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By D. O. Hobson

Zirconium single crystals of various specific orientations were fabricated by rolling or drawing. The resulting textures were determined and are discussed with respect to the deformation modes that produced them. The crystals deformed in a predictable manner by combinations of up to third-order twinning with three twinning modes and by slip. Twinning was found to play a major role in initial texture formation. Texture changes produced by slip occurred only at the higher reductions. The twinning sequences that produced each intensity peak during the initial reductions could be identified. Schmid factor criteria were found useful in predicting which deformation modes to expect for each crystal orientation and fabrication procedure. The possible application of these data to poly-crystalline material is discussed. PREFERRED orientation or texture has a significant effect on the properties of most materials, causing anisotropy in fabricated cubic metals and enhancing the natural anisotropy of noncubic metals. This study evaluates the effects of several fabrication methods on the textures formed from specific starting orientations of zirconium single crystals and, it is hoped, gives an insight into the effects of the same operations on poly-crystalline material. BACKGROUND In fcc and bcc metals, texture changes take place by gradual lattice rotations caused by the operation of one or more slip systems. Deformation twinning plays an insignificant role in the deformation of such metals. In zirconium and its alloys, however, and in many other hep metals the ability to twin allows very rapid texture changes to be made with very small amounts of deformation. The deformation systems found in zirconium and its alloys are prism slip and three twinning modes.1 Slip occurs on the {1010}< 1120) system. There is little or no appreciable basal slip in zirconium. The twinning planes, illustrated in Fig. 1, are {1012}, {ll2l}, and {1122}. Two twinning modes, the {1012} and the {ll2l} operate for a tensile stress along the basal pole. A compressive stress parallel to the basal pole is required for {ll22} twinning. These twinning operations cause a 35- to 85-deg reorientation of the basal pole. The {1012} twin is the predominant tensile twin at room temperature. The twinning shears, S, are shown in the figure. A criterion for predicting which deformation system will operate when a grain is subjected to a known stress state is the Schmid (orientation) factor. This factor gives the fraction of the applied stress that computer program was written2 to calculate the Schmid factors for the four deformation modes in zirconium. It assumed three orthogonal stress axes and considered ninety-one different orientations of the basal pole in one octant of this stress space. At each basal pole position the Schmid factors were calculated for seven positions of rotation at 10-deg increments of the unit cell about the basal pole. Schmid factors were determined for a total of 637 orientations and for twenty-four deformation systems in each orientation. The program listed the Schmid factors for uniaxial stress parallel to each axis and, to approximate rolling, or-thonormal biaxial stress was also considered. Fig. 2 shows the range of orientations over which the various types of deformation would tend to predominate in biaxial plane strain with the stresses, equal magnitude. The exact boundary position between regions of different deformation modes depends, however, on the relative values of the critical shear stress for each deformation mode. Fig. 2 is drawn on the assumption that they are equal and it therefore may be only approximately correct. It is also recognized that the biaxial stress analysis may not be applicable in certain crystal orientations. EXPERIMENTAL PROCEDURE Single crystals of zone-refined zirconium, produced by Wilson of this Laboratory,3 were electrical-discharge-machined to form specimens for rolling, tube-drawing, and rod-drawing studies. Specimens were rolled at room temperature on 2-|--in.-diam hand-powered rolls from three different starting orientations: 1) the basal plane parallel to the rolling plane and the [1120] in the rolling direction, (0001)[ll20]; 2) the (1120) plane parallel to the rolling plane and the basal pole in the rolling direction, (1120)[0001]; and 3)_the (1120) plane parallel to the rolling plane and the [1100] in the rolling direction, (1120)[ll00]. Drawing specimens were cut with the [0001] direction as the drawing direction in the tube blank and [1120] as the drawing direction in the rod specimen. The drawing

