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By K. A. Johnson, H. F. Yancey

Physical properties have been used for a long time in characterizing different kinds of coal, and such physical properties as friability and slacking have been included along with chemical properties in grouping coals according to the widely used system of classification adopted by the U. S. Geological Survey. Nevertheless, the usefulness of physical properties for classifying the different ranks or kinds of coal has been limited because it has not been possible to express these properties in definite form as numerical values. Because of the present wide interest in the formulation and adoption of a satisfactory system of coal classification, the Northwest Experiment Station of the U. S. Bureau of Mines, in cooperation with the College of Mines of the University of Washington, has recently completed a study of the physical and chemical properties of approximately 100 different coals ranging in rank from lignite to anthracite. Purpose and Scope For this investigation samples were collected in approximately 45 mines and prospects in Washington and 23 mines in other states. The following studies, in addition to proximate and ultimate analyses, were made of the samples: Determination of (1) friability, (2) slacking or weathering characteristics, (3) yield of products by low-temperature carbonization in a laboratory retort, and (4) agglutinating value. Most of the coals examined were subjected to each of the tests enumerated, but with coal of some ranks this was unnecessary in some instances, and in others it was not feasible to do the work involved. A report which includes the analyses of the coals and the details of the methods of examination used in the investigation is being published by the Bureau of Mines.' It is the purpose of the present report to show the results of the friability, slacking, low-temperature and agglu-

Jan 1, 1932

By W. A. Wood, H. L. Wain, R. I. Garrod

The mechanical behavior of recrystallized chromil~m of high purity has been studied, principally in torsion and to a lesser extent in tension, at temperatures between —196oand 350oC. Depending upon the conditions of test, the material may show brittle or ductile behavior or an intermediate or subduc-tile state having some of the characteristics of each. This latter state existed at temperatures between approximately ±50°C and was characterized by a) extensive creep at stresses well below the normal fracture stress, b) nonelastic loading/unloading effects during creep, c) strain softening under cyclic loading, and d) final failure of a brittle type. Suggestions are made on the dislocation processes and interactions which give rise to subductile behavior The ductile-brittle transition in bee metals has been studied mainly by tension and bend tests. These methods, however, favor crack propagation which may follow too closely on initiation for detailed study of the transition itself. For work of this nature, therefore, other modes of deformation less favorable to crack propagation may be preferable. This paper describes a study of the ductile-brittle transition in chromium which is based mainly on torsional testing although a few subsidiary experiments were made in tension. It appears to reveal at the transition an intermediate state that cannot properly be described as either brittle or ductile. Torsional tests on chromium have been made by other workers1 but not, as here, primarily for study of this intermediate state. EXPERIMENTAL The chromium, in the form of swaged rod, was prepared by techniques already described.' The particular material used was one in which the main impurities were 0.03 wt pet 0 and 0.006 wt pet N and one in which transition from ductile to brittle states in torsion conveniently fell at about room temperature. For torsion, test specimens were from 5/16-in.-diam rod to provide test portions 1-1/4 in. long by 7/32 in. diam, a twist of 1 deg thereby corresponding throughout this paper to 0.0015 surface shear. The specimens before test were annealed for 2 hr at 1200°C in vacuo, which left them with a re-crystallized grain size of about 0.01 mm, and then electropolished. They were tested under dead-weight loading in an apparatus in which they could be surrounded by a furnace or cooling chamber, tests in practice being made at various temperatures between -196" and +350°C. For tension tests, cylindrical specimens were prepared in a similar manner and tested at room temperature under dead-weight loading. RESULTS (TORSION) Subductile State. The state described above as intermediate between brittle and ductile may be perhaps best defined by reference to torque/twist curves at various temperatures. These are grouped in Fig. 1. Below about -50°C the material was brittle, in the sense that it exhibited little plastic deformation under stress and fractured by cleavage along planes of maximum resolved tension, which in torsion produces the well-known helical type of fracture. The deformation is typified by the curves for -196" and -150°C in Fig. 1; it shows a slight but progressive deviation from linearity above a certain torque, here about 50 lb-in., until fracture occurs at about 95 lb-in. A feature to which it is desired specially to call attention is that under none of the loads did the specimens show significant creep.

Jan 1, 1964

By H. S. Wang, Y. P. Gupta

Diffusion of zinc and germanium in liquid silver is measured in the temperature range 975" to 1400°C by use of the capillary-reservoir technique. The ex-perinzental results are discussed in terms of the fluctuation and the "hole" theories of liquid diffusion, assunzing the solute as a point charge equal to the difference in the valences of the solute and solvent atoms. The additional coulombic interaction term due to the excess solute charge is evaluated in terms of the Thomas-Fenni approximation. The theoretical and experimental results agree with both the fluctuation and "hole" theories of liquid diffusion. No perceptible effect on solute diffusion in liquid silver of the size difference between the solute and solvent atoms/ions is apparent. DIFFUSION in liquid silver of electropositive solutes indium, tin, antimony, and homovalent gold has been previously reported by Leak and Swalin1 and Gupta,' respectively. These solutes have nearly the same atomic size but differ principally from one another in excess valence (+2, +3, +4, respectively). The observed differences in the temperature dependence and the rate of solute diffusion were explained in terms of an added coulombic interaction between the solute and the solvent atoms. In the case of diffusion of gold in liquid silver, the data were found to be consistent with an effective valence for gold of -0.85, as proposed by Le Claire.3 Recently, Wang and Gupta4 have reported a study of diffusion of ruthenium, iron, and cobalt in liquid silver. The results of diffusion of these solutes and their temperature dependence were found consistent with the hole theories and the fluctuation theories of liquid diffusion, if ruthenium, iron, and cobalt were diffusing in liquid silver with relative valences -2, -1.3, and -0.5, respectively, instead of -3, -3, and -2 as suggested by the relative position of these elements in the Periodic Table of Elements. Furthermore, the predicted valences for these solutes were observed to be consistent with the sparsely available information on the magnetic properties of some of the dilute alloys of copper and silver with these solutes. In theoretical calculations of solute diffusivity, the solute was assumed as a point excess charge equal to the difference in the valences of the solute and solvent atoms. Both the assumption of a point excess solute charge and the use of the Thomas-Fermi approximation to calculate the potential of a solute charge are less precise for the case of electronegative solutes. Therefore, it was not possible to infer from the data on ruthenium, iron, and cobalt an effect, if any, on solute diffusion of the relative differences in either the Period or the size of the solute and solvent atoms or the solute atoms themselves. A study of the diffusion of Period 4 elements, specifically zinc and germanium was, therefore, undertaken since zinc and germanium, respectively, have relative valences of +1 and +3 in liquid silver and the data obtained on diffusion of these solutes could be compared with the available data on diffusion of Period 5 electropositive solutes, indium, tin, and antimony in liquid silver. From such a comparison, it was hoped to learn something about the effect, if any, of the ion size or the structure of the ion core on impurity diffusion in liquid silver. EXPERIMENT The diffusion of tracer zinc and germanium in liquid silver was studied by the capillary reservoir technique, modified adequately for use at high temperatures. In principle, capillaries containing liquid silver

