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By M. Metzger, L. E. Hendrickson

Grain boundary attack in 16 pct HCl was found to be substantially the same at low penetrations in zone-refined aluminum (individual impurities 0.1 at. ppm), superior electrolytically refined aluminum (51 at. ppm), and aluminum with various impurities at much higher levels. It was concluded that impurity atom segregation affecting corrosion would have been detected and that the corrosion susceptibility did not originate in this segregation but in the structure of the boundary. It was pointed out that the significance of most previous studies in this system had been obscured by an unrecognized autocatalytic copper reaction. Although general corrosion rate was also impurity-insensitive , there was shallow pitting attributed to iron seg-regation and a hillocked surface texture associated with copper; these were interpreted as due to cathodic damage affecting- cathode distribution. THE grain boundary corrosion suffered by high-purity aluminum in hydrochloric acid has been the object of some interest (the earlier work is summarized in Ref. 1). The central metallurgical question here is whether the corrosion susceptibility of a boundary originates in its structure or in impurity atom segregation. An attempt to study this question revealed large catalytic effects associated with small quantities of the copper impurity in the aluminum, 220 ppm, or in the corrodent, and these magnified the preferential boundary attack and obscured the intrinsic susceptibility question.' After the catalytic effects had been examined,"' test conditions could be designed to avoid them and methods developed for studying the shallow boundary penetrations prevailing when they were absent.= It then became possible to determine whether intrinsic boundary corrosion in aluminum involves impurity segregation. The older work provided no firm information on grain boundary segregation of specific solutes influencing corrosion although several studies suggested iron segregates.4,5 perryman4 found in 10 pct HC1 that the slowly developing (microns per month) grain boundary grooves were deeper in material of higher iron content (range 10 to 550 ppm, with 5 to 80 pprn Cu) but he did not measure the depths of general corrosion, which were probably several times greater, and his reference surfaces may have varied more than did the groove depths. Metzger and Intrater's results for 20 pct HC~,' which yielded higher time-average rates (mm per month) and deeper penetrations, suggested that boundary segregation of iron (range 4 to 230 ppm, with 22 pprn Cu) decreased the penetration rate. However. in the stronger acid the autocatalytic l.E. HENDRICKSON, Student Member AIME ,and M. METZGER, Member AIME, are Research Assistant and Professor of Physical Metallurgy, respectively, Department of Mining, Metallurgy and Petroleum Engineering, University of Illinois, Urbana, Ill. Manuscript submitted March 11, 1968. IMD effect of the copper impurity is greater1,2 and it is now evident that their corrosion rates had been much magnified by this effect and did not provide a proper basis for the analysis of segregation. In exploratory studies of other solutes (made under the same conditions), 1000 ppm additions of Mg, Mn, or Si or 100 ppm Ca were without effect.1 Montariol6 noted that boundary attack in 22 pct HC1 persisted after zone refining although with fewer deep fissures (ranges 0.06 to 4 ppm Cu, 4 to 23 ppm Fe). Autocatalytic effects may have influenced these results also and those of Perryman.4 The present objective was, as a first step, to see whether quantitative tests designed to exclude autocatalytic influences would indicate the existence of low-level impurity effects on intrinsic boundary corrosion. Comparison of electrolytically refined with zone-refined aluminum of lower copper and iron contents revealed no differences in boundary corrosion, but certain impurity-sensitive differences in general corrosion morphology were noted and investigated further at higher impurity levels. I) EXPERIMENTAL PROCEDURE A) Material. A selection from commercially available material was made with the cooperation of several producers. An electrolytically refined lot (III-A, 1 ppm Cu, 2.4 ppm Fe) studied previously3 provided a starting point. Since material of substantially higher copper content could not be used if the autocatalytic corrosion reaction were to be avoided,2,3 a lot (III-B) of about the same purity was added as a check, two zone-refined lots (I-A and I-B) with copper and iron an order of magnitude lower were selected for comparison, and an intermediate lot (11) was included. Analytical data are given in Table I. For copper in I-B and iron in I-A and I-B, the actual concentration is thought to be near the limit given, i.e., about 0.1 ppm. For titanium, vanadium, and chromium in III-B, the actual amounts are thought to be, like those in III-A, substantially lower than in the zone-refined lots (these elements concentrate in the solid on freezing). Data are given later for some additional lots surveved. B) Specimen Preparation and Procedure. one by 3 cm blanks with a notched stem were cut from 1-mm cold-rolled sheet, annealed 24 hr in air at 650°C, and quenched in an air stream (42°C per sec initial cooling rate, 100 sec to cool to 100°C). The high annealing temperature maximized diffusivities and approach to equilibrium impurity distributions. A water quench, in principle more efficient in preserving the distribution established, was undesirable because the boundaries were almost plane and they tended to shear and migrate during the quench and thus to be separated from any existing impurity atmosphere. Test procedures, previously described,3 involved electropolish-ing, etching 2 min in 10 pct HF at 24.0°C, and expos-