Jan 1, 1969

By P. Greenfield, C. C. Smith, A. M. Taylor

J. E. Harris (Berkeley Nucclear Laboratories, England)—Greenfield et al.11 attribute abrupt changes in slope of their log o/log i curves for heat-treated Mg/0.5 pet Zr alloy (zA) to &apos;atmosphere&apos; locking. It is proposed here that a more reasonable explanation of the apparent strengthening at low rates of strain can be based on precipitation either during the preanneal or during the creep tests. All the tests were carried out above 0.5 Tm where solute atmospheres are likely to be largely evaporated2 and can migrate sufficiently rapidly so as not to impose any &apos;drag&apos; on the moving dislocations. McLean3 has derived an expression for determining the temperature Tc above which, due to the high-migration rate of the atmospheres, Cottrell or Suzuki locking can play no part in determining creep strength. This expression, which holds for an applied shear stress of not greater than 5 X 107 dynes per sq cm is: Tc/Tm= 7/6.8 - log10? where i = secondary creep rate The values for T, corresponding to the maximum and minimum reported creep rates at each temperature have been calculated from the data of Greenfield et al. These are given in Table VII. All the test temperatures were above T,, the margin being greater for the higher temperatures and for the lower strain rates where the breaks in the log s/log ? curves occurred. Dorn and his collaborators14, 17 have studied systematically the effect of solute hardening on the creep properties of an A1/3.2 at. pet Mg alloy. In the temperature range where strain aging occurred in tensile tests, abnormally high-activation energies for secondary creep were obtained but at temperatures above 0.43 Tm, solute alloying did not have any effect on the creep parameters. Moreover, there have been no reports of any strain aging phenomenon during elevated temperature tensile tests with ZA material.18 Instead of the observed strengthening being due to atmosphere locking, it is now proposed that precipitates play an important role in enhancing the creep strength of the material. There are two possibilities—precipitation of zirconium hydride during the high-temperature preanneal and/or precipitation of the hydride or a-zirconium during creep. On the basis of the former the results can be interpreted in terms of a critical stress being necessary to force the dislocations through or over preexisting precipitates. From the latter, if the strengthening is due to pre- cipitation during the test then hardening should be associated with a critical strain rate. At low rates of strain, time is available during the tests for precipitation to occur either directly onto dislocations (thus pinning them) or generally throughout the matrix (which would impede dislocation movements). Examination of the data of Greenfield et al. suggests that both mechanisms may be operative since they observed precipitation during creep and also found that their alloys exhibited high-creep strength in the early stages of the low-stress tests, i.e., before creep-induced precipitation had time to occur. It is not easy to understand why they considered that precipitation of zirconium hydride is unlikely to occur at 600°C while it can take place in tests in air at as low a temperature as 200°C. Precipitation of the hydride during the preanneal cannot be ruled out merely on the basis of metallographic examination. Hydride precipitates in ZA type alloys are very small and can only be accurately resolved in the electron microscope.9 For example, in this laboratory20 hydride platelets with major dimensions <(1/10) µ have been observed by electron transmission through thin film specimens of hy-drogenated ZA material. Complex interactions between dislocations and such particles are illustrated in Fig. 12. Additional evidence for precipitation during pre-annealing is provided by the data presented in Greenfield&apos;s Fig. 1 and Table IT. These show that the creep strength at 200o and 400°C increases with the time of preanneal at 600°C. Such increases cannot be explained on the basis of increases in grain size alone for further improvements in strength were observed when the material was annealed for longer times than that required to stabilize the grains. Although the main discussion is confined to ZA material, similar arguments can be used against the strain aging hypothesis proposed to explain the binary Mg/Mn alloy data. In this case no precipitation is possible during the preanneal, but precipitation-hardening during creep can occur.

Jan 1, 1962

By James K. Hallenburg

INTRODUCTION The delayed fission neutron, or DFN technique for uranium ore body analysis uses the first down-hole method for detecting uranium in place quantitatively. This technique detects the presence of and measures the amount of uranium in the formation. DFN TECHNIQUE DESCRIPTION The DFN technique depends upon inducing a fission reaction in the formation uranium with neutrons, resulting in an anomalous and quantitative return of neutrons from the uranium. Since there are no free, natural neutrons in formation, a good, low noise assessment may be made. There are several methods available for determining uranium quantity in situ. The method used by Century uses an electrical source of neutrons. This is a linear accelerator which bombards a tritium target with high velocity deuterium ions. The resulting reaction emits high energy neutrons which diffuse into the surrounding formation. They lose most of their energy until they come to thermal equilibrium with the formation. Upon encountering a fissile material, such as uranium, these thermal neutrons will react with the material. These reactions produce additional neutrons, the number of which is a function of the number of original neutrons and the amount of fissile material exposed. The particular source used, the linear accelerator, has several distinct advantages over other types of sources: 1. It can be turned off. Thus, it does not constitute a radioactive hazard when it is not in use. 2. It can be gated on in short bursts (6 to 8 microseconds). This results in measurements free of a high background of primary neutrons. 3. The output can be controlled. Thus, the neutron output can be made the same in a number of tools, easily and automatically. There are several interesting reactions which take place during the lifetime of the neutrons around the source. During the slowing down or moderating process the neutron can react with several elements. One of these is oxygen 17. This results in a background level of neutrons in any of the measurements which must be accounted for in any interpretation technique. These elements are usually uninteresting economically. The high energy neutrons will also react with uranium 238. However, the proportions of uranium 235 and 238 are nearly constant. Therefore, this reaction aids detection of uranium mineral and need not be seperated out. Upon reaching thermal energy the neutrons will react with any fissile material, uranium 235, uranium 234, and thorium 232. At present, we do not have good techniques for seperating out the reaction products of uranium 234 and thorium 232. However, uranium 234 is a small (.0055%) percentage of the uranium mineral and thorium 232 is usually not present in sedimentary deposits. When the uranium 235 reacts with thermal neutrons it breaks into two or more fragments and some neutrons. This occurs within a few microseconds after the primary neutrons have moderated and is the prompt reaction. One system uses this; the PFN or prompt fission neutron technique. We don&apos;t use this method because the neutron population is low and, therefore, the signal is small and difficult to work with, accurately. Within a few microseconds to several seconds the fission fragments also decay with the emmission of additional neutrons. Now, with a long time period available and a large neutron population we gate off the generator and measure the delayed fission neutrons after a waiting period. These neutrons can be a measure of the amount of uranium present around the probe. Thermal neutrons are detected with the DFN technique instead of capture gamma rays to avoid some of the returns from other elements than uranium. LOGGING TECHNIQUE The exact logging technique will depend, to some extent, upon the purpose of the measurement. However, the general technique is to first run the standard logs. These will include: 1. The gamma ray log for initial evaluation of the mineral body and for determining the position of the borehole within the mineral body, 2. The resistance or resistivity log for determining the formation quality, lithology, and porosity. 3. The S. P. curve for estimating the redox state and shale content, and measuring formation water salinity, 4. The hole deviation for locating the position, depth, and thickness of the mineral (and other formations), and 5. The neutron porosity curve. The neutron porosity curve is most important to the interpretation of the DFN readings. The neutrons from this tool are affected in the same way by bore hole and formation fluids as the DFN neutrons are. Therefore, we can use this curve to determine effect of the oxygen 17 in the water. Of course, this curve can be used to determine formation porosity. It can also be used to calculate formation density.