Jan 1, 1970

By Kun Li, Alex Simkovich

The rate of dissolution of alumina in carbon-saturated liquid iron has been studied experimentally in a system where alumina was in the form of a cylindrical rod immersed in an iron bath contained in a graphite crucible. Data obtained consisted of the concentrations of aluminum in the melt as a function of time. In the case of static experiments, the data are shown to agree with theoretical prdictions based on the diffusion of aluminum.. The rate of dissolution was greatly increased by the rotation of the alumina rod. It is concluded that the diffusion of aluminum from the alumina/metal interface is the rate-controlling step. In the past, thermodynamic investigations of systems encountered in ferrous process metallurgy have received widespread attention. More recently, considerable work has been devoted to the study of kinetics associated with these systems in an effort to determine their rate controlling mechanisms. The alumina-iron system is of great importance in ferrous metallurgy. Yet information concerning kinetics of reaction in this system is seriously limited. The present study was made in order to establish the rate-controlling step for dissolution of solid alumina in liquid iron. LITERATURE REVIEW A number of papers concerning dissolution of solid metals in liquid metals have been reported in the literat~re. Generally, for these simple systems, dissolution is controlled by mass transfer of the dissolving species. Complex systems involving dissolution of solid metal carbides and oxides in liquid metals and slags have been studied to a much lesser extent. Skolnick5,6 reported on the reaction between liquid cobalt and poly-crystalline cylinders of tungsten carbide, in which the cylinders were dissolved while being rotated about their longitudinal axes at various speeds and temperatures. As a result of unexpected preferential grain boundary attack by the liquid cobalt, large errors in the measured dissolution rates occurred because of loss of tungsten carbide grains to the liquid cobalt. Nevertheless, it was possible to establish that the liquid Co-W carbide reaction was not controlled by mass transfer. In a similar approach, cooper7 was able to show that artificial sapphire rods, (alumina single crystals) dissolving in lime-alumina-silica slags obeyed a mechanism of mass transfer control. Here, again, the rods were rotated at various speeds and temperatures, and the process was followed as a function of these variables. Forster and Knacke8 took a practical approach to reaction between slags and refractories. By blowing argon through refractory cylinders of silica, silli-manite, or dolomite and directing the gas to rise along the slag-refractory interface, it was possible to increase the rate of mass transfer. Although the method was admittedly crude, it nevertheless permitted an evaluation of the relative stabilities of refractories with respect to slag attack. Data were interpreted on the basis of mass transfer control. EXPERIMENTAL TECHNIQUE Apparatus. An illustration of the apparatus used in this study is shown in Fig. 1. The furnace consisted of a Morganite recrystallized alumina tube wound with a molybdenum coil. A secondary molybdenum heater was mounted around the upper half of the primary coil to aid in controlling the thermal gradient within the furnace. The primary heater tube was 3 in. in ID and 30 in. long. A reducing mixture of 95 pct N and 5 pct H was maintained around the heating elements. Thermal insulation was provided by alumina powder. The chamber within the primary combustion tube contained a boron nitride block near the top to assist in controlling the thermal gradient to the furnace and also to provide a bearing surface for the rotating graphite shaft. The outside diameter of the graphite shaft was $ in. A separate threaded graphite specimen holder was screwed into the end of the shaft. The holder contained a tapered hole drilled into the end to guide the oxide specimens as they were pressed into it for mounting. Additional guidance for the rotating graphite shaft was furnished by a water-cooled bronze bushing attached to the top of the furnace. A steel clamp was fastened to the upper end of the graphite shaft and rested on a thrust bearing; the shaft and clamp were driven by a dc motor through a set of gears. Two O-rings located immediately above the bronze bushing maintained a gas-tight seal about the graphite shaft. The lower half of the alumina tube housed the crucible and charge, which were placed on a 3/4-in. diam movable alumina support tube. With this arrangement, charges could be inserted into or removed from the furnace while the hot zone was maintained at or above 1000°C. To control the temperature of the furnace, the thermocouple was mounted inside the support tube and in contact with the crucible bottom. Stray electric fields in the furnace were of sufficient intensity to cause erratic indications by the thermocouple. By enclosing the thermocouple protection tube in a molybdenum sheath and grounding this shield, the problem was eliminated. Output of the thermocouple went to an automatic continuous balance controller. Procedure. A typical run was as follows. First, electrolytic iron was premelted in graphite crucibles and cast into graphite molds with the same configura-