Jan 1, 1969

By T. H. Alden

T. H. Alden (General Electric Research Laboratory)—This paper as well as earlier ones of Dr. Wood represent an important contribution to the experimental description of fatigue fracture. The mechanism of fracture proposed by the authors, however, is not established by this data nor supported by other data existing in the literature. Although taper section metallography provides a rather detailed picture of fatigue crack geometry, photographs so obtained must be interpreted with care. The narrow bands revealed by etching, frequently associated with surface notches, are labeled by the authors "fissures". Measurement shows, taking into account the 20 to 1 taper magnification, that the depth of these structures is at most 2 to 3 times the width. This distinction is important in the conception of a mechanism of crack formation. It is difficult, for example, to imagine a deep, narrow fissure arising from a "ratchet slip" model. A surface notch, on the other hand, may form easily by this mechanism. The notches observed in the present work are the subsurface evidence of the surface slip bands or striations in which fatigue cracks are known to originate.4-6 It is clear that an understanding of the structure of these slip bands is of key importance in understanding the mechanism of fracture. The evidence presented shows that these regions etch preferentially, possibly because they contain a high density of lattice defects, or as the authors state equivalently, because they are "abnormally distorted." However, it is not possible to conclude that the distortion consists of a high density of vacant lattice sites. The fact of a high total shear strain in itself does not assure a predominance of point defects as opposed to other defects, for example, dislocations. Other evidence in the literature which suggests unusual densities of point defects formed by fatigue7-' refers not to the striations or fissures, but to the material between fissures (the "matrix"). If a choice must be made, the preferential etching would seem to be evidence for a high dislocation density, since dislocations are known to encourage chemical attack in copper;g no such effect is known for the case of point defects. A third alternative is that the slip bands are actually cracked, but that near its tip the crack is too narrow to be detected by the authors' metal-lographic technique. In this case the rapid etching can be readily understood in terms of the increased chemical activity of surface atoms. Unless a vacancy mechanism is operative, the motion of dislocations to-and-fro on single slip planes will not lead to crack growth. Point defect or dislocation loop generation are the principal non-reversible effects predicted by this model. In any case, the nonuniform roughening of the surface in a slip band6 requires a flexibility of dislocation motion which is not a part of the to-and-fro fine slip idea. The same is probably true of crack growth by a shear mechanism. Either some dislocations must change their slip planes near the end of the band and return on different planes,'0 or dislocations of opposite sign annihilate." The mechanism by which these processes occur in copper at room temperature or below is that of cross slip. Thus cross slip appears to be essential to fatigue crack growth.6'10"12 The fact that a tensile stress opens the slip bands into broad cracks does not indicate the structure of the bands or the mechanism by which cracks form. The charactersitic concentration of slip into bands during fatigue shows a low resistance to shear strain in these regions. (This fact in itself may be inconsistent with a high concentration of vacancies.) The authors contend also that continuing shear produces an additional mechanical weakening so that the bands fracture easily (are pulled apart) under the influence of the superimposed tensile stress. It is equally possible that the only weakness is a weakness in shear, that the crack propagates by a shear mechanism, and that subsequently the tensile stress pulls the crack apart. Even the direct observation of bands opened by a tensile stress would not be conclusive since, as argued above, they may be fine cracks. The same argument applies to internal cracks, their existence in the presence of a tensile stress not indicating the mechanism of formation. Internal cracks originating in regions of heavy shear have also been seen following tensile deformation of OFHC copper,13 so that this mode of fracture is not unique to combined tensile and fatigue straining. The authors point out in their companion report14 that 90 pct of the cracks formed during pure tor-sional strain were within 8 deg of the normal to the specimen axis. If the tensile stress were an important factor in crack propagation, it is surprising that the cracks cluster about the plane in which the normal stress vanishes. Similarly, a study of zinc single crystals showed that for various orientations the life correlated well with the resolved shear stress on the basal plane,'= and was not dependent on the normal stress across this plane. W. A. Wood and H. M. Bendler (Authors' reply) -Dr. Alden's discussion emphasizes the essential point in the relation of slip band structure to

Jan 1, 1963

By J. D. Sudbury, J. E. Landers, D. A. Shock

The external corrosion of casing is one of the most important problems facing the present day production man. A 1953 NACE report' estimated the annual cost of casing corrosion at $2,200,000 in 22 fields studied. The fields represented only 10 per cent of the wells in the United States. It was significant that 77 per cent of the failures reported were due to external corrosion. A variety of means for combatting the casing corrosion problem have been discussed in papers such as the NACE survey' mentioned previously. No attempt to revicw these will be made in this paper. Thc scope of this paper has been limited to a discussion of the following major items: (I) an instrument for studying external electrolytic corrosion; (2) use of this instrument to determine the quantity of protective current required to prevent corrosion of casing; and (3) problem of accelerated external corrosion of the oil string at the base of the surface string. ELECTROCHEMICAL MECHANISM OF CORROSION It IS gcncrally belleved that one major cause of external corrosion is the existence of electrolytic cells operating between various formation waters. A theoretical discussion of the role of earth potentials in casing corrosion has been presented by L. de Witte and F. J. Radd.2 A brief picture of the electrolytic corrosion action between two differcnt formations (A and B) is presented in Fig. I. This picture is a review to many but is given to insure clarity. In the anode area, oxidation takes place as iron ions go into solution in formation A as a product of corrosion. In the cathode area. reduction takes place and hydrogen atoms are formed at the boundary between the pipe and formation B. The flow of electrons. as indicated. is into the pipe at the anode or corroding area and out of the pipe into the formation at the cathode. In order to conform with regulations of this journal, the flow of a conventional current (I! is also indicated in this sketch. All subsequent references will be to this so-called conventional current flow and will be indicated by the symbol (I). As this action takes place the layer of hydrogen developed on the cathode offers a resistance to the flow of current in the cell. It is said (hat the cathode has been polarized. This polarizing film can be rcmoved by addition of a so-called dcpolarizing agent which reacts with and removes this hydrogen film. Such an agent must be present in ordcr for this corrosion reaction to go at a rate sufficient to cause a severe corrosion problem. The two common depolarizing agents are: (I) oxy-sen. which readily reacts with hydro gen to form water, and (2) certain bacteria which use atomic hydrogen as part of their life process. It is not difficult to explain the presence of these agents. Oxygen may be present in some very shallow formations. Sulfate reducing bacteria are found to exist in nearly any ground where mud pits might be dug. THE CASING POTENTIAl-PROFILE Instrumentation A sketch of the equipment* uscd in determining casing potential profiles is shown in Fig. 2. The tool is run in the hole using a hoist truck with a three-conductor cable. This tool must be run with tubing and rods out of the hole and should be run with the flow line disconnected. By proper choice of electrode size it can be run in any size casing. The electrodes must be run in an open hole or a hole filled with oil. Measurements cannot be made while immersed in water. The tungsten carbide-tipped knives serve as the electrical robes and arc spaced 25 ft apart. The potential difference along a 25-ft section of casing is measured with a potentinmeter to an accuracy of about 5 mv. Current flowing in the pipe can then