Jan 1, 1979

By C. W. Sherman, N. J. Grant

The correlation of the high temperature chemical properties of slag-metal systems with some easily measured property of either slag or metal at room temperature has been the goal of both process metallurgists and melting operators for many years. There are several rapid methods for estimating various constituents in steel in addition to the conventional chemical methods which are quite fast, but these do not reveal the nature of the slag as a refining agent, which is of primary interest to the steelmaker. Furthermore, there are several methods for examining slag, the three principal ones being slag pancake, petrographic examination, and the previously mentioned chemical analysis. The main objection to the last two is the lime required to make a satisfactory estimate of the mineralogical or chemical components. The objection to the first is the inadequacy of the information obtained. A new technique has been developed by Philbrook, Jolly and Henry1 whereby the properties of slags are evaluated from an aqueous solution leached from a finely divided sample of slag. It is known that the pH or hydrogen ion concentration (of saturated solutions that have dissolved certain basic oxides, notably calcium oxide) will indicate a pronounced basicity. Philbrook, Jolly and Henry devised the pH measurement technique in order to supply open hearth operators with a fast, reasonably accurate method of estimating slag basicity. They offered the method as an empirical observation and made no claims as to its theoretical justification. The results were presented as an experi-metally observed relationship which applied over an important range of basic open hearth slags. They found that, in plotting the measured pH against the basicity, the best relationship existed between the pH and the log of the simple V ratio, CaO/SiO2. Extensive investigation also showed that there were several variables in the experimental technique that influenced the results and necessitated following a standard procedure to obtain reproducible pH readings. These variables were: 1. Particle size of the slag powder used. 2. Weight of sample used per given volume of water. 3. Time of shaking and standing allowed before the pH was measured. 4. Exclusion of free access of atmospheric carbon dioxide to the suspension. 5. Temperature of the extract at the time the pH was measured. In subsequent investigations of the pH method by Tenenbaum and Brown2 and by Smith, Monaghan and Hay3 the general conclusions of Philbrook&apos;s work were reaffirmed. It was the object of the present investigation to extend the technique to a point where it could be used to evaluate slags of all types. Experimental Results PARTICLE SIZK OF SLAG POWDER A large sample of commercial blast furnace slag of intermediate basicity (V-ratio 1.15) was selected for the study. The slag had been put through a jaw crusher until all of it passed through a 20 mesh screen. Five fractions of this crushed material were separated, -20 to +40, -40 to +60, -60 to +100, -100 to +200, and -200 mesh. A representative sample of 0.5 g was removed from each fraction and the pH determined using the method of Philbrook. Check pH analyses on the sample fractions varied due to the different amounts of shaking. To eliminate this variable, a mechanical shaker was employed. In order to know the exact time of contact between the slag and water, it was found necessary to filter the extract at the end of the shaking period. Using the mechanical shaker and a filtering apparatus, similar runs were made on the five fractions for contact times of 5, 10, 20, and 40 min. Random checks gave reproducible results within 0.02 pH. The data are plotted in Fig 1. It can be seen from the plot that each slag fraction is hydrolyzed to an extent that is roughly proportional to the surface area exposed to the water. The (—100 to +200) mesh material changed very little in pH after 10 min. shaking time. The curves are symmetrical and lie in proper relation to one another. The —200 mesh curve appears to be somewhat flatter than the others, but this can be attributed to the portion of very fine material that is not present in the other fractions. The closeness of the (-100 to +200) mesh curve to the —200 mesh curve and the fact that a —100 mesh sample would contain amounts of slag down to 1 or 2 microns in diam were considered sufficient reasons for selecting a —100 mesh sample as representative of the whole sample of slag for the purposes of this investigation.

