the corresponding cubic twinning modes have approximately the same magnitude of shear. The twinning modes listed in Tables 111 and IV are therefore by the criteria given above the most
Jan 1, 1969
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Part II – February 1968 - Papers - Hydrostatic Tensions in Solidifying MaterialsBy J. Campbell
Various models are discussed for the evaluation of the negative pressures which may occur in solidifying materials which exhibit various deformation modes: elastic-plastic, Bingham, viscous, or creep flow. The inadequacy of the previously proposed elastic-plastic solution for solidifying metals is revealed by comparison with the more reliable creep results which are given graphically for aluminum, copper, nickel, and iron. The maximum tensions experienced in the liquid phase of solidifying spheres ranging in size from large castings to submicron powders are in the range from —10' to —105 atm for these metals. THERE has been much recent interest in the negative pressures associated with the volume change on solidification and in the possibility of the occurrence of cavitation. Considering the freezing of a highly supercooled liquid, an attempt to evaluate the stresses in the liquid ahead of the rapidly moving solidification front has been made by Horvay1 on a microscale and by Glicksman2 on a macroscale. In a casting of a wide freezing range alloy, the pressure differential due to viscous flow of residual liquid through the pasty zone has been discussed by Piwonka and Flemings,3 In a previous publication4 the author has attempted to estimate the negative pressure occurring in the residual liquid of a spherical casting, employing an elastic-plastic model to describe the collapse of the solidified shell under the internal tension. An earlier model assuming a rigid shell was shown to be inaccurate by many orders of magnitude. The elastic-plastic model is critically reviewed here, and other models are developed which are thought to be more closely related to metals and other materials near their melting points. The spherical geometry (Fig. 1) is chosen because the highest shrinkage pressures would be developed, although the analyses are readily adaptable to cylindrical geometry. A parallel sided casting experiences little internal tension because of the relatively easy dishing inward of the sides. (This commonly observed phenomenon has previously been attributed solely to atmospheric pressure.) Furthermore, small regions of confined liquid in a large solidified volume of a casting approximate reasonably well to spherical geometry. ELASTIC-PLASTIC MODEL The author has shown4 that as solidification proceeds the internal hydrostatic tension builds up until the elastic limit of the shell is exceeded. At this point the internal pressure is closely -2Y/3. Subsequently a plastic zone spreads from the inner surface toward the outer surface of the shell. When the whole casting is deforming plastically a rather more generalized analysis taking account of the externally applied pressure PA + 2y/b gives the internal pressure as: P = Pa + 2y/a + 2ys/b - 2 Y In(b/a) [1] The 2y/a and 2ys/b terms result from the tendency of the liquid-solid and solid-vapor interfaces to shrink, reducing their energy, and thereby helping to collapse the solid phase and compress the liquid phase. The 2y/b term would be important only for powders. The last term arises because of the plastic restraint of the solid, resisting collapse and so effectively expanding the residual liquid. From Eq. [I] it is easily shown that there is a minimum in the pressure at the radius amia= y/Y [2] which is of the order of 103K for the metals aluminum, copper, and iron, and corresponds to the minimum pressure Pmin = 2 Y[l-ln(bY/y [3] The results of a fully worked out elastic-plastic solution are given in a previous reporL4 The main criticism which may be leveled at this analysis when applied to metals at their melting points is the strong dependence of the yield stress on the strain rate. The strain rate varies with both solidification conditions (e.g., whether chill-cast or slowly cooled) and during solidification, as is indicated in the following section. Thus an appropriate choice of Y is very arbitrary. Before proceeding to a discussion of models which are strain-rate-dependent, it is necessary to evaluate the strain rate as a function of the rate of solidification. SOLIDIFICATION RATE Various empirical relations have been deduced5 for the rate of thickening of the solid shell by pour- out tests on partially solidified spheres. These, however, are unsatisfactory for our purposes since they become very inaccurate when the liquid core is very small. A theoretical approach is therefore necessary, and some solutions are set out below. Making the assumptions of constant surface temperature of the casting during freezing, no superheat, and a material freezing at a single temperature, Adams8 deduces the approximate solution: which becomes when b » a: Employing a semiempirical approach vallet6 finds:
Jan 1, 1969
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Part IX – September 1968 - Papers - The Effect of Preferred Orientation on Twinning in IronBy C. E. Richards, C. N. Reid
The influence of preferred orientation on the incidence of defbrtnation tuinning has been studied. High-purity iron with almost vandonz grain orientation was cotnpared uitll iron of the sa)ne grain size and composilion lza,ing a strong (110) fiber texture. As expected from published work on single crgslfls, /he ))lean stress for the onset of luitzning-, and the l,olu)nt. fraclion of twinned nzaterial obserlled in lension differed fron the 1-a1ue.s it2 co?nPression for tnolerial with a slrong texlure. The llinning stress of "rctndorrl " )zalerial did not 17ary with the sense of the aPPlied unin.via1 stress, but sirprisinglg the incidence of 1c)i)zning- was about three 1i))zes greater ill conzp?'ession Illon in lension. These results (Ire attributed entirely to ovienbation and may be nderslood in ler?ns of the shear slresses acting on the allowed twinning syster)is. J. HE twins most commonly formed in bcc metals may be described as regions of the crystal in which a particular set of (112) planes is homogeneously sheared by 0.707 in the appropriate ( 111) direction. A similar twin-related crystal could be produced by a shear of 1.414 in the reverse (111) direction but twinning by this large displacement has never been reported. Thus, twinning is unidirectional and a shear stress which produces twinning does not do so when its sense is reversed. The sense of a shear Stress is reversed when the loading is changed from tension to compression, or vice versa. Consequently, for a given orientation of a crystal relative to a uniaxial stress, only a fraction of the twelve (112) twinning systems are geometrically capable of operating in tension, and the remaining systems may operate only in compression. Therefore, when twinning is involved, there are expected to be differences in behavior between crystals tested in uniaxial tension and those tested in compression. This has been verified experimentally by Reid et 01.' and Sherwood el al.,' although a critical stress criterion was not encountered. Furthermore, twinning stresses in colmbium," tungten, tantalum,' irn,' i-Fe,\ nd molybdenum7 single crystals have been shown to depend critically on orientation, although again twinning did not occur at a critical value of the macroscopic shear stress. However, when twinning occurs, it generally does so on the most highly stressed systems, 1--4'6'8'9 implying that the stress level does have some relevance to twin formation. In view of the large orientation dependence of twinning in bee single crystals, it might be expected that such an effect would be present in poly crystalline material which possesses a recrystallisation texture. Indeed, riestner" showed that the twinning stress in tension is very orientation-sensitive it1 <'grain-oriented, silicon-iron;" this material possessed a very strong t c m^ii a nnr x_____k . i-_ii__ ri_______j. _x r»i_._:__i preferred orientation obtained by secondary recrystallisation. Reid et a/.' observed a marked difference in the tensile and compressive yield stresses of polycrys-talline columbium which was rationalised in terms of the effect of a preferred orientation on twinning. No other such illformation is known to the authors. Several investigations of twinning in polycrystalline bcc metals have been reported in which the possible existence of a preferred orientation was not even mentioned. It is the purpose of this paper to show that there is a strong effect of texture on twinning in polycrystalline iron, and to poilt out the difficulty in eliminating preferred orientation in recrystallised metals. 1. EXPERIMENTAL METHOD Material and Specimen Preparation. Low-carbon, high-purity iron was obtained from the National Physical Laboratory in the form of $-in. diam rod which had been cold-swaged from a diam of 1 in. The composition of the material is given in Table I. The as-received bar was cold-swaged directly to 0.185 in. diam from which cylindrical tensile and compression specimens were machined. Specimen geometry is illustrated in Fig. 1. The gage length was 0.30 in. long and 0.10 in. diam; it should be noted that, apart from the extra heads which are necessary for tensile loading, the geometry and dimensions of the two types of specimen are identical. The specimens were heat treated either by sequence A or B outlined in Table 11. The essential difference between these two treatments is that in one case the material was repeatedly cycled through the y- to a-phase change in order to produce grains of almost random orientation ("random" iron)