Jan 1, 1970

By Ralph A. Sherman, John Blizard

The experimental investigation described in this paper was conducted to determine the relative combustibilities of different samples of blastfurnace coke when burned in a current of air in a small furnace. It was undertaken in connection with the work done by Perrottl and Kinney2 on the process of combustion in the blast-furnace hearth.3 Reference is often made to the "combustibility" of coke by blastfurnace men, but exactly what is meant by the term "combustibility" is somewhat vague. Brassert,4 in a paper before a meeting of blastfurnace men in 1914, refers to combustibility as follows: The value of the coke in relation to the heat reactions in the furnace is determined not only by the carbon content but even more so by its combustibility. This, in turn, is governed by its size, the physical and chemical composition of the carbonaceous substance forming the cell walls, and the interior and surface structure of the coke pieces. These properties are, in turn, influenced by the chemical and physical properties of the coals used for coking, the density of the cake of coal in the oven, the coking time, temperature and heat regulation of the ovens, and last, but not least, by the method of quenching, screening and handling the finished coke. What principally concerns the blast furnace is the rate of progression of the combustion, which depends not so much on the chemical analysis as on the physical qualities of the coke. It is this rate of progression that we term combustibility, which is the speed at which the carbon molecules in the coke combine with oxygen under given conditions. In general, what the blast furnace requires is a coke which will burn rapidly and with intensity at the tuyeres, yet which has a sufficiently strong structure and hard surface to resist abrasion and solution by CO2 in the upper part of the stack.

Jan 1, 1923

By John Blizard, Ralph A. Sherman

The experimental investigation described in this paper was conducted to determine the relative combustibilities of different samples of blastfurnace coke when burned in a current of air in a small furnace. It was undertaken in connection with the work done by Perrottl and Kinney2 on the process of combustion in the blast-furnace hearth.3 Reference is often made to the "combustibility" of coke by blastfurnace men, but exactly what is meant by the term "combustibility" is somewhat vague. Brassert,4 in a paper before a meeting of blastfurnace men in 1914, refers to combustibility as follows: The value of the coke in relation to the heat reactions in the furnace is determined not only by the carbon content but even more so by its combustibility. This, in turn, is governed by its size, the physical and chemical composition of the carbonaceous substance forming the cell walls, and the interior and surface structure of the coke pieces. These properties are, in turn, influenced by the chemical and physical properties of the coals used for coking, the density of the cake of coal in the oven, the coking time, temperature and heat regulation of the ovens, and last, but not least, by the method of quenching, screening and handling the finished coke. What principally concerns the blast furnace is the rate of progression of the combustion, which depends not so much on the chemical analysis as on the physical qualities of the coke. It is this rate of progression that we term combustibility, which is the speed at which the carbon molecules in the coke combine with oxygen under given conditions. In general, what the blast furnace requires is a coke which will burn rapidly and with intensity at the tuyeres, yet which has a sufficiently strong structure and hard surface to resist abrasion and solution by CO2 in the upper part of the stack.

Jan 1, 1923

By Harrison R. Cooper

Computer process analysis and control techniques are overcoming major hurdles to acceptance in the mineral industry. With the growing list of new advances characteristic of a rapidly maturing discipline, management of the companies on the leading edge are keenly aware of the advantages of using computer methods in process applications. Significant advancement is already evident in such technical areas as operations research, mathematical modeling, statistical methods, and computer-based procedural techniques. The early advances during the past decade are already documented in prior symposium proceedings of this series. Thus, the currently active areas of the advancing technology are emphasized here. This section deals with applications in pyrometallurgical and kiln processes. The two sections which follow deal with concentrating operations from two points of view: 1) mathematical modeling, and 2) on-line control. In the metallurgical field, emphasis on developing effective process computer applications for the steel industry began in the late 1950's. Simulation techniques also received substantial attention. The steel industry was soon joined by the cement industry in the development of computer methods for process applications. Computers were in use for feed-material blending and kiln control in the early 1960's. Computer development in other pyro processes, such as aluminum reduction and glass-making, also marked significant advances by the mid 1960's. Aluminum smelter potline control is a nearly universal application at this point, and the development of glass furnace computer process control represented a recent important technical advance in digital control techniques. Steel Hot strip rolling was the earliest significant process computer application in the metallurgical industry. Computer control of rolling mill operations is now a steel mill standard component, particularly in plants newly placed into production. 1, 2 Initial computer installations principally carried out procedural routines in setting mill clearances for production lot control. Recent developments are leading toward feedback control based on mathematical model techniques. 3

Jan 1, 1969

By George S. Rice

The increasing use of mechanization at the face of the workings in coal mining and the consequent necessity of special supports of the roof has led, in several countries, to considerable scientific investigation, including physical tests in mines as well as on specimens of roof rocks to obtain data on the behavior of the immediate roof strata and on the effect of its pressure on supports while the coal is being mined. The investigations discussed in this paper do not include studies of the ultimate effect of subsidence and movement of the roof rock over the mine excavation, upon higher strata and the surface, but are confined to the immediate underground effects in the workings. The more recent principal investigations which have been brought to the attention of the writer are as follows: Germany.—The trial of strip packing, the usual method employed in Great Britain in longwall workings, as compared with complete packing heretofore used in Germany and in France to minimize subsidence; the behavior and strength of metal props under load; the testing of the strength of coal measure rocks, in the laboratory of the Technical High School of Breslau; and an investigation, by a special commission, concerning "bumps" as a possible cause of instantaneous outbursts of gas in coal mines of Lower Silesia. France.—The cause of instantaneous outbursts of gas in the Gard mines and tests by the official French experimental organization of the "electrical resistivity" of coal as a possible means of detecting a condition preceding an instantaneous outburst. Great Britain.—The subsidence of the roof and rise of the floor preceding and during excavation of the coal, in longwall and in room-and-pillar or bord-and-pillar workings; the compression and lateral movement of the road packs in longwall back from the face; the extent of separation of the immediate roof layers from the higher strata following mining excavation;