Jan 1, 1950

By S. M. Marshall

FOR a number of years European investigators have used laboratory methods of predicting the probable strength of coke made from coal, and recently several investigators in the United States have reported the use of various tests for this purpose. There is at present no method accepted as standard, however, nor is there even agreement as to the general type of test that should be used. Furthermore, because the details of most of the tests have not been worked out carefully, one investigator can not hope to duplicate the work of another. The extension of coke manufacture to new localities in the United States, and the increasing need for cokes of exceptional qualities made from the most economical mixtures, made it desirable to have some simple laboratory test which will determine whether given coals, alone or blended with other coals, are more satisfactory from the standpoint of coke strength than others of different cost. The work described herein has resulted in the development of a simple laboratory test which, it is believed, can be generally adopted in coal laboratories, and which will give concordant results even though performed by different investigators in different laboratories. The general method of predicting whether a coal or a mixture of coals will produce a strong coke, resistant to crushing and shattering, has been to correlate the known strengths of the cokes produced in commercial ovens with some measurable constituent or with some property of the coals, and then to use the relationship so found for forming an estimate of the coking strengths of coals unknown. Several such correlations have utilized the percentages of the various ultimate constituents of coal, such as the oxygen content and the hydrogen-oxygen ratio;(39)§ other correlations have involved the proportion of a, (3 and y compounds, (17&apos;21,30 or of "oil and solid bitumens."(16,30) Also a relationship has been traced between the coking properties of coal and the rate of change of the resistance offered to the flow of an inert gas by fine particles of the coal while being slowly heated. (11,17b) But the most general corre-

Jan 1, 1929

By John Eash

DURING recent years nickel has had an increasingly important role as an alloying element in the copper-tin bronzes. Nickel additions not only produce better casting alloys but also make alloys whose properties can be varied by precipitation hardening; thus leading to increased commercial application of copper-nickel-tin alloys. Recent investigations have indicated a decrease in the solubility of tin in the alpha phase as the annealing temperature is lowered and as the nickel content is increased within certain limits. A further change caused by the nickel additions is produced in the excess phase of the copper-tin bronzes. The alpha plus delta eutectoid is replaced by a clear precipitated constituent in the alloys containing up to 15 per cent tin and not less than 1 per cent nickel. This paper has a dual purpose. The first is to present a new determination of the alpha-phase boundary in alloys containing from 0 to 20 per cent nickel, together with the liquidus and solidus temperatures above that field. The second purpose is to give the equilibrium conditions existing in alloys exceeding the alpha phase containing up to 31 per cent tin and 5 per cent nickel, so that the disappearance of the alpha plus delta eutectoid constituent may be explained. After considering the earlier investigations of the related alloy systems and the experimental procedure used in this investigation, the alloys will be discussed in groups as separate quasibinary systems containing constant amounts of nickel. The systems considered contain 0, 1, 2, 3, 5, 10 and 20 per cent nickel. The straight copper-tin system was reinvestigated in order to establish a foundation on which to build the remaining material. The 1 per cent nickel alloys studied give the relations existing in the region of the eutectoid transformation between the copper-tin system and the 2 per cent nickel copper-tin system which has been investigated in detail. The thorough examination of the latter system was made since 2 per cent of nickel is representative of the commercial additions to the cast bronzes and also because it is sufficient to produce

Jan 1, 1932

By A. M. Gaudin

The study that is presented here was undertaken in order to condense information concerning comminution, and covering a great variety of conditions, into one or several rules which would be of use in the development of a systematic theory as well as in many directly practical ways. As the result of this work, the following conclusions appear justified: 1. Rocks may be classified, from the point of view of comminution, into two general classes which are (a) structurally homogeneous, and (b) structurally heterogenous. Structurally homogeneous rocks are those in which fracture takes place through grains and grain boundaries alike; heterogeneous rocks are those in which fracture passes in preference through grain boundaries. 2. If a sized product composed of structurally homogeneous rock grains is crushed, a product results in which the relation between the percentage weight of grains of various sizes and these sizes themselves follows a definite law. This is not true of structurally heterogeneous rocks. 3. Ball milling with structurally homogeneous rocks, and under certain conditions, presents exceptions to this rule. 4. In ball milling with structurally homogeneous rocks, there exists a critical ratio of size of feed to size of balls, above which the machine operates essentially by surface wear, and below which it operates essentially by breaking across the body of the particle. 5. In ball milling, with structurally homogeneous rocks, and when the size of feed grains exceeds the critical size, the particles worn off are of a substantially definite size which depends upon the ball size. 6. In the case of a typical heterogeneous rock, such as Manhattan schist, particles are crushed in such a way that there is a greater proportion of grains of the size that is the average grain-size of the rock than there would be in that range of size with a structurally homogeneous rock. This has been found to be true with all the crushers tested. 7. Different methods of crushing produce grains of different shapes. 8. The importance of sizing the — 200-mesh portion of a crushed product, in crushing-efficiency investigations, has been greatly under-