Jan 1, 1969
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Extractive Metallurgy Division - Developments in the Carbonate Processing of Uranium OresBy F. A. Forward, J. Halpern
A new process for extracting uranium from ores with carbonate solutions is described. Leaching is carried out under oxygen pressure to ensure that all the uranium is converted to the soluble hexavalent state. By this method), alkaline leaching can be used successfully to treat a greater variety of ores, including pitchblende ores, than has been possible in the past. The advantages of carbonate leaching over conventional acid leaching processes are enhanced further by a new method which has been developed for recovering uranium from basic leach solutions. This is achieved by reducing the uranium to the tetravalent state with hydrogen in the presence of a suitable catalyst. A high grade uranium oxide product is precipitated directly from the leach solutions. Vanadium oxide also can be precipitated by this method. The chemistry of the leaching and precipitation reactions are discussed, and laboratory results are presented which illustrate the applicability of the process and describe the variables affecting leaching and precipitation rates, recoveries, and reagent consumption. THE extractive metallurgy of uranium is influenced by a number of special considerations which generally do not arise in connection with the treatment of the more common base metal ores. Perhaps foremost among these is the very low uranium content of most of the ores which are encountered today, usually only a few tenths of one percent. A further difficulty is presented by the fact that the uranium often occurs in such a form that it cannot be concentrated efficiently by gravity or flotation methods. In these and other important respects, there is evident some degree of parallelism between the extractive metallurgy of uranium and that of gold and, as in the latter case, it has generally been found that uranium ores can best be treated directly by selective leaching methods. It is readily evident that this parallel does not extend to the chemical properties of the two metals. Unlike gold, which is easily reduced to metallic form, uranium is highly reactive. It tends to occur as oxides, silicates, or salts. Two ores are of predominant importance as commercial sources of this metal: pitchblende which contains uranium as the oxide, U3O51 and carnotite in which the uranium is present as a complex salt with vanadium, K2O-2UCV3V2O5-3H2O. These ores may vary widely in respect to the nature of their gangue constituents. Some are largely siliceous in composition, while others consist mainly of calcite. Sometimes substantial amounts of pyrite or of organic materials are present and these may lead to specific problems in treating the ore. Further complications may be introduced by the presence of other metal values such as gold, copper, cobalt, or vanadium whose re- covery has to be considered along with that of the uranium, or whose separation from uranium presents particular difficulty. In general, there are two main processes for recovering uranium in common use today.'.2 One of these employs an acid solution such as dilute sulphuric acid to extract the uranium from the ore. A suitable oxidizing agent such as MnO, or NaNO, is sometimes added if the uranium in the ore is in a partially reduced state. The uranium dissolves as a uranyl sulphate salt and can be precipitated subsequently by neutralization or other suitable treatment of the solution. The second process employs an alkaline leaching solution, usually containing sodium carbonate. The uranium, which must be in the hexavalent state, is dissolved as a complex uranyl tricarbonate salt, and then is precipitated either by neutralizing the solution with acid or by adding an excess of sodium hydroxide. The latter method has the advantage of permitting the solutions to be recycled, since the carbonate is not destroyed. This is essential if the process is to be economical, particularly with low grade ores. With each of these processes, there are associated a number of advantages and disadvantages and the choice between using acid or carbonate leaching is generally determined by the nature of the ore to be treated. In the past, more ores appear to have been amenable to acid leaching than to carbonate leaching and the former process correspondingly has found wider application. With most ores, acid leaching has been found to operate fairly efficiently and to yield high recoveries. One of the main disadvantages has been that large amounts of impurities, such as iron and aluminum, sometimes are taken into solution along with the uranium. This may give rise to a high reagent consumption and to difficulties in separating a pure uranium product. Excessive reagent consumption in the acid leach process also may result