Jan 1, 1956

By H. R. Spedden, A. M. Gaudin, M. P. Corriveau

A preliminary study of silver ion adsorption by sphalerite in ion exchange column with influent electrolyte marked with radiosilver is described. Rapid ion exchange occurs at first followed by slow reaction controlled perhaps by solid state diffusion. One experiment with radiocopper instead of radiosilver is reported briefly. IT has been known for many years that sphalerite is floated after it has been activated by a metallic cation, particularly copper.' The activation of sphalerite by copper is known to be an exchange of an atom of copper for an atom of zinc at the surface of the sphalerite.2,3 It has been estimated from various guesses of the available mineral surface that the depth of the copper-bearing coating is of the order of thickness of one atom. However, the exact mechanism of the activation process is unknown. A number of metals other than copper act in the same general manner."' " In particular, it has been known that silver replaces zinc at the surface of sphalerite. As copper is usually divalent, whereas silver is monovalent, it may well be assumed that there are differences, perhaps major differences, in the detailed scheme of activation by these two cations. Furthermore, since silver has unusual photoelectric properties and may be a contributor to the fluorescence of sphalerite, a study of its activating mechanism might open up some interesting avenues for exploring these other phenomena. The choice of silver as an activator of sphalerite was suggested also by the fact that its radioactive tracer, silver 110, is particularly convenient in that it has a long half-life and is energetic enough to permit counting through a counter window. The experimental technique selected, therefore, included the preparation of solutions of silver nitrate con- taining a proportion of active silver nitrate sufficient to give convenient counting data. In further considering the method to be used, a desirable choice seemed the use of batch experimentation in which a given solution was allowed to act on a certain lot of mineral for a given length of time at a given temperature, this period of mutual reaction being followed by analyses of the separated solid and solution. But an alternative method seemed more attractive. This is the method now so familiar to the users of ion-exchange resins, which was first made famous by the Russian chromatographer, Tswett.6-8 It consists in forming the mineral into a porous column through which the solution is allowed to flow at a constant rate. The usual method of allowing a batch of solid to react with solution is the equivalent of a single plate distillation operation while the chromatographic or ion-exchange column is a multiple-plate method—the multiplicity of the plates being represented by the reciprocal of the rate of flow of solution through the column. It seemed to us that the chromatographic method had such

Jan 1, 1952

By J. Nutting, D. H. Kirkwood

The oxidation of lead sulfide in air between 200° and 350°C has been investigated by electron diffraction from thick sulfide films and from galena surfnces. It has been demonstrated that sulfate is the stable reaction product up to 570°C. Sulfate is HAGIHARA has investigated' single crystals of galena roasted in air by the reflection electron-diffraction technique, which owing to the very limited penetration of the beam into the crystal gives information of the nature of the surface only. He has shown that up to 280°C the first oxidation product is lead sulfate, followed by lead mono-oxysulfate (PbO . PbS04). At longer times and higher temperatures more complex patterns appeared which could not be analyzed. All of these patterns were of streaks or spots arising from crystals oriented on the galena surface, and it is probable that these crystals are lead compounds whose structures have not been determined, such as the other oxysulfates (2Pb0 • PbS04 and 4Pb0 . PbS04) or a number of oxides. Certain lead sulfide films, formed chemically, give ring patterns in transmission electron diffraction2 because they are polycrystalline, and should also give ring patterns of the products after oxidation. It was thought that a diffraction study would reveal the sequence of phases produced in the reactions at different temperatures, since X-ray powder patterns are available for many lead compounds. PREPARATION OF FILMS The films were prepared by passing H2S over a saturated solution of lead nitrate in water. Once a silvery film had formed on the solution surface, no further thickening was apparent. The films were transferred by a gauze to a bath of distilled water for washing and pieces of film were caught on small discs on which they were dried. The discs were formed initially on galena up to temperatures of 300°C, followed by oxide and oxysulfates in turn at longer times. The appearance of- these phases is believed to result from an inadequate rate of supply of sulfur to the top surface 01. the crystal. standard Siemens mounts, made of platinum alloy, and had seven 20-p apertures drilled through them. The parts of the film which had dried onto the disc surface were light blue in color, which is the interference color of a film about 600A in thickness. A strong pattern of lead sulfide was obtained in transmission electron diffraction through the apertures but slight broadening indicated a crystallite size of around 200A. Tilting a sulfide film in the beam produced arcing of the rings, increasing the intensities of the (Ill), (3111, and (222) rings and reducing (200) and (220). This arises from preferred orientation in the film, a [loo] direction of the crystallites being normal to the plane of the film. These specimens were oxidized in an oven maintained at the required temperature. The reported times include that taken to heat the film to the reaction temperature. STABLE PHASES FORMED IN OXIDATION The conditions in which various oxidation products of lead sulfide are stable have been considered by the authors in a previous paper.3 It was shown that in a normal atmosphere, taken as containing lo-' atm of SOs, lead sulfate would be stable up lo about 570°C. This was confirmed by oxidizing thin films of sulfide for several days, and the analysis of the transmission-diffraction pattern is given in Table 1. The fit with the patt$rn from X-rays is good, except for the missing 3.62A ring. Some disagreement in intensities of reflections given by X-rays and electrons is to be expected. Up to 570°C a spotty pattern of sulfate was still obtained, indicating grain growth, but above this temperature the film disintegrated. Probably this is associated with the decomposition to PbO . PbS04. It needs to be emphasized that the atmosphere

Jan 1, 1965

By Borje Hjortzberg-Nordlund

THE great Swedish export iron ore mines are Kiruna and Malmberget in the north above the Arctic circle and Grängesberg in Central Sweden, see Figs. 1 to 3. These mines exported in 1951 about 13 million metric tons of high grade iron ore and concentrates. The origin of these three ore fields seems to be the same. They are of pre-Cambrian age and are regarded as typical instances of primary eruptive ore that has thrust up as glowing masses of lava flow between two somewhat older beds of porphyry. Apparently the ore and the porphyry became segre. gated from common parent magmas by a process of differentiation. Despite the fact that the Kiruna orebody belongs to the earliest pre-Cambrian formation, it has been influenced to an unusually small extent by later metamorphosisms, apart from its having been set on edge through folding and wrenching off by a number of later faults. The Kiruna ore occurs along a stretch of more than 4 miles as a series of slabs or lenses sloping steeply toward the east and sandwiched between two beds of porphyry. The main orebody has a length of about 3 miles and an average width of 300 ft with a maximum of 600 ft. The dip varies from 65" to 45" toward the east and the known depth is 3000 ft, although magnetic surveys indicate it may be at least 6000 ft. Malmberget has undergone a more thorough transformation, having been pressed and crumpled into a meandering band of disconnected layers and lenses. The largest of the more connected bodies of ore, the Great Ore Layer, outcrops on a low mountain ridge and has a total length of about 4 miles and a maximum width of about 300 ft. The dip varies from 30" to 70" towards the north. The main orebody in Grangesberg, the so-called