Jan 1, 1926

By C. O. Worden, C. A. Zapffe, F. K. Landgraf

SUMMARY FOLLOWING the discovery of Parke and Ham that deoxidation control of cast molybdenum can be predicated upon simple fractographic examination, a special study of that metal was undertaken to investigate those patterns ascribed to forgeability and nonforgeability. An elaborately developed system of cleavage patterns immediately rewarded the study; and they are reported here as a necessarily preliminary contribution calling attention to information which is both new in type and in origin. In general, the present observations confirm those of Parke and Ham, and Woodside; but they also disclose a wealth of detail and correlated phenomena which greatly expand the earlier information. For example, the oxide pattern of nonforgeability is found to be complex, perhaps involving as many as three distinctive patterns. And the nature of the carbide seems to be at least twofold. In addition, transgranular facets are here shown for the first time. Elaborately complex, but in a characteristic manner, these facets depict distortion in original crystal growth which provides truly extraordinary patterns. No carbide and oxide forms display themselves transgranularly, except in profile as exceedingly thin superficial films at the grain boundaries. Crystallographic features are also rare-a condition undoubtedly resulting from the great substructural distortion; but occasionally registrations are found of cleavage on {001}, and faulted areas believed to be Neumann-type deformation on {112}. INTRODUCTION Parke and Ham, 1 and again Woodside, 2 have reported that the forgeability of molybdenum cast by their vacuum-electric-arc process can be predicted with great dependability by a simple fractographic observation. They state that nonforgeability is the result of a grain boundary oxide which can be readily identified on the fracture facet at high magnification; and they convert the nonforgeable condition to a forgeable one by increasing the carbon content of the melt until the oxide structures subsequently observed in the fractograph become replaced by a second strongly marked pattern characteristic of carbide and coincidentally indicative of forgeability. Considerable importance immediately attaches to such observations: (I) because of their direct commercial application to one of metallurgy&apos;s inviting and relatively unexplored metals; (2) because of a general scientific curiosity regarding the nature of these characteristic markings; and (3) perhaps more important, because of

Jan 1, 1948

By H. S. Martin

ALTHOUGH it was known some years ago at the- Utah Copper Co. mills that fine grinding improved flotation recoveries, no accurate data were available until recently as to just how far the grinding could be carried economically. In 1923 the ultimate degree of fineness for flotation feed was supposed to be about 10 per cent. on 65 mesh, with approximately 55 per cent. through 200 mesh, which meant that most of the mineral would pass 100 mesh. At this time Garfield and Wilfley tables were used ahead of flotation and a good deal of the coarse mineral removed prior to the ball mill regrind. Shortly afterwards, mill-scale tests developed the fact that on a feed containing not over 10 per cent. +65¬mesh material flotation alone would give a copper recovery equal to that obtained by the combination of tables and flotation, but that on much coarser feed the recovery with flotation alone was lowered. This was at a time when all the sulfide minerals were floated if possible, so that the only requisite was to grind fine enough to free the mineral from gangue. EARLIEST USE op MICROSCOPIC EXAMINATION OF TAILINGS As early as 1921, the writer had attempted to determine by chemical analysis the relative proportions of copper minerals in tailings from an ore that made extremely poor flotation results. Chemical analysis was not satisfactory or conclusive, and samples of these tailings were sent to the U. S. Bureau of Mines Station at the University of Utah for micro-scopic examination. The question at that time was to determine, if possible, which copper minerals had been lost and why, but R. E. Head, in his report, revealed other interesting data. He said in part: Briefly stated, the mineral particles or grains may be classified into separate groups as follows: 1. Free grains of pyrite, chalcopyrite, chalcocite and bornite, respectively, which contain no other included sulfides; 2. Grains in which all three of the copper sulfides are represented (the core may he of chalcopyrite, partially altered to bornite, these two minerals being entirely surrounded by a shell of chalcocite); 3. Grains composed of equal amounts of bornite and chalcocite or chalcopyrite and chalcocite.

Jan 1, 1929

By H. A. Doerner

The process for smelting zinc developed several centuries ago is still in use. Through the experience accumulated over this long period of time, details of the process have been perfected until there is little opportunity to make any further improvement except by a radical change in method. Such a change was accomplished by the process recently developed by the New Jersey Zinc Co. The process to be herein discussed is a still more radical departure, which has been developed to large-scale laboratory operation by the Metallurgical Division of the U. 5. Bureau of Minesl. † The reduction of zinc oxide by carbon is a highly endothermic reaction, which requires temperatures in the range 1200° to 1400&apos; C. for even a slow reaction rate. The transfer of the heat of reaction through thick fire-clay walls, the high radiation loss in the type of furnace used, and the practical impossibility of recovering or using the combustible products of the reduction (CO) cause a deplorable waste of fuel. With the one exception mentioned, all zinc smelting is done in small retorts manually charged and discharged. Attempts to mechanize these operations have been only partly successful, and there seems to be no way to avoid or improve the uncomfortable conditions in which the work is done. The reduction of zinc oxide by methane has a relatively high reaction rate at 1000&apos; C. At this temperature most ore residues do not sinter, and it is possible to use metal retorts. These factors make gaseous reduction especially adapted to a continuous operation and compared to reduction by carbon make possible: (1) higher rate of reaction at lower temperature, (2) more nearly complete extraction of the zinc, and (3) much better utilization of fuel and reagent. Although the reaction between methane and zinc oxide requires 105,900 calories per mole, compared to 86,860 cal. in the carbon reduction, it is obvious that much less fuel will be required to supply 105,900 cal. through 36 in. of metal at 1000&apos; C. than to transfer 86,860 cal. through 1 in. of fire clay at 1300° C. Moreover, the gaseous products of gaseous reduction (CO and H2) can supply 183,430 cal. by complete combustion.