Jan 1, 1955
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Part X – October 1968 - Papers - Internal Void Formation in Powder Metallurgy TungstenBy G. Das, S. V. Radcliffe
The substructural features developed in tungsten as a function of annealing temperature (up to 2200°C) and type of material [undoped and doped powder metallurgy (PM) tungsten and electron beam melted tungsten] have been investigated by transmission electron microscopy. For doped PM tungsten wires, characteristic "par-ticulate" substructural features developed rapidly with increase in annealing temperature above 700°C. The features consisted of parallel rows of elongated or circular shapes (500 to 1000A diam) lying along the direction of the wire axis and were identified as internal voids by diffraction contrast experiments. In recrystallized doped PM rod, larger voids were observed and were identified by precision dark field analysis to be cubic in shape and bounded by (100) planes. In marked contrast with both the doped PM materials, recrystallized undoped PM rod exhibited only very occasional and randomly arranged voids. Furthermore, no voids were observed in either material after electron beam melting. The high concentration of voids in the doped PM materials is attributed primarily to vaporization of doping additions or their pvoducts situated at the original grain boundaries , whereas the few voids in undoped material are considered to be traces of microporosity which were not eliminated during sintering. A tentative mechanism is suggested for the dezlelopment of the voids in relation to the processing sequences (sintering and working) and to the subsequent annealing. In recent years, a characteristic substructural feature consisting of rows of small elongated or circular regions of light contrast lying along the direction of working has been seen in thin foil electron microscopy studies of annealed sheet, wire, and rod tungsten. These features were present in the published micrographs of sheet by Weissmann et al.1 and of wire by Meieran and Thomas2, although the authors did not draw attention to them. Wronski and Fourdeux3 observed similar features in sintered rod tungsten (it was not specified whether or not the material was doped*) and interpreted them on the basis of their ap- particles, based on extraction replica evidence from the fracture surface of the initial hot-rolled slab material from which the sheet was prepared. No diffraction contrast experiments on the features were reported in any of these studies. The present investigation was undertaken with the primary objectives of: a) identifying the nature of these substructural features in tungsten by electron diffraction contrast experiments, since the contrast for voids can be expected to differ from that for crystalline or glassy particles, and b) elucidating the origin of the features and their development. For the latter purpose, doped and undoped powder metallurgy tungsten was obtained as rod and wire to represent different stages of reduction during final processing. These materials were examined both in the as-processed condition and after annealing to successively higher temperatures. In addition, the same doped and undoped materials were examined after vacuum melting in rod form. I) MATERIALS AND PROCEDURE Doped powder metallurgy (PM) tungsten wire (commercial purity 99.9 pct W) was obtained in the as-drawn and surface ground condition (0.030 in. diam "ground seal rod"). Doped and undoped tungsten rod (0.075 in. diam) representing an earlier stage of final processing was obtained from the same commercial source (Refractory Metals Division, General Electric Co.). Lengths of both the doped and undoped rod materials were single-pass melted in an electron-beam zone refiner to examine the effect of vacuum melting on the substructure. Annealing was carried out in a tungsten crucible in a tantalum strip resistance furnace under a vacuum of l0-15 mm Hg. Longitudinal sections of the wire and rod materials were examined by light and electron microscopy. The preparation of thin foils suitable for electron transmission from 0.030 in. diam tungsten wire and the rod specimens was carried out by means of a high-precision microjet technique developed to provide lack of jet stability and precise control of the area thinned. The method is described in detail elsewhere.' The foils were examined in a JEM 6A electron microscope using a goniometer stage (±20 deg tilt, 360 deg rotation) and operated at 100 kV. To minimize contamination problems a 200 µ condenser aperture was used in conjunction with a useful beam current of 50 µA. II) RESULTS AND DISCUSSION A) Diffraction Contrast Analysis. In order to determine the optimum conditions for the development of the substructural feature, a series of isochronal 30 min annealing experiments were carried out on specimens of the doped PM tungsten wire. The transmission electron microscopy analysis showed that the as-drawn wire, Fig. 1(a), consists of 'fibers' whose long axis is closely parallel to the wire axis of (110). The fiber width averages some 0.5 µ. Dense disloca-