Jan 1, 1953

By Borje Hjortzberg-Nordlund

THE great Swedish export iron ore mines are Kiruna and Malmberget in the north above the Arctic circle and Grängesberg in Central Sweden, see Figs. 1 to 3. These mines exported in 1951 about 13 million metric tons of high grade iron ore and concentrates. The origin of these three ore fields seems to be the same. They are of pre-Cambrian age and are regarded as typical instances of primary eruptive ore that has thrust up as glowing masses of lava flow between two somewhat older beds of porphyry. Apparently the ore and the porphyry became segre. gated from common parent magmas by a process of differentiation. Despite the fact that the Kiruna orebody belongs to the earliest pre-Cambrian formation, it has been influenced to an unusually small extent by later metamorphosisms, apart from its having been set on edge through folding and wrenching off by a number of later faults. The Kiruna ore occurs along a stretch of more than 4 miles as a series of slabs or lenses sloping steeply toward the east and sandwiched between two beds of porphyry. The main orebody has a length of about 3 miles and an average width of 300 ft with a maximum of 600 ft. The dip varies from 65" to 45" toward the east and the known depth is 3000 ft, although magnetic surveys indicate it may be at least 6000 ft. Malmberget has undergone a more thorough transformation, having been pressed and crumpled into a meandering band of disconnected layers and lenses. The largest of the more connected bodies of ore, the Great Ore Layer, outcrops on a low mountain ridge and has a total length of about 4 miles and a maximum width of about 300 ft. The dip varies from 30" to 70" towards the north. The main orebody in Grangesberg, the so-called

Jan 1, 1953

By J. L. Moriarty, Irving Johnson, H. M. Feder

The crystallization of ternary alloys has been studied as a coprecipitation phenomenon by measuring the substitutional carrying of trace metals with CeCd11 precipitating from liquid cadmium. The Doerner-Hoskins logarithmic distribution law has been found to apply in all cases; the coprecipitation coefficients obtained were: 1.48 (La), 1.06 (Th), 0.63 (Pr), 0.24 (Gd), 0.17 (Sm), 0.13 (U), 0.10 (Er), 0.09 (Sr). Li, Na, K, Ba, Y, Sc, and Zr were not measurably carried. It has been observed that coprecipitation was most extensive for those tracers which form with cadmium an intermetallic compmdnd isostructural with CeCd11 or closely related thereto. For these tracers an inverse relation between Solubility in cadmium and coprecipitation coefficient was noted. THE partition of impurities between the liquid and solid phases of a metal or a congruently melting intermetallic compound has been extensively studied by the methods of zone melting.' However, when the composition of a liquid alloy and of the solid phase crystallizing from it differ grossly, partition of an impurity cannot be investigated in this manner. Partition of the impurity under equilibrium conditions may be studied by investigation of the appropriate phase diagram and partition under nonequi-librium conditions may be studied by observation of coring in the solidified alloys.2 The nonequilibrium case is of special interest in metallurgical practice because many complex alloys are cooled too rapidly to permit the uniform diffusion of impurities throughout the crystallizing phase(s). With this in mind, the present study was undertaken to obtain quantitative data on the phenomenon of coprecipitation via substitutional solid solution in certain metallic systems. It will be noticed that rather than adopting metallurgical ter- minology we have chosen to refer to the partition of impurities during alloy crystallization as coprecipitation.3 In the terminology of coprecipitation the impurity is referred to as the tracer and the precipitating phase as the carrier. From aqueous solution, coprecipitation may occur as a result of adsorption on the surface of the carrier, by occlusion of the liquid within the crystals, or by solid solution of the tracer in the carrier. By slow cooling of liquid metallic solutions it is relatively easy to form large, regular crystals of the carrier; the effects of adsorption and occlusion may be minimized and the influence of substitutional solid-solution formation may be made to predominate. Previous studies of the crystallization of some intermetallic compounds4 and of copper, silver, and gold5 have shown that the coprecipitation or partition behavior of trace metals is entirely analogous to that observed in aqueous systems when ionic substitution occurs, e.g., coprecipitation of Ra++ with BaSo4. The precipitation of CeCd11 from liquid cadmium was chosen for study. This choice was influenced by the following consideration. If the relative atomic sizes of the tracer atom and the atom for which it substitutes determine the tendency to coprecipi-tate, then a lattice having a substitutional site of well-defined size would be desirable. In CeCd116 (structure type cubic BaHg117) the cerium atom is completely surrounded by a cage of twelve nearly equidistant cadmium atoms. Thus, atoms much larger or much smaller than cerium should be poorly accommodated in this cage. The choice of a lanthanide central atom allowed the testing of the size hypothesis with a number of lanthanide tracers which differed in size but not in valence or electro-negativity. EXPERIMENTAL The general technique of this investigation was to prepare a slightly undersaturated solution of carrier in liquid cadmium to which a tracer was added. The concentration of tracer was always so low that saturation over the entire temperature range investigated was never exceeded. The solution was cooled in a stepwise fashion. After each step a por-

Jan 1, 1964

By M. S. Burton, B. W. Christ, G. V. Smith

Evidence of the effects which high-angle grain boundaries and veining subgrain boundaries have on the yield phenomenon of zone-refined iron is reported. Room-temperature tensile tests on 50-mil wive at several gram sizes produced upon recrystallization at diffevent temperatures below 910C (a-y phase-transfornzatzon temperature) show that upper and lower yield stress decrease with increasing grain size. The upper yield point effectively disappears at grain sizes of 81 and 102 u in samples of this diameter. However, samples of 129 p grain size. produced during recrys-tallization at 950°C, exhibit a pronounced upper yield point and an increased lower yield stress. Possible causes of the reversal in the grain-size dependence of yielding are discussed. Veining substructure, detected with picval-HC1 etchant, but not with 2 pct nital, is formed during the a-y transformation, and is believed to account for the observed effecls. The strengthening associated with high-angle boundaries in zone-refined tron is discussed in terms of: 1) the stress dependence of slzp multiplicity, and 2) the stress dependence of dislocation emission from grain boundaries. WIDE use of transmission electron microscopy and dislocation etch-pitting techniques has led to a growing awareness of the presence of dislocation substructures in annealed pure metals. Whereas much speculation'-4 has developed about the influence which subgrain structures have on the mechanical behavior of metals, particularly the yield strength, only limited experimental evidence correlating subgrain structures with lower yield strength has been presented. 2,3,5-7 It is the purpose of this note to present experimental evidence of the effects which grain boundaries and subgrain boundaries have on both the upper and lower yield strength of zone-refined iron. Effects due to high-angle boundaries formed upon recrystallization below the a-y phase transformation are compared with effects due to veining subgrain boundaries formed upon "recrystallization" above the a-y phase-transformation temperature. These effects are further compared with the reported influence 2,3,5-7 which low-angle boundaries have on the lower yield strength of bcc transition metals. EXPERIMENTAL PROCEDURE The starting material for these experiments was a 1-in.-diam zone-refined ingot prepared at Battelle Memorial Institute. Initial purification of electrolytic iron by vacuum-induction melting was improved by a floating zone-melting treatment in ultrapure hydrogen.' Chemical analysis of this zone-refined iron appears in Table I. Tensile samples of 50-mil wire were prepared by rolling and drawing portions of the ingot. An intermediate recrystallization anneal at 625°C after rolling to a reduction in area of 85 pct was carried out in an evacuated Vycor capsule (10-=5 mm Hg). Further reduction in area of 91 pct was followed by recrystallization in evacuated Vycor capsules at temperatures between 600" and 950°C, see Table 111. All samples