Jan 1, 1937

By Lyman Taylor, Alexander R. Troiano

STUDIES of the transformation of austenite at constant subcritical temperatures have been numerous since the work of Davenport and Bain.1 Considerable information has been obtained on low-alloy steels and on high-carbon alloys containing undissolved carbide or graphite at the austenitizing temperature. Little is known of the isothermal transformation of austenite containing in solution large amounts of both carbon and a single alloying element. In this investigation four steels containing one per cent carbon and with chromium in the range 3 to 9 per cent have been examined with the view to establishing the fundamental character of the isothermal reactions when all carbon and chromium are initially in solution in austenite. EXPERIMENTAL PROCEDURE Alloys The chemical compositions of the steels investigated are given in Table I. The 4 per cent Cr alloy is a commercial steel. The other steels were made by the Carpenter Steel Co. as 50-lb., induction-furnace heats and rolled to 5/8-in. round bars. Bars were softened at 650° to 700°C. before the specimens were cut. [ ] Metallographic Method Most of the lines on the transformation diagrams presented here have been placed on the basis of the microscopic examination of partially reacted specimens. Thees specimens were approximately ½ by ¼ by 1/8 in. in size. Specimens of the 9 per cent Cr steel were held 10 to 12 hr. at 1200° to I225°C. before quenching to the various subcritical temperatures. The other steels were held for 2 to 2 ½ hr. at 1200°C. before quenching. These treatments, carried out in an atmosphere of purified nitrogen, produced an austenite grain size larger than A.S.T.M. No. I, some grains being 1 to 2 mm. in diameter. There were a few undissolved carbide particles in some specimens of the 9 per cent Cr steel. It is believed, however, that any errors in the results due to incomplete solution of carbon and chromium in austenite are negligible; that is, austenite compositions may be considered as being those listed in Table I. X-ray Methods Constituents were identified and martensite axial ratios determined from Debye

Jan 1, 1945

By John T. Eash, Clair Upthegrove

During recent years nickel has had an increasingly important role as an alloying element in the copper-tin bronzes. Nickel additions not only produce better casting alloys but also make alloys whose properties can be varied by precipitation hardening; thus leading to increased commercial application of copper-nickel-tin alloys. Recent investigations have indicated a decrease in the solubility of tin in the alpha phase as the annealing temperature is lowered and as the nickel content is increased within certain limits. A further change caused by the nickel additions is produced in the excess phase of the copper-tin bronzes. The alpha plus delta eutectoid is replaced by a clear precipitated constituent in the alloys containing up to 15 per cent tin and not less than 1 per cent nickel. This paper has a dual purpose. The first is to present a new determination of the alpha-phase boundary in alloys containing from 0 to 20 per cent nickel, together with the liquidus and solidus temperatures above that field. The second purpose is to give the equilibrium conditions existing in alloys exceeding the alpha phase containing up to 31 per cent tin and 5 per cent nickel, so that the disappearance of the alpha plus delta eutectoid constituent may be explained. After considering the earlier investigations of the related alloy systems and the experimental procedure used in this investigation, the alloys will be discussed in groups as separate quasibinary systems containing constant amounts of nickel. The systems considered contain 0, 1, 2, 3, 5, 10 and 20 per cent nickel. The straight copper-tin system was reinvesti-gated in order to establish a foundation on which to build the remaining material. The 1 per cent nickel alloys studied give the relations existing in the region of the eutectoid transformation between the copper-tin system and the 2 per cent nickel copper-tin system which has been investigated in detail. The thorough examination of the latter system was made since 2 per cent of nickel is representative of the commercial additions to the cast bronzes and also because it is sufficient to produce

Jan 1, 1933

By R. E. McNulty, R. D. Heidenreich, C. H. Gerould

TIIE electron microscope techniques and their application to magnesium alloys that are to be discussed in this paper are the result of research at The Dow Chemical Co. over the past three years. The view- point underlying the work is not wholly metallurgical, but has evolved through a variety of problems related to the physics and chemistry of surfaces. It can be said that the interest and stimulus were closely associated with a desire to employ effectively the electron microscope in research concerning the properties of solids as related to their physical structure. Only a portion of this work will be described here, and, consequently, many points of interest and debate are of necessity either only briefly recognized or are completely omitted. As has been pointed out by Desch,1 a great deal of the knowledge of the structure of metals has been obtained through microscopic studies of the surfaces of metallic specimens prepared in a particular manner. This information, when added to that obtained by means of thermal, electrical, X-ray, dilatometric and other methods, has been of great value both from a theoretical and a practical view- point. With the introduction of new instruments such as the electron diffraction camera and the electron microscope, it would be expected that still more information could be obtained. These two instruments have in many instances been very effective when directed toward the investigation of metallic surfaces, provided the proper methods of surface preparation were employed. Experience shows that the problems of surface preparation greatly limit the general application of these instruments to metallographic studies. It was found necessary to discard the standard metallographic procedures in applying the electron microscope to magnesium alloys and to work out new methods, which were required to satisfy certain conditions. These methods are unique to magnesium only in the specific chemical reactions occurring during etching. The presentation of the methods and results will be ordered as follows: I. Electron Microscopy of Surfaces. 2. Surface Preparation of Magnesium Alloys. 3. Discussion of Microstructures. a. Pure Magnesium and Single-crystal Studies. b. Types of Precipitation. c. Some Common Structures. d. Special Micrographs and Techniques. e. Structure of Mg-A1 Solid Solutions. 4. Correlation of "Fine Structure" with Corrosion Behavior of Magnesium Alloys.