Jan 1, 1969
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Extractive Metallurgy Division - Equilibrium Pressure Measurements Above ZnS from 680° to 825°CThe pressure of the gas in equilibrium with sphalerite has been determined in the temperature range of 680' to 825°C, using the Knudsen orifice method. A comparison of these experimental pressures with those calculated from thermal data and from other equilibrium measurements shows that the vapor above sphalerite is predominantly dissociated ZnS. Equations have been given for correctly calculating dissociation pressures using the Knudsen orifice method. It has been shown that the experimentally determined pressure is the same, whether the zinc sulphide is sphalerite or not, or a mixture of wurtzite and sphalerite. CONFLICTING points of view appear in the literature on the constitution of the vapor in equilibrium with solid zinc sulphide in the vicinity of 800°C. By comparing the dissociation pressure calculated from thermodynamic data and the vapor-pressure determination of ZnS by Veselovski,1 Lumsden2 has concluded that the vapor consists largely of dissociated ZnS. Sen Gupta,' however, concludes from his spectroscopic determinations that the vapor is largely ZnS molecules. In view of the fact that the thermodynamically calculated' dissociation pressure is higher than that experimentally measured by Veselovski, it seemed in order to repeat Veselovski's measurements. Experimental Procedure The method used for the determination of the pressures in this papel- is the Knudsen effusion cell. The apparatus and procedure were described in a previous paper- from this laboratory on the determination of the vapor pressure of silver. The only difference is that the Knudsen cell in this work is made from platinum and there is no external cover around the cell. The cell is an ordinary platinum crucible of 2.2 cm top diameter with a capsule cover. It was thought that platinum might stand up at these temperatures to the solid and gaseous ZnS, since it was found that the weight of the platinum cell itself did not change appreciably on heating ZnS in it at the working temperatures. To insure that reaction of the zinc sulphide with the cell was not giving' a false value, a stabilized zirconia cell was employed for check runs. Fig. 1 shows the comparison, which is satisfactory. Veselovski previously had measured the vapor pressure of ZnS using a silica Knudsen effusion cell. On repeating his experiment in this laboratory, it was found that ZnS at-tacked the silica cell, giving it a marked frosty appearance. This led to the belief that Veselovski's result:; may be in error. Also, he was operating at pressures above the range ordinarily considered safe for the Knudsen method. The effusion rate was measured by weighing the cell before and after each run. The weight loss during heating to temperature and cooling down was measured and subtracted from the weight loss during the actual run. The zinc sulphide used in this investigation was from two sources: Fisher cp grade, and a sample of pure sphalerite supplied by Mr. E. A. Anderson of the New Jersey Zinc Co. Before and after the series of runs with Fisher ZnS, X-ray analysis showed that both wurtzite and sphalerite were present. However, the ratio of sphalerite to wurtzite increased. All measurements were made below the transition temperature which has been reported" to be 1020°C. The data obtained in this investigation are tabulated in Table I. The pressure was calculated by the usual Knudsen formula" on the assumption that ZnS molecules were effusing. From these data, using pure sphalerite in the platinum Knudsen cell, the vapor pressure of ZnS, in mm of Hg, as a function of temperature is given by the solid line in Fig. 1. The best straight line, as determined by the method of least squares, is given by 14405 logpzns =-14405/T +11.032. A comparison of these results with Veselovski's shows that his results are about 50 pct lower. Discussion The vapor in equilibrium with solid zinc sulphide in the temperature range of this study will consist of Zn, S2, and ZnS mol, since other species of zinc and sulphur' are relatively unstable. The question to be settled is whether or not ZnS is largely dissociated. The derivation8 which follows gives the method of calculating the pressure of zinc and sulphur over solid ZnS, assuming complete dissociation, from Knudsen cell data. The free energy of the reaction 2 ZnS(solid) ? 2 Zn(gas) + S2(gas) is given by ?F?° = -RT In K = —RT In p12p2 where p1 is the zinc pressure and p is the sulphur pressure. If dissociation occurs in a closed system,