Jan 1, 1932

By David N. French

In a recent paper, Miyoshi, Hara, and sugimotoL have shown that hardness increases and crack resistance decreases with polishing time in tungsten car-bide-cobalt alloys. They attribute the changes in hardness and crack resistance to cold working in these alloys. More recently Exner2 explains the decrease in crack resistance with the amount of material removed (polishing time) by suggesting that polishing removes a high compressive residual surface stress due to the initial grinding operation. He cites previous work on steel to show grinding can induce surface compressive stresses but offers no direct experimental measurements to support this in cemented tungsten carbides. In recent work we have observed changes in residual stress in the W C phase as measured by X-ray diffraction techniques with changes in polishing conditions.3 As a result of the work of Miyoshi et al.,L a brief study was undertaken to investigate the effects of polishing and grinding on the residual stress in the WC phase and have been reported.4 A single composition of tungsten carbide —10 wt pct Co was used. Two initial conditions were studied: an annealed condition with about -30,000 psi residual stress from the differences in thermal coefficients of expansion of WC and cobalt and, on the same specimen, a surface ground with a 150 grit diamond wheel. Stress was measured in the WC phase using X-ray diffractometry as a function of the amount of material removed by metallographic polishing with 6 diamond paste. The results are shown in Fig. 1. Two things are noted, 1) polishing with 6 p diamond paste has little effect on the annealed sample and 2) the magnitude of the grinding stress is markedly reduced as material is removed. By the time 0.1 mil is removed the surface has a metallographic polish satisfactory for light microscopy examination. Thus the surface, even though polished, can still retain most of the stress due to grinding. Since WC is itself slightly ductile, it seems reasonable that high compressive stresses can be generated in the surface by the plastic deformation accompanying grinding. Exner2 suggests, by analogy with steel, that as a result of grinding both WC and cobalt in the

Jan 1, 1970

By Thomas M. Drown

I DESIRE to communicate to the Institute the results of a few analyses which bear on the condition of carbon in gray and white iron. These analyses were made in the course of an investigation, now in progress, of the chemical composition of "chilling" irons. It will be remembered that Bell says he found no material difference in the amount and condition of carbon in gray and white pig iron made at the Clarence furnace, in England, and he therefore refers the difference in color and appearance in these two varieties of iron to the size of the particles of graphite. I quote from his "Chemical Phenomena of Iron Smelting:" "The inference I would draw from the information afforded by these analyses is, that the condition of iron in respect to its so-called 'richness' is, within certain limits, entirely independent of its chemical constitution.. .. In the fluid state, I conceive the carbon, so taken up, confers upon the iron the property of fusion much below the temperature at which the pure metal melts, and the carbon itself may be regarded as dissolved in the iron. If, during the process of manufacture, the pig metal has been formed at a low temperature, consolidation, I imagine, takes place under such circumstances that the crystals are so minute, and the carbon which is separated assumes the uncombined or graphitic form in particles so minute as to be invisible, and, in consequence, the iron is white. If, on the other hand, the furnace is working at a very high temperature, the intensely heated iron crystallizes with large facets, upon which the extruded carbon assumes the condition of distinct plates or flakes. Should the temperature be less intense, these crystals are of smaller dimensions, and the separated carbon is less conspicuous, and, as the temperature of the furnace declines, the crystals decrease in size, as do the flakes of carbon, until both disappear in white iron.. .. Returning, then, to temperature as the cause of differences in quality of pig iron, the 'chilling' of gray metal, and its conversion into white, may be regarded as the effect of preventing, by rapid cooling, the formation

By C. Baldwin Sawyer

J. S. Vanick,* Washington, D. C. (written discussion).—To those who have been confronted with the study of the gas-metal reactions, this paper is a most welcome contribution. My personal interest in work bearing upon this general problem, stimulated by an appreciation of the difficulties inherent to problems of this type, prompts a few words of discussion. Table 2 of the paper shows a gradual increase in the nitrogen content with an increase in pressure, and an interpretation follows in which nitrogcn is used as the compressed medium when the conditions admit that cyanogen gas could be active as a contaminating ingredient. Fusions of electrolytic iron made in the induction furnace in an atmosphere of deoxidized nitrogen and out of contact with contaminating materials have shown no microscopic evidence of -a nitrogen increase; using a refractory-lined graphite crucible in the furnace under the same conditions or admitting air often resulted in the occurrence of nitride needles in the solidified melt. These results suggested that a nitrogenous compound served as a vehicle for the introduction of nitrogen and that such compound was not available when the pure gas and carbon-free refractory were used. The fusion of pure iron in pure nitrogen is perhaps a matter of theoretical interest. The author's work serves a more practical purpose when applied to steels rather than iron. Table 2 reports the absence of nitride needles in melts made under pressure of one atmosphere, although the quantity of nitrogen present would seem to exceed microscopically detectable percentages. In some recent work29 on carburized iron, nitride needles have been observed in areas analyzing as low as 0.015 per cent. nitrogen. This low percentage of nitrogen would indicate that the solubility limit is less than 0.030 per cent. for hypoeutectoid steels. There is the possibility that the areas of pearlite which exist in a hypoeutectoid steel restrict the distribution of nitrogen and limit its presence to the ferritie fields. In view of this work and the references quoted by the author, I am led to expect that the value for the solubility of nitrogen in solidified iron may approach