Jan 1, 1946

By T. Johnston, B. Cox

The results of oxidation and corrosion experiments on niobium in oxygen and steam at temperatures of 350° to 650°C, and in dilute sulphate solutions at 300°C are presented. The oxidation of niobium in oxygen can be explained in terms of a pre-transition period, which obeys an approximately parabolic rate law, and a post-transition period in which a more rapid linear rate is partially stifled by restriction of the gas flow due to the gvowth of the porous outer film. Due to changes in the porosity of the outer layers the restriction presented by the porous outel. film attains a limiting value. Subsequent oxidation obeys a linear rate law and shows an almost linear dependence of the rate on gas pressure. liltimately a second failure of the protective film may take place leading to a further acceleration in the oxidation rate. In water vapor the oxidation of niobium follows a parabolic rate law and does not show a transition to linear kinetics. The higher oxide, Nba05, was usually absent from the NbO/NbO2 film which was formed. The addition of a small partial pressure of oxygen to the water vapo3, resulted in accelerated oxidation according to the normal kinetics for oxidation in oxygen. The oxygen reacted preferentially with the niobium, and the protective oxide film was reformed when all the oxygen had been consumed. This behavior supports the theory that nucleation of Nb205 on the surface of the protective NbO/NbO2 film is the cause of the accelerated oxidation. After oxidation in steam at high-pressure Nb2Os was found in the protective film. The mode of formation of Nb2O5 under these conditions did not produce a change in kinetics, but was thought to explain the comparatively large dependence on pressure of the oxidation rate. The kinetics of oxidation in oxygenated aqueous solutions at 300°C were similar to those for oxidation in oxygen. A penetrating attack on niobium sheet may be related to the second breakaway observed by some investigators of oxidation in oxygen.

Jan 1, 1963

By I. Cornet

INTRODUCTION WITH the greatly expanding use of magnesium during the war, it appeared necessary to the War Metallurgy Committee that the notch sensitivity of magnesium alloy extrusions be further investigated and the influence of various factors upon notch sensitivity be noted. Accordingly, the National Defense Research Committee of the Office of Scientific Research and Development placed a research contract with the University of California, supervised by the War Metallurgy Committee. The work discussed herein was done under "Restricted" Project NRC-21, reported in Dec. 1943 1; it has been released for publication by the O.S.R.D. SCOPE OF THE INVESTIGATION The notch sensitivity of various magnesium alloy extrusions was determined under axial tension, and also under several conditions of nonaxial tension. Hardness, grain size and other metallographic features were observed; stress-strain data were obtained, and the chemical compositions of the alloys were determined, in order to correlate these quantities with the notch sensitivity. Notch sensitivity under axial tensile load was determined for a few specimens which had been cold worked to various degrees by tensile prestraining. Magnesium alloy extrusions studied included Dowmetal 0, X, J, and M. For comparison, extrusions of aluminum alloy 24S-T, cast bars of aluminum alloy I22-T2, and cast bars of magnesium alloy C were also tested, The specified chemical composition of these alloys is given in Table I. All bars tested were within specification limits of composition. Investigation of the tensile notch sensitivity of various magnesium alloy extrusions, under conditions of axial and eccentric load, showed little or no correlation with stress-strain or other conventional data. Since the many uncontrolled variables present might mask significant relationships, one alloy was selected for intensive study. Magnesium 0 alloy extrusions were subjected to experimental heat treatments, and the changing hardness, tensile strength, microstructure, and notch sensitivity observed. EXPERIMENTAL TECHNIQUES AND PROCEDURES Tensile Testing Bars used for axial loading were machined with 3/8 in.- and with 1/4-in. minimum diam, and included specimens with 6o° V notches (Fig I and 2). Each V-notched specimen was roughed out carefully and then finished with a honed tool. These V-notched bars were sampled frequently, sectioned, polished, and examined at 500 X magnification to control

Jan 1, 1948

By W. A. Anderson

Recrystallization of cold-worked metals has long been known to proceed by a process of nucleation and growth.&apos; When a cold-worked metal is heated to a temperature at which recrystallization will ensue, nuclei of new grains, essentially strain-free, appear and grow. As the process proceeds, nuclei continue to appear and to grow, until the cold-worked matrix has been entirely consumed and recrystallization has been completed (Fig. I). Conducted isothermally, a measurement of the fraction of the matrix recrystallized plotted against time, yields an isothermal recrystallization curve, showing the time course of the recrystallization process (Fig. 2).2 Evidently, then, the rate of recrystallization is determined by the rate at which nuclei form and the rate at which they grow. The rate of nucleation N is the number of nuclei that form in unit time in unit volume of the unrecrystallized matrix, and the rate of growth G is the increase in radius of the recrystallized grain per unit time. In recent years attempts have been made to determine N and G as these vary with the well-recognized variables affecting recrystallization: time, temperature, degree of deformation, etc.1 Such studies yield information that is more fundamental than that conveyed by the conventional recrystallization diagram,&apos; since the rate of recrvstallization is thus analyzed into its two component rates3 Methods are now available by which N and G can be measured, and analytical expressions have been developed for the interrelationships among N, G, the isothermal recrystallization curve, and the final grain size, which greatly facilitate analysis.2-4 The application of these methods has been demonstrated recently for the recrystallization of silicon ferrite.2 Data on N and G in dependence upon the recognized recrystallization variables are, however, very fragmentary;" values of N and G have been determined for some metals, but the effect of temperature, which would yield the fundamentally important activation energies, has been too little studied. Thus far there has been no detailed study of the recrystallization of any one metal in terms of X and G ovcr appreciable ranges of the variables time, temperature, degree of deformation, and original grain size. It is the purpose of the present paper to provide such a study, employing aluminum.