Jan 1, 1967

By Clinton M. Young

The experiments herein described were carried on in 1908-9 by- the State Geological Survey of Kansas. Some months before taking up work on black powder the Survey had resumed work on an interrupted investigation of explosions in coalmines, a subject which is engaging the attention of numerous investigators. An unusual number of serious disasters has directed to the subject a study which discloses the disquieting fact that, in the United States, the ratio of lives lost per ton of coal mined has been 011 the increase. Methods of coal-mining have changed to some extent with the great increase of output, attained in comparatively recent years. These changes involve the working of very extensive mines, with increased difficulty of ventilation, increased accumulation of coal-dust, and a very great increase in the amount of explosive used. This last point assumes truly startling proportions when it is carefully observed. In the fields of the Middle West it is not now uncommon for a miner to use six kegs (150 lb.) of black powder in a " pay" of two weeks, while within the memory of men still active, one keg (25 Ib.) would last two men for a " pay." So great has the use of explosives become in some fields that the skilled coal-miner is hard to find, and the coal is not mined, but blasted. A preliminary study of the subject of explosions in coalmines has led to the belief that the use of large quantities of explosives, in some cases by slightly-trained men, had riot been

Jan 1, 1911

By J. O. Lewis

The operation of gas-condensate fields is comparatively new and involves physical principles with which the industry was not prcviously familiar. It has been necessary to devise methods for testing gas-condensate wells and to correlate laboratory and field data. In this paper new methods are advanced for interpreting well G.P.M.† tests whereby dilution by dry gas can be estimated and information supplied on revaporization of condensates by dry gas. Inaccuracies in well test data are discussed. Changes in flow rates can cause changes in the G.P.M. of the effluent and it may take some time for a well to become stabilized after an important change in flow rate. Retrograde tests as usually conducted cannot be directly compared with field G.P.M. data, because the retrograde tests usually include solution gas in the condensates, which are reported On the cumulative basis whereas field data (G.P.M.) usually report pentaneS PlUS on a rate or instantaneous basis. Introduction Though long known to physicists, the phenomena Of retrograde condensation became known to the oil and gas industry Only in recent years, when deeper drilling disclosed that the behavior of vapors under changing pressures was different in high-pressure reservoirs than under the low-pressure operations with which the industry was familiar. These deep, high-pressure reservoirs in which condensation and vaporization behaved inversely to the accustomed manner became known as "gas-distillate," or preferably "gas-condensate" fields. Partly to prevent precipitation and retention of liquids in the reservoir, but still more to prevent the waste of residue gas, the operation known as "recycling," or preferably "cycling," was instituted, in which the residue gas is reinjected into the reservoir, thus maintaining pressure and driving the wet gas to the producing wells. For lack of field experience to serve as a guide, the industry had to assume that theory and laboratory experiments could accurately forecast retrograde behaviors in operating these gas-condensate fields, but it is obvious that these assumptions should be checked at the first opportunities against actual field experience. To make such checks, it is necessary to accumulate a large quantity of reliable field data, but experience has shown that it is difficult to obtain reliable field data and that the laboratory data as usually presented are not in directly comparable form. The problems of correlation involve the complex phase behavior on the one hand, and a knowledge of field data and a visualization of underground conditions on the other hand. This paper is an approach from field experience, The purposes of this article are to discuss the sources of uncertainty in the data and to present methods of analyzing, interpreting and correlating laboratory and field data. Data mostly from lower Gulf Coast fields are presented, from which some conclusions can be derived, but better data from more sources than those available to the writer will be required before satisfactory answers to many questions can be obtained. This paper is presented to stimulate the analysis and publication of data from other fields, the reexamination of field and laboratory methods, and the taking of more complete and reliable field tests. For these purposes, the writer presents some speculations that otherwise would not be appropriate.

Jan 1, 1947

By J. O. Lewis

The operation of gas-condensate fields is comparatively new and involves physical principles with which the industry was not prcviously familiar. It has been necessary to devise methods for testing gas-condensate wells and to correlate laboratory and field data. In this paper new methods are advanced for interpreting well G.P.M.† tests whereby dilution by dry gas can be estimated and information supplied on revaporization of condensates by dry gas. Inaccuracies in well test data are discussed. Changes in flow rates can cause changes in the G.P.M. of the effluent and it may take some time for a well to become stabilized after an important change in flow rate. Retrograde tests as usually conducted cannot be directly compared with field G.P.M. data, because the retrograde tests usually include solution gas in the condensates, which are reported On the cumulative basis whereas field data (G.P.M.) usually report pentaneS PlUS on a rate or instantaneous basis. Introduction Though long known to physicists, the phenomena Of retrograde condensation became known to the oil and gas industry Only in recent years, when deeper drilling disclosed that the behavior of vapors under changing pressures was different in high-pressure reservoirs than under the low-pressure operations with which the industry was familiar. These deep, high-pressure reservoirs in which condensation and vaporization behaved inversely to the accustomed manner became known as "gas-distillate," or preferably "gas-condensate" fields. Partly to prevent precipitation and retention of liquids in the reservoir, but still more to prevent the waste of residue gas, the operation known as "recycling," or preferably "cycling," was instituted, in which the residue gas is reinjected into the reservoir, thus maintaining pressure and driving the wet gas to the producing wells. For lack of field experience to serve as a guide, the industry had to assume that theory and laboratory experiments could accurately forecast retrograde behaviors in operating these gas-condensate fields, but it is obvious that these assumptions should be checked at the first opportunities against actual field experience. To make such checks, it is necessary to accumulate a large quantity of reliable field data, but experience has shown that it is difficult to obtain reliable field data and that the laboratory data as usually presented are not in directly comparable form. The problems of correlation involve the complex phase behavior on the one hand, and a knowledge of field data and a visualization of underground conditions on the other hand. This paper is an approach from field experience, The purposes of this article are to discuss the sources of uncertainty in the data and to present methods of analyzing, interpreting and correlating laboratory and field data. Data mostly from lower Gulf Coast fields are presented, from which some conclusions can be derived, but better data from more sources than those available to the writer will be required before satisfactory answers to many questions can be obtained. This paper is presented to stimulate the analysis and publication of data from other fields, the reexamination of field and laboratory methods, and the taking of more complete and reliable field tests. For these purposes, the writer presents some speculations that otherwise would not be appropriate.