Jan 1, 1955
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Part IX – September 1969 – Papers - Preferred Orientations in Cold Reduced and Annealed Low Carbon SteelsBy P. N. Richards, M. K. Ormay
The present Paper extends the previous work on cold reduced, low carbon steels to preferred orientations developed after various heat treatments. In recrystal-lized rimmed steel, cube-on-comer orientations increased with cold reductions up to 80 pct. Above that {111}<112> and a partial fiber texture with (1,6,11) in the rolling direction dominated. During grain growth, cube-on-corner orientations have been observed to grow at the expense of {210}<00l>. In re-crystallized Si-Fe (111) (112) and cube-on-edge type orientations are dominant near the surface and the (1,6,11) texture near the midplane for reductions up to 60 pct. With larger reductions {111)}<112> and the (1,6,11) texture are dominant. In cross rolled capped steel a relationship of 30 deg rotation was observed between the (100)[011] of the rolling texture and the main orientations after re crystallization. Most orientations present in recrystallized specimens can be related to components of the rolling texture by one of the following rotations: a) 25 to 35 deg about a (110) b) 55 deg about a (110) C) 30 deg about a (Ill) THE orientation texture of recrystallized steel is of interest where the product is to be deep drawn, because preferred orientation is related to anisotropy of mechanical properties such as the plastic strain ratio (r value);1,2 and in electrical steel applications where a high concentration of [loo] directions in the plane of the sheet improves the magnetic properties of the material. It is interesting to note that both these aims are to a large extent achieved commercially, even though the orientation texture of cold rolled steel does not show large variation3 and the recrystallized orientations are generally given as being related to the as rolled orientations mostly by 25 to 35 deg rotations about common (110) directions.4-6 There is, as yet, no single completely accepted theory on recrystallization. The three mechanisms that have been investigated and discussed are: a) Oriented growth b) Oriented nucleation c) Oriented nucleation, selective growth Largely from the observations of the recrystalliza-tion process by means of the electron microscope,7-11 there is now considerable evidence that the "nucleus" of the recrystallized grain is produced by the coalescence of a few subgrains to form a larger composite subgrain, which finally grows by high angle boundary migration into the deformed matrix. From the intensive work on the recrystallization of rolled single crystals of iron, Fe-A1 and Fe-Si al-loys4-" he following observations have been made: 1) The change in orientation during primary recrys-tallization can usually be described as a rotation of 25 to 36 deg about one of the (110) directions. 2) The (110) axes of rotation often coincide with poles of active (110) slip planes. 3) If several orientations are present in the cold rolled structure, the (110) axis of rotation will preferably be a (110) direction that is common to two or more of the orientations. 4) With larger amounts of cold reduction (70 pct or more) departure from these observations became more frequent. 5) After larger cold reductions, rotations on re-crystallization about (111) and (100) directions have been observed. K. Detert12 infers that a rotation relationship of 55 deg about (110) directions is also possible, by stating that the recrystallized orientation {111}<112> can form from the orientation {100}<011> of cold reduced partial fiber texture A.3 The observation by Michalak and schoone13 that (lll)[l10] formed during recrys-tallization in fully killed steel containing (111)[112],— as well as (001)[ 110] which is related to the {111}<011> by a 55 deg rotation about <110>-implies a possible 30 deg rotation relationship about the common [Ill]. Heyer, McCabe, and Elias14 have recrystallized rimmed steel after various amounts of cold reduction, by a rapid and by a slow heating cycle and found that the preferred orientations strengthened with increased cold reduction. The most pronounced orientation up to about 70 pct cold reduction was found to be {1 11}< 110>, after 80 pct cold reduction both {111}<110> and {111}<112>, after 85 and 90 pct cold reduction, {111}<112>, and after 97.5 pct cold reduction it was {111}<112> and (100)(012). In the present work, the orientation textures of the recrystallized specimens are examined under various conditions of steel composition, amount and method of cold reduction, and method of recrystallization. The relationships between the preferred orientations of the as rolled and recrystallized specimens, and the conditions for the formation of the various orientations during recrystallization are investigated.
Jan 1, 1970