Jan 1, 1924

By R. A. Liddle

Intermitt'en'I'ly during the past 10 years showings of oil and gas in tests drilled in the eastern part of Texas have stimulated the search for production. Tests on the flanks of the long-known salt domes, principally Keechi and Butler, have found oil in small quantity in the Woodbine formation of the basal part of the Upper Cretacrous. In the central part of Cherokee County, Colliton et all in 1926, in their Clapp No. 2 found a good showing of 37" B6. oil at about 3500 ft. Several wells were drilled in 1926 and 1927 as a result of this showing. On Jan. 22, 1927, Humble Oil & Refining Co. wildcatting on Carey Lake salt dome, obtained commercial production in its Clark No. 1. This inaugurated intensive exploration both for salt domes and for other types of structure. As a result several new domes and a few promising structures of other types have been discovered. Development in East Texas durinG 1927 Carey Lake Dome Location.—On the Neches River in Anderson and Cherokree counties, 10 miles west of Jacksonville, Cherokec (lounty. (Fig. 1.) date of Discovery.—During 1925 geologisls of the Humble Oil & Refining Co. working in the Neches River valley discovered slight surface fracturexs, cratic dips, and slickensided clays and sands in green-sands of the Mount Selman formation north of Carey Lake. A number of core tests were drilled by the Humble Oil & Refining C'o. during 1925 and 1926, some more than 1500 ft. deep, to check their surface obsuvations of faulting, and the possibilities of a salt dome. On May 16, 1927, solid rock salt was reached at 2142ft. in the first deep test on the prospect. Surfacc Indications.—Surface indications of the Carey Lake dome, though not as evident as manifestations at the previously known domes of Palestine, Keechi, Butler, Grand Saline, Steen and Brooks, are more noticeable than on any of the domes discovered in 1927. F. E. Poulsen, of the Pure Oil Co., who examined the area before the deep tests were drilled, noted the alignment of erratic surface dips which suggested faulting, especially in conjunction with slickensiding, and the local deflec-

Jan 1, 1928

By B. Ramaswami, U. F. Kocks, B. Chalmers

The latent hardening of silver and an Ag-Au alloy was investigated by lateral compression, overshoot in tension and cormpression, and the stability of multiple-slib orientations. The latent hardening of a secondary slip systenz depends on its relation to the primary slip system. For most secondary slip systems the latent hardening is larger for Ag-10 at. pct Au than for pure silver. The maximum increase in. flow stress on a secondary slip system over that of the primary slip system was 40 pct. The work hardening during the lateral-compression test on the latent system after prestress on the primary system is iuterbreted in terms of the preferential distribution of barriers to dislocation movement with respect to the active slip system in work-lzardened fcc crystals. The work-hardening in fcc crystals is mainly due to the dislocation interactions and the barriers to dislocation movement formed as a result of reactions between dislocations of different slip systems. The operation of sources on the latent system depends on the flow stress of those systems; hence, the increase in flow stress of a latent system due to glide on an active system, which is called latent hardening, is an important element in understanding the phenomenon of work hardening. The problem of latent hardening has attracted the attention of many investigators in the past. For example, a theoretical study of the elastic latent hardening of the latent systems due to glide on an operative system has been made by Haasen' and ~troh. These calculations, however, neglect the stress required for the intersection of forest dislocations by the glide dislocations, a factor which would be important for producing macroscopic strains on the secondary slip systems. The importance of this factor will become evident from the results presented here. Attempts have also been made to determine the latent hardening of different slip systems by experimental means by the methods summarized in Table I.3-9 The experimental methods used have been subject to certain limitations. For instance, in the method used by Hauser,9 frictional constraints between the specimen and the compression platen were not eliminated by proper lubrication (see Hos- ford10). Secondly, with the exception of Kocks,6 Hauser,9 and Rohm and Kochendorfer,11 latent-hardening studies have been made on only one of the slip systems, i.e., on either the conjugate or the coplanar slip system; hence, extensive results are not available on the latent hardening of different slip systems in the same materials, with the exception of aluminum.6 It was therefore decided to study the latent hardening of the conjugate, critical and half-related slip systems in silver. Similar experiments were done in Ag-10 at. pct Au to study the effect of solute (gold) on the latent hardening of silver. Lastly, indirect evidence can be obtained by a study of the orientation stability of crystals of multiple-slip orientations in tension and compression. This method has been used by Kocks6 to supplement his studies of latent hardening in aluminum. Similar studies were made at room temperature in single crystals of silver. EXPERIMENTAL PROCEDURE The single crystals of the desired orientations were grown and the tensile test specimens were prepared as described in Ref. 12. The compression tests were made on 1/4-in.-cube specimens. The specimens were cut from single crystals, in the Servomet spark-erosion machine.13 The two cut surfaces were planed using the lowest available planing rate in the machine to minimize the deformation layer. A brass strip was used as the planing tool. This method of preparation ensured plane parallel faces for the compression tests. The deformed material was removed by prolonged etching in a weak etching solution. A weak etching solution was used to prevent pitting of the surfaces and to ensure uniform etching. About 25 to 50 µ of material were removed from all faces by the etching treatment. The specimens were then annealed for 24 hr at 940°C in oxygen-free helium and cooled in the furnace to room temperature over a period of 7 hr. After annealing, the orientation of the specimens was determined by Laue back-reflection technique to make sure that no recrystallization had occurred on annealing. The compression-test technique and setup are described in Ref. 14. The Laue back-reflection technique was used to study the overshoot in tension, the overshoot in compression, and the stability of the axial orientation in tension and compression. The tests were interrupted after every few percent strain to determine the axial orientation. In investigating the overshoot in compression, the operative system was determined by studying the asterism of the Laue spots.