Jan 1, 1947

By P. R. Swann, J. G. Parr

Quenched structures were studied in alloys containing up to 12.5 pct cobalt. The subsequent decomposition of a 10 pct cobalt retained-ß phase alloy was investigated using metallographic and X-ray diffraction methods. Hardness measurements also were made during the decomposition process. Precipitation of Ti2Co is by nucleation and growth; and an activation energy of 50,000 cal per mole was determined. The values of the coefficient ß suggest that the precipitate is pearlitic at temperatures between 450 and 475°C, and spheroidal between 500 and 525°C. THIS paper describes part of a series of invesligations into phase transformations in binary alloys of titanium with transition elements. The general approach is similar to that taken in work on titanium-iron and titanium-nickel alloys.' Previous investigators'' have established the titanium-rich end of the titanium-cobalt phase diagram, reproduced in Fig. 1. Orrell and Fontana' showed that alloys containing more than about 6 pct" cobalt quenched from the ß range, produced 100 pcl retained-p phase. The isothermal decomposition of alloys containing between 0.8 pct Co and 15.5 pct CO was investigated by the same workers in the temperature range 650 to 1000°C. They reported that these alloys transformed into a or Ti,Co depending on the cobalt content, but no quantitative data were given. In the work to be described a series of alloys containing 0.8 pct Co to 12.5 pct Co was examined in the quenched condition. The 10 pct Co alloy (the lowest cobalt content to retain 100 pct ß on quenching) was selected for further work on the tempering kinetics of the ß decomposition. Experimental Procedure Since our own melting equipment was not installed at the outset of this work, the Physical Metallurgy Division of the Department of Mines and Technical Surveys (Ottawa, Canada) prepared the alloys. These were made of Japanese sponge, (which when melted had a value of 103 DPH, using a 1-kg load), and electrolytically prepared cobalt. The al- loys, made up to contain 0.8, 1.6, 3.3, 5.8, 8.3, 10.0 and 12.5 pct Co, were homogenized by swaging into rods at 900°C. Filings were taken from the rods, and any iron chips from the file were separated magnetically. Size fractions of both plus and minus 200 mesh (about 75p) were shown by their constitution, after annealing just below the eutectoid temperature, to contain the same cobalt content. Consequently, it was permissible to use the —200-mesh fraction, knowing it to be representative of the rod composition. Quenching in argon was carried out in a newly designed furnace, whose features include (1) an Inconel furnace tube, (2) a positive pressure of argon maintained at all times in the furnace—even when a sample is removed or inserted. The furnace is shown in Fig. 2 and is described in the Appendix. The tempering processes were carried out on powder samples sealed in evacuated quartz capsules. Since the highest tempering temperature was 525OC, no protection against reaction with the quartz was necessary. (Tests were made on filings of iodide titanium and showed no hardness increase after equivalent heat-treatments.) A thermocouple was attached to the capsule, which was heated to the

Jan 1, 1959

By G. A. Swanquist, E. M. Morales

INTRODUCTION The idea of water management and control at the Church Rock Mill operations began to take shape in February 1979. At that time, we were already investigating the feasibility of decreasing the fresh water requirements so that the solids would become the limiting factor in tailings impoundment utilization. The area for solution evaporation could be kept at a fraction of the normal requirements under the standard process of full water usage. The Church Rock Mill is an acid leach circuit followed by solids/liquid separation with thickeners in counter current decantation, and solvent extraction. Following the normal design of acid leach circuits, reuse of tailings solution was not incorporated in the original mill process design. INITIAL WATER CONTROL INVESTIGATIONS The investigations to decrease the fresh water requirements centered around modifying the grinding circuit from the present semi-autogenous grinding (SAG) mill in closed circuit with hydrocyclones, to open circuit grinding with a rod mill. The open circuit grinding with the SAG mill and rod mill in series had the potential of decreasing the water requirements for grinding and leach dilution by approximately 50% or 1.4 m3/min (300 gpm). The grinding pulp density would be maintained at 70 to 72% solids, and the leach dilution to 50% solids would be accomplished with acid tailings liquor recycle. In such a grinding circuit arrangement, the SAG mill would provide the primary or coarse grind, and the rod mill would be used for the fine grind. By the SAG mill and rod mill series grinding method of water control and other secondary water controls in various places downstream from the grinding circuit, the required necessary evaporation area was estimated at 120 acres of liquid surface. A second method of water control at grinding was investigated. A two-stage cyclone classification circuit appeared to have a good potential of achieving the same water reduction at a much lower capital and operating cost. However, in retrospect, this would not have been a viable method since a high slime recycle load would have been established hindering classification. The use of reagents to neutralize the acid tailings solution was not considered seriously at that time, since it would have materially increased operating costs, although it would have also allowed more tailings solution recycle and consequently, less fresh water usage. However, with the tailings solution deposition area available at that time, it was not then necessary to incur the high cost of neutralization. The control expected by the series grinding of semiautogenous and rod mills would have been sufficient to maintain a water consumption/evaporation equilibrium well in line with the available land area. IMPLEMENTATION OF NEUTRALIZATION OPERATIONS During the summer of 1979, the UNC Church Rock Mill experienced a tailings dam breach which resulted in a prolonged mill shutdown. Upon resumption of operations at the end of October 1979, tailings deposition was restricted to a small portion of the tailings impoundment area. Figure 1 shows the general tailings area and the limits of the present deposition area in the central part including the borrow pits. These borrow pits had been excavated to provide materials for tailings dam construction. Immediately after resumption of operations, it became evident that it would be necessary to control the quantity of liquid to be evaporated because of the small confined area available for tailings solution deposition and to maximize the deposition time in the tailings area. The water control required had to be exercised on a large scale, and to be in operation as quickly as possible. An obvious solution was to reuse the tailings liquor in mill process. Immediate steps were taken to install the necessary equipment for tailings neutralization on an interim basis. Anhydrous ammonia was selected as the primary neutralization reagent since it was the quickest system that could be placed in operation. Previous laboratory tests indicated fair results with ammonia neutralization. Such a system required a minimum of installed equipment and handling. INITIAL NEUTRALIZATION OPERATIONS Actual neutralization operations began on November 26, 1979. The raffinate solution which normally would have been discarded was pumped to a 3.7 m (12ft) diam by 4.3 m (14ft) tank for reagent contact, see Figure 2. At this tank, anhydrous ammonia was added directly from the tanker trailers and controlled at pH 7.0 nominally. Agitation was provided by air sparging. The neutralized product formed a highly viscous slurry in the grinding circuit which resulted in pumping and cyclone classification problems.

Jan 1, 1982

By Takahide Wakamatsu, Shigeru Mukai

Fundamental investigations were made on the treatment of slime and the chrysocolla flotation, both of which are urgent problems to be solved in copper oxide mineral flotation. Unfavourable effects of slime on flotation are caused by the slime adsorption at the air/liquid Interface as well as the slime coating on the mineral surface. The adsorption of slime at the air/liquid interface was measured by using various kinds of slime particles. As a consequence, goethite, bentonite and talc tended to adsorb markedly at the interface. As a desliming method, slime flotation with a polymer flocculant such as polyethylene-oxide prior to the ordinary copper oxide flotation was found to be effective. The use of both a copper-avid organic reagent and an alkyl xanthate was examined for a selective collection of chrysocolla through xanthate adsorption tests, chrysocolla float- abllity tests and flotation tests for synthetic and natural ore. The copper-avid reagents used were salicylaldoxime, 8- hydroxyquinollne and benzoin-a-oxime. As a result, the ad- sorption of higher xanthate such as amyl xanthate on chrysocolla as well as the chrysocolla-to-air bubble attachment was increased by the presence of a copper-avid reagent under suitable reagent addition and pH of pulp. Flotation tests for synthetic and natural ores confirmed that chrysocolla could be floated sufficiently and selectively with a copper- avid reagent like 8-hydroxyquinoline or salicylaldoxime with its subsequent collection by amyl xanthate.

Jan 1, 1976

By H. F. A. Hergt, K. L. Sutherland, J. Rogers

In 1938 Ralston4 reviewed the many attempts to find a satisfactory collector for the separation of cassiterite from its ores and in 1944 Dean and Ambrose2 summarized some further attempts. Generally, soaps and amines are effective but nonselective collectors. We have discovered that reagents containing either the polar group — SO4- or — SO3- are excellent collectors for cassiterite and promise to be selective. The response to these reagents of cassiterite and of minerals commonly associated with it was studied, using the captive-bubble technique. Using these fundamental data, the practicability of separation and concentration of tin was investigated by flotation tests in a 2000-gram Denver cell. Experimental Methods Reagents All inorganic reagents were of Analar grade. The preparation and purification of sodium cetyl sulphate, cetyl trimethyl-ammonium bromide, laurylamine and cetylamine have been previously described.5 The other collectors were commercial surface-active agents, which were used without purification. Tests Captive-bubble Tests and Cylinder Flotation Tests have been previously de- scribed.5,10 The full lines shown in the figures relating solution composition to contact (flotation) distinguish solutions in which contact (flotation) is possible from those in which it is not. The curve is derived by successive approximation and the accuracy is ±0.2 pH units and ± 5 mg. per liter of collector or depressant. Solution compositions for which it was shown experimentally that contact or flotation is possible are marked by a circle, those for which it is not possible, by a cross, and those for which it is doubtful by a cross within a circle. It is assumed that at all other solution compositions within (without) the curve, contact or flotation is possible (not possible). After testing in the collector solution, the mineral was removed, washed, and tested by the captive-bubble method in water, or floated in a cylinder with frother only. In this way the composition of solutions in which a mineral was conditioned but in which properties of the collector solution prevented contact or flotation can be defined. The composition of solutions in which conditioning was possible lie between the full and broken curve, and the experimental results are indicated by a square. The curves show the limits of composition of solutions in which flotation in a cell would be possible but many factors other than those considered in these the determine recovery and grade of a given mineral in practice. Flotation Tests in 500 and 2000-gram Denver SUbmachines,—Melboume tap water, containing 12 parts calcium, 6 parts

Jan 1, 1947

By J. Rogers, H. F. A. Hergt, K. L. Sutherland

In 1938 Ralston4 reviewed the many attempts to find a satisfactory collector for the separation of cassiterite from its ores and in 1944 Dean and Ambrose2 summarized some further attempts. Generally, soaps and amines are effective but nonselective collectors. We have discovered that reagents containing either the polar group — SO4- or — SO3- are excellent collectors for cassiterite and promise to be selective. The response to these reagents of cassiterite and of minerals commonly associated with it was studied, using the captive-bubble technique. Using these fundamental data, the practicability of separation and concentration of tin was investigated by flotation tests in a 2000-gram Denver cell. Experimental Methods Reagents All inorganic reagents were of Analar grade. The preparation and purification of sodium cetyl sulphate, cetyl trimethyl-ammonium bromide, laurylamine and cetylamine have been previously described.5 The other collectors were commercial surface-active agents, which were used without purification. Tests Captive-bubble Tests and Cylinder Flotation Tests have been previously de- scribed.5,10 The full lines shown in the figures relating solution composition to contact (flotation) distinguish solutions in which contact (flotation) is possible from those in which it is not. The curve is derived by successive approximation and the accuracy is ±0.2 pH units and ± 5 mg. per liter of collector or depressant. Solution compositions for which it was shown experimentally that contact or flotation is possible are marked by a circle, those for which it is not possible, by a cross, and those for which it is doubtful by a cross within a circle. It is assumed that at all other solution compositions within (without) the curve, contact or flotation is possible (not possible). After testing in the collector solution, the mineral was removed, washed, and tested by the captive-bubble method in water, or floated in a cylinder with frother only. In this way the composition of solutions in which a mineral was conditioned but in which properties of the collector solution prevented contact or flotation can be defined. The composition of solutions in which conditioning was possible lie between the full and broken curve, and the experimental results are indicated by a square. The curves show the limits of composition of solutions in which flotation in a cell would be possible but many factors other than those considered in these the determine recovery and grade of a given mineral in practice. Flotation Tests in 500 and 2000-gram Denver SUbmachines,—Melboume tap water, containing 12 parts calcium, 6 parts