Jan 1, 1965

By P. W. Bakarian

Previous determinationl,2,3 of the texture of magnesium and its alloys have shown only slight variations in the principal features of the structure. This investigation presents pole figures for magnesium and two of its alloys, in which differences of some magnitude will be shown. Schmid and Wassermann have considered the texture of magnesium in analogy with that of zinc—also a hexagonal lattice. Whereas the zinc texture is said to be derived primarily through basal slip and secondarily through {IO2}† twinning, the {102} twinning is considered impossible at the later stages of the rolling in magnesium because of its smaller axial ratio. This state of affairs appears reasonable for pure magnesium, but for alloy textures the situation is more complex. A double orientation similar to that found in zinc has been reported by J. D. Hanawalt,4 and the addition of small amounts of calcium to magnesium and its alloys to produce a double texture was noted by J. C. McDonald.5 The pole figures of this investigation, using an improved X-ray technique, show these various textures. The dependence of directional properties of rolled sheet on modifications of texture is well recognized. Correlation of physical properties with existing texture should be even more significant if quantitative valuations are attached to the various areas on the pole figures. Such a quantitative technique is developed herein. Experimental Method Two alloys were used, besides high-purity magnesium. In each case, the metal was extruded to bars 1/2 in. thick and hot-rolled to a thickness of about 0.075 in. It had been established previously that such a reduction was more than sufficient to eliminate the extruded structure. The rolling proceeded in the same direction as that of the extrusion, without any cross rolling. The temperatures corresponded to normal commercial practice, averaging around 600°F. A unique method of preparing the sample was developed in this work. Instead of using a flat specimen, a stem of the metal was cut out of the rolled sheet in the desired direction (rolling direction) as shown in Fig. I. From a sheet of 0.075 to 0.065-in. gauge, the stem was cut to a square cross section with a jeweler's saw, rounded with a file and polishing paper to a diameter of 0.060 in. and evenly etched in dilute hydrochloric acid to a diameter of 0.038 + 0.001 in. In this way, a cylinder of the original sheet with its axis in the desired direction was produced. By using this type of specimen for the pin-point pictures, any variance in the absorption of the diffracted beam at the various angular settings of the specimen, was completely eliminated.*

Jan 1, 1942

By C. E Shoenfelt, Gail F. Moulton

Proven and developed oil reserves, and productive capacity increased during 1943 in the fieids of the Rocky Mountain region. Oil production during the year was nearly 45 million barrels, or slightly less than in 1942. The rate of production at the start of 1944 was slightly less than at the start of 1943. Pipe-line projects scheduled for completion during 1944 should permit a substantial increase in the rate of production. Wildcat exploration was more extensive in Montana during 1943 than in other states in the region. The results of wildcat drilling were unsatisfactory, although new oil fields were discovered on the Gebo, Little Buffalo Basin and Steamboat Butte structures of Wyoming, the Gage anticline of Montana, and the Clark Lake structure of Colorado. The area of the structures on which the discovery wells were drilled is known to be considerable, but further drilling is required to determine the importance of these fields. The most important increase in proven reserves resulted from the drilling to newly discovered deeper producing formations in the Elk Basin and other fields of the Big Horn Basin area of northern Wyoming. Lack of a market and unfavorable prices for heavy black oils had prevented complete exploration of favorable areas in the Rocky Mountain region for many years. In particular, the effect on further exploitation of the Big Horn Basin area had been quite serious. The increased demands for all oils created by the war and an increase in price in February 1943, combined later with Government approval of construction of pipe lines from the Big Horn Basin area to the Billings and the Casper districts, provided a basis for undertaking a drilling program. The important additions to reserves were made by drilling in previously discovered fields. The newly discovered fields resulted from drilling on favorable structures which had been known for several years. A continuation of the favorable results obtained during 1943 seems possible only if further testing of the newly discovered fields is satisfactory and if drilling on less favorable known structures or geophysical prospects results in the discovery of new fields. The amount of drilling in the Rocky Mountain states of Colorado, Montana and Wyoming, was about the same during 1943 as .in 1942. However, owing to the fact that a number of wells of large potential production were completed in the Elk Basin field, the total initial production of the prodicing wells was- nearly twice as great for 1943 as for 1942. Explorational activity at the end of 1943 seemed to be directed to geophysical methods, which are required to discover structures hidden beneath the rocks of Tertiary age in the Powder River and other large sedimentary basins. It is in

Jan 1, 1944

By K. S. Krishnam, A. G. Guy

VOLUME 6 of the Transactions of the Baikov Institute of Metallurgy, Moscow, is devoted to the subject of "the experimental and theoretical study of the physical characteristics of dilute solid solutions,11 and summarizes work that has been done largely in the years 1958-9. In view of the attention that Soviet investigators have given to this subject, it seemed useful to carry out an independent experimental investigation in an effort to judge the scientific basis and practical significance of this field of study. The present note is a preliminary report of this investigation. The first property studied by the Soviet group was X-ray spectra of solid-solution alloys.' An anomaly observed at low concentrations (--0.05 at. pct) of the alloying element led to the theory that each impurity atom in a transition-metal base alloy is the center of a "block" of affected atoms with a radius of about 10"7 cm. This theory was further developed in a later paper.2 By this time similar anomalies had been found in diffusion coefficients3 and in thermal expansion.4 The entire development up to 1959 was reviewed in a comprehensive paper, and further theoretical ideas were also published at this time. Finally, the volume mentioned above was published in 19607 giving new experimental data on anomalies in optical properties and Hall constant, and a new theoretical treatment also appeared.' Although western scientists have done both theoretical work, summarized recently by Friedel,9 and considerable experimental work on dilute solid solutions, there is little support for the marked anomalies reported in the Soviet papers. Of the physical properties studied by the Soviet investigators, thermal expansion was chosen for the present investigation because of the relative ease of obtaining the necessary precision of measurement. A Leitz dilatometer was used for this purpose, and a special technique involving interchanging of the two specimens being compared permitted a precision of 0.05 x X in average thermal expansion over the range 27° to 600°C. The specimens were heated and cooled in vacuum or in a protective atmosphere at a rate of 50 °C per hr. Ferrovac E iron was used as the comparison specimen and in every case had a coefficient of expansion higher than (or equal to) that of the alloy. Since unintentional impurities are an important factor in studies of dilute alloys, special attention was given to the purity of the iron and the alloys used. The alloys were the same of those used by Abrahamson10 and by Michalak," and their preparation is described in these references. Chemical analyses of the Ferrovac E iron and of typical Fe-W and Fe-Mo alloys are given in Table I. The purity of the iron and alloys is undoubtedly higher than in the