Jan 1, 1947

By J. Rogers, H. F. A. Hergt, K. L. Sutherland

IN 1938 Ralston4 reviewed the many attempts to find a satisfactory collector for the separation of cassiterite from its ores and in 1944 Dean and Ambrose2 summarized some further attempts. Generally, soaps and amines are effective but nonselective collectors. We have discovered that reagents containing either the polar group -SO4- or _S03- are excellent collectors for cassiterite and promise to be selective.1 The response to these reagents of cassiterite and of minerals commonly associated with it was studied, using the captive-bubble technique. Using these fundamental data, the practicability of separation and concentration of tin was investigated by flotation tests in a 2000gram Denver cell. EXPERIMENTAL METHODS Reagents All inorganic reagents were of Analar grade. The preparation and purification of sodium cetyl sulphate, cetyl trimethyl-ammonium bromide, laurylamine and cetylamine have been previously described.5 The other collectors were commercial surface-active agents, which were used without purification. Tests Captive-bubble Tests and Cylinder Flotation Tests have been previously described.5-10 The full lines shown in the figures relating solution composition to contact (flotation) distinguish solutions in which contact (flotation) is possible from those in which it is not. The curve is derived by successive approximation and the accuracy is ±0.2 pH units and ± 5 mg. per liter of collector or depressant. Solution compositions for which it was shown experimentally that contact or flotation is possible are marked by a circle, those for which it is not possible, by a cross, and those for which it is doubtful by a cross within a circle. It is assumed that at all other solution compositions within (without) the curve, contact or flotation is possible (not possible). After testing in the collector solution, the mineral was removed, washed, and tested by the captive-bubble method in water, or floated in a cylinder with frother only. In this way the composition of solutions in which a mineral was conditioned but in which properties of the collector solution prevented contact or flotation can be defined. The composition of solutions in which conditioning was possible lie between the full and broken curve, and the experimental results are indicated by a square. The curves show the limits of composition of solutions in which flotation in a cell would be possible but many factors other than those considered in these tests determine recovery and grade of a given mineral in practice. Flotation Tests in 500 and 2000-gram Denver Submachines.--Melbourne tap water, containing 12 parts calcium, 6 parts

Jan 1, 1947

By A. G. Buyers, J. Chilton, W. E. McKee

STUDIES in the high-temperature separations chemistry of thorium-uranium fuels are complicated by the corrosive nature of these molten metal systems at 1700°C. Separations research pointed toward the removal of fission products from irradiated alloys has included a frozen salt-bed technique which minimizes container reaction with molten metal. The procedure consists of high-frequency induction melting of the metal sample which is supported by a vertical column of unmelted salt. The molten alloy melts its immediate salt environment and as it slowly falls down through the column, many of the fission-product poisons are transferred into the fused salt environment. The molten salt-metal zone is encompassed at all times by unmelted salt, preventing container contact. EXPERIMENTAL Experimental methods were separated into three parts: salt-bed preparation, melting, and analytical evaluation. A) Bed Preparation—The procedure for casting calcium-fluoride briquettes was to compress the powdered salt at 5,000 to 10,000 psi and place this compact in a graphite crucible. This assembly was inserted into a vacuum system and surrounded by an alumina crucible as well as molybdenum, tantalum, or stainless-steel foil thermal-radiation shields. The pressure was reduced and the crucible heated under vacuum to about 800°C with the fore pump operating. Argon was then admitted to about 0.8 atm and heating continued until the CaF2 had melted 5 min at the melting point seemed satisfactory). Apparatus used included a 1-in. graphite crucible with 1/8-in. walls, 1-in. ID in a 2-in. induction coil, and a 6-kw Ajax high-frequency converter. B) Melting—Calcium-fluoride briquettes, 1 in. in diam and 1/2 to 1 in. thick, were prepared and vertically stacked to obtain the desired column length. An irradiated alloy sample (nut = 10") was placed on top of the salt column and the assembly was connected to the vacuum system. After evacuation of 5 to 10 , purified argon was admitted and the system flushed twice. The final argon pressure was about 0.8 atm. The sample was heated by induction at a power of about 6.5 kw. It then melted its way down through the salt and freely dropped into a small alumina crucible. The molten metal is followed during its downward course by the induction coil which is mounted upon a power-driven machine-threaded shaft. Experimental conditions used in the foregoing work

Jan 1, 1960

By H. L. Luo, W. Klement

By rapidly quenching Ag-Pt alloys from the melt, a continuous series of solid solutions has been obtained. At equilibrium''2 these fcc elements form a peritectic system, Fig. 1. Weighed amounts of silver and platinum powder (325 mesh, purity greater than 99.9 pct) were mixed for 24 to 120 hr, pressed into compacts, sintered at 1000°C in a hydrogen atmosphere for at least 16 hr, and then furnace-cooled. Because of the difficulty in achieving homogeneity in alloys containing more than about 40 at. pct Pt, the sintered compacts were induction-melted under hydrogen in alumina crucibles and then cold-rolled into wires. Small amounts ("30 mg) of alloys cut from various sections of the sintered compacts or rolled wires were heated to at least 50' ~ above the liquidus in an alumina insert held within an induction-heated graphite crucible; then the molten alloy was ejected by a blast of helium onto a lightly polished copper strip held on the inner periphery of a rotating wheel. The flakes thus obtained were typically 1 sq mm in area or often slightly larger for the silver-rich alloys. X-ray diffraction patterns were obtained with nickel-filtered copper K radiation in a 114.6-mm-diam Debye-Scherrer camera with rotated specimens. Lattice parameters and associated uncertainties were estimated from extrapolations against the Nelson-Riley function. High-angle lines were always resolved and spacings were computed relative to r(CuKa!,) = 1.540508 The details of these techniques have been discussed previously.s'6 Lattice parameters of the solid solutions are plotted in Fig. 2, together with the data of Schneider and Esch,' Johansson and Linde,' and Novikova and pudnitskii. Each of the present lattice spacings represents two or more independent determinations. The alloys were homogeneous within 2 at. pct of nominal composition as estimated from the uncertainties in the lattice spacings. Many of the mechanisms involved in the achievement of metastable solid solutions by rapidly quenching from the melt have been previously discussed. There is some evidence" that such solid solubility cannot be obtained when the liquid alloys are cooled

Jan 1, 1963