Jan 1, 1962

By P. W. Bakarian

Previous determinationl,2,3 of the texture of magnesium and its alloys have shown only slight variations in the principal features of the structure. This investigation presents pole figures for magnesium and two of its alloys, in which differences of some magnitude will be shown. Schmid and Wassermann have considered the texture of magnesium in analogy with that of zinc—also a hexagonal lattice. Whereas the zinc texture is said to be derived primarily through basal slip and secondarily through {IO2}† twinning, the {102} twinning is considered impossible at the later stages of the rolling in magnesium because of its smaller axial ratio. This state of affairs appears reasonable for pure magnesium, but for alloy textures the situation is more complex. A double orientation similar to that found in zinc has been reported by J. D. Hanawalt,4 and the addition of small amounts of calcium to magnesium and its alloys to produce a double texture was noted by J. C. McDonald.5 The pole figures of this investigation, using an improved X-ray technique, show these various textures. The dependence of directional properties of rolled sheet on modifications of texture is well recognized. Correlation of physical properties with existing texture should be even more significant if quantitative valuations are attached to the various areas on the pole figures. Such a quantitative technique is developed herein. Experimental Method Two alloys were used, besides high-purity magnesium. In each case, the metal was extruded to bars 1/2 in. thick and hot-rolled to a thickness of about 0.075 in. It had been established previously that such a reduction was more than sufficient to eliminate the extruded structure. The rolling proceeded in the same direction as that of the extrusion, without any cross rolling. The temperatures corresponded to normal commercial practice, averaging around 600°F. A unique method of preparing the sample was developed in this work. Instead of using a flat specimen, a stem of the metal was cut out of the rolled sheet in the desired direction (rolling direction) as shown in Fig. I. From a sheet of 0.075 to 0.065-in. gauge, the stem was cut to a square cross section with a jeweler's saw, rounded with a file and polishing paper to a diameter of 0.060 in. and evenly etched in dilute hydrochloric acid to a diameter of 0.038 + 0.001 in. In this way, a cylinder of the original sheet with its axis in the desired direction was produced. By using this type of specimen for the pin-point pictures, any variance in the absorption of the diffracted beam at the various angular settings of the specimen, was completely eliminated.*

Jan 1, 1942

By Gail F. Moulton, C. E. Shoenfelt

Proven and developed oil reserves, and productive capacity increased during 1943 in the fieids of the Rocky Mountain region. Oil production during the year was nearly 45 million barrels, or slightly less than in 1942. The rate of production at the start of 1944 was slightly less than at the start of 1943. Pipe-line projects scheduled for completion during 1944 should permit a substantial increase in the rate of production. Wildcat exploration was more extensive in Montana during 1943 than in other states in the region. The results of wildcat drilling were unsatisfactory, although new oil fields were discovered on the Gebo, Little Buffalo Basin and Steamboat Butte structures of Wyoming, the Gage anticline of Montana, and the Clark Lake structure of Colorado. The area of the structures on which the discovery wells were drilled is known to be considerable, but further drilling is required to determine the importance of these fields. The most important increase in proven reserves resulted from the drilling to newly discovered deeper producing formations in the Elk Basin and other fields of the Big Horn Basin area of northern Wyoming. Lack of a market and unfavorable prices for heavy black oils had prevented complete exploration of favorable areas in the Rocky Mountain region for many years. In particular, the effect on further exploitation of the Big Horn Basin area had been quite serious. The increased demands for all oils created by the war and an increase in price in February 1943, combined later with Government approval of construction of pipe lines from the Big Horn Basin area to the Billings and the Casper districts, provided a basis for undertaking a drilling program. The important additions to reserves were made by drilling in previously discovered fields. The newly discovered fields resulted from drilling on favorable structures which had been known for several years. A continuation of the favorable results obtained during 1943 seems possible only if further testing of the newly discovered fields is satisfactory and if drilling on less favorable known structures or geophysical prospects results in the discovery of new fields. The amount of drilling in the Rocky Mountain states of Colorado, Montana and Wyoming, was about the same during 1943 as .in 1942. However, owing to the fact that a number of wells of large potential production were completed in the Elk Basin field, the total initial production of the prodicing wells was- nearly twice as great for 1943 as for 1942. Explorational activity at the end of 1943 seemed to be directed to geophysical methods, which are required to discover structures hidden beneath the rocks of Tertiary age in the Powder River and other large sedimentary basins. It is in

Jan 1, 1944

By E. J. Pasierb, H. W. Paxton

Mavkers ill a diffusion couple in the iron-chromium system move towards the high chromium side indicating Dcr > DFe at the marker composition. By a combituztion of measurements of D& and D a: a function of composition, this is also shown independently. DFe is calculated as a function of composition. and shown to be in reasonable agreement with measured values by other workers. MEASUREMENTS of marker movements in diffusion couples have been used from time to time to demonstrate that a vacancy or interstitial mechanism may be operative. Since there is a possibility that ring diffusion1 may be operative in chromium, the present experiments are of interest in showing some non-ring mechanism in iron-chromium alloys around the equiatomic composition. EXPERIMENTAL PROCEDURE The movement of markers originally at the interface between 1-in. sq sections of pure Cr (6 mm thick) and outer slabs of 30 Cr-70 Fe alloy was followed as a function of time at temperatures from 1150" to 1425"C, in a Kanthal-wound furnace. Temperature control was +5°C over extended periods. The analyses of these alloys are given in Table I. Selection of suitable markers presented a considerable experimental problem; the eventual solution was to draw quartz rod down to 0.01 cm and seat this in V-grooves 0.01 cm deep on each side of the chromium prior to welding. A preliminary experiment in which the groove was machined in the alloy gave identical results. Welding was accomplished by passing a heavy current through specimens under moderate pressure in a helium atmosphere. This method produced good welds with a planar interface as shown by subsequent metallo-graphic investigation. Any markers which did not adequately fill their groove and showed subsequent contamination from the atmosphere during heat treatment were not considered reliable. The composite sample was ground and metal-lographically polished on the four sides perpendicular to the interface. Fiducial marks (deep milled slots) were made outside the diffusion zone to check on total volume change. All necessary measurements were made on a metallograph reading to +0.0005 cm. The samples were wrapped in tantalum foil and given diffusion anneals for times to 200 hr in carefully purified dry hydrogen in a sealed McDanel porcelain tube. Chromium-zirconium chips were introduced near the specimen as an additional getter. The specimens were cooled relatively slowly after the diffusion anneal to preserve the McDanel tube but no significant error in effective time at temperature was thereby introduced. At least 1 mm was ground off the surface before measurements were taken. It was observed that the grain size following short diffusion anneals was several mm and was appreciably larger in the 30 Cr alloy than in the pure Cr. No significant grain boundary penetration was present as indicated by the etch limit. The results are presented in the next section. Measurements of D were made by standard sectioning techniques with chemical analysis. Machining difficulties limited the

Jan 1, 1961

By A. J. Mortlock

Cobalt and nickel have been diffused at tracer concentrations in gold at several temperatures in the range from approximately 700° to 950°C. The diffusion penetration profiles were determined by a serial sectioning technique in which the gold is first anodized and then the anodic layer is dissolved in acid. In this ulay sections as thin as 250A could be removed reproduci-bly. In all cases, the region close to the specimen surface was characterized by irregular behavior in the sense that the logarithm of concentration was not linear in the square of the penetration distance. In sotne cases, there zuas an indication of the operation of very slow dijfusion in this region, while in others the apparent diffusion coejj'icient was negative. Possible reasons for this anomalous behavior are briefly discussed. In recent years it has been found that the region close to the surface of a metal can sometimes exhibit anomalously slow diffusion characteristics relative to the interior of the metal. One of the best examples of this fact is the work of Styris and omizuka,' who showed that the apparent diffusion coefficient for zinc in the region withi: about 1 p of the free surface of copper was about ,,,, that at deeper penetrations. This result is particularly interesting, because it is free from the possibly complicating effects of low solubility of the diffusing tracer in the solvent metal. In the case of diffusion under conditions of low solubilitjr, interpretaticn of the results in terms of lattice diffusion is difficult because of the enhanced short-circuiting produced by segregation to dislocations.2'3 Measurements by Duhl et 1. suggest that cobalt diffusing in gold may also show a near-surface effect of this type. Once again the solubility is high, so that this result could be of great interest. However, the technique used for analyzing the diffusion penetration zones by Duhl, viz. the counting of residual gamma activity in the specimen following sectioning, appears to have indicated a near-surface effect in a parallel experiment on the self-diffusion of gold reported at the same time. The latter result is known to be spurious, since Kidson5 has demonstrated that self-diffusion in gold does not show this effect. Duhl et 01. also reported some measurements on the diffusion of nickel in gold, but failed to give any data for the near-surface region. As the solubility of nickel in gold is high, such data would also be of special interest. We, therefore, decided to conduct another set of experiments on the diffusion of nickel and cobalt in gold, using a sectioning technique that allows the individual sections to be assayed for solute content and thus gives direct determinations of penetration profiles. Also, by sectioning with an anodizing/stripping tech- nique, very thin layers can be removed and the region close to the surface studied in detail. MATERIALS The gold specimens were supplied as single crystal disks $ in. in diam by a in. high by Monocrystals Co. of Cleveland, Ohio. The gold itself was of spectro-scopic purity, i.e., better than 99.99 pct pure. METHOD Specimen Preparation. One flat end face of each gold crystal was spark planed with a Servomet spark erosion machine set for minimum spark energy. Following this treatment the crystals were preannealed for 2 to 4 days at temperatures of either 400" or 700°C. The three crystals preannealed at 700°C showed signs of recrystallization. The spark-planed end face of each crystal was then coated with the appropriate amount of 63i or 60 radioactive tracer. This deposit was laid down in a simple plating bath containing the as-supplied solution of the radioactive isotope as well as sufficient ammonium oxalate to saturate the solution. Some ammonium oxalate remained undissolved on the floor of the bath for this purpose. During plating further additions of ammonium oxalate were sometimes required to allow the plating to continue satisfactorily, perhaps due to passivation of the undissolved oxalate already present. The thickness of the deposited layer was determined by comparison of the apparent surface activity of the plated specimen with that of a similar specimen having a weighable deposit of the isotope on its end face. Correction for self-absorption of the radiation was made in this calculation. Annealing. The deposited crystals were annealed in a hydrogen atmosphere in sealed silica tubes. During this heat treatment they were supported, active face down, on optically flat silica plates. The temperature was measured with calibrated Pt vs Pt-10 pct Rh thermocouples, and the tabulated values can be taken to be correct to Z°C. All the crystals showed evidence of recrystallization following these heat treatments, suggesting that initially they may not have been good single crystals or had suffered strain during delivery. Concentration Profile Analysis. After annealing, the crystals were sectioned by the anodizing-stripping technique.6 The anodizing involved suspension of the specimen with its cylindrical axis horiz6ntal by a gold wire in a 200-ml beaker containing 1 M Hg304. A cathode in the form of a strip of gold sheet, 2 in. wide and positioned to be in contact with the curved side of the beaker, completely encircled the specimen. An anodizing current of 30 ma, corresponding to a current density of 5 ma per sq cm on the surface of the specimen, was passed for times ranging from 5 to 150 min depending on the thickness of gold to be removed; the solution was stirred continuously during this process. Following this treatment, the specimen

Jan 1, 1969