Jan 1, 1945

By M. H. Loveman

The orebody described below has been rediscovered and developed within the last 3 years. It has, however, been known and worked by the Chinese for hundreds of years. When assay values and size are considered, it contains what is probably one of the largest single bodies of zinc and lead sulphides yet found. The tonnages developed at other places, as at Broken Hill, are much greater but the average zinc and lead sulphide contents are considerably lower than at Bawdwin. Bawdwin is situated in the semi-independent State of Tawng Peng, one of the numerous units which make up the Northern Shan States. These States are under British rule and are generally considered as a portion of Burma. They are governed as a separate administrative unit, however, under the Lieutenant Governor of Burma. Each State is under its own chief, or Sawbwa, who has considerable power over his own subjects. Bawdwin is approximately in latitude N 23°6&apos;, longitude E 97°201, about 50 miles south of the nearest point on the Chinese border and 450 miles north of Rangoon (Fig. 1). The period at which mining was first begun at Bawdwin is unknown. The most reliable records have been obtained by deciphering local Chinese inscriptions and from these it is concluded that the work dates back to at least the beginning of the 15th century. The first undoubted reference to the mines by a European is by Syrnes in 1795. Crawford in 1827 estimated the output of silver from the mines at $600,000 anually. At about the middle of the 19th century the rebellion of the Chinese Mohammedans in the neighboring Chinese province of Yunnan so weakened the power of the Chinese that the incursions of hostile tribes (Kachins) made work extremely dangerous. The mines were finally abandoned by the Chinese about 1868. The . closing down of the mines was probably not entirely due to outside causes but may have been influenced somewhat by the increasing difficulty of handling the water, as the workings gradually descended below the water level of the district. Several attempts were made by the Burmese kings, Mindon Min and Thebaw, to resume operations, but because of a

Jan 1, 1917

By G. F. Loughlin

MORE than 20 years have passed since the publication of Lindgren and Ransome&apos;s report on the Cripple Creek District,1 which was made when the district was much more active and prosperous than in recent years. They concluded that the output of the district, which had reached its maximum of about $18,200,000 in 1900, would gradually decline, and their conclusion has been confirmed by records of subsequent production. Between 1905 and 1915 annual declines were partly compensated by encouraging increases, especially in 1908, 1914, and 1915; but a rapid continuous decline followed, due largely to the war and its after effects, until in 1922 the value of output was only slightly more than $4,000,000. It rose to nearly $5,000,000 in 1924, but declined again in 1925 and in 1926, when it was about $4,400,000, and represented ores mainly from deep levels in the Cresson and Portland mines. The profitable operations of these two mines were the principal factors leading to a study of ore at deep levels in the district by the U. S. Geological Survey in coopera-tion with the Colorado Metal Mining Fund. The principal reasons for Lindgren and Ransome&apos;s conclusion were three: (1) the greater cost and difficulty of deep exploration; (2) the decrease in the number of veins with increasing depth, and (3) the probability that the telluride ore, believed to have formed at comparatively low temperature, would not persist indefinitely -in depth. Operations since they made these statements have verified the first two, but call for some modification of the third. Rich telluride, ore is being mined at a profit in the Portland mine 3000 ft. below the present surface, or 5000 ft. below the original surface of the Cripple Creek volcano, as interpreted by Lindgren and Ransome. The question arises, therefore, as to the number and extent of such deep deposits, and the answer, so far as it can now be given, must be based mainly on structural data, supplemented by data on the processes of ore deposition. Presentation of these data based on a study of deep mines in the southeast quarter of the district, the only

Jan 1, 1927

By E. P. Pfleider, D. H. Yardley

Layers of magnetic taconite of above average magnetic iron content extend down dip on the Mesabi Range to depths beyond the reach of open pit mining. A selected layer with thickness of 75 to 100 ft underlies many square miles. Such a selected layer can provide over 50 million tons of recoverable concentratc per square mile, at lower concentration ratios than in the present open pit taconite operations. The system contemplated would consist of large scale underground quarrying by a lane and pillar method. Working heights would be 60 to 100 ft; room widths, 50 to 75 ft; and productivity targets, about 40 tons per man-shift. The most critical problems would he roof control and blasthole drilling. The successful operation of large open pits and concentrating plants for treatment of magnetic taconites indicates that the basic techniques and economic problems of pellet production have been solved. The open pit reserves are large, but they are not necessarily available in sufficient quantity or quality to provide an adequate raw materials base for all potential producers. Furthermore, as the more easily available open pit crudes are used up, the pits will become deeper, stripping costs per ton of concentrate will increase, and recoveries will decrease as leaner crudes are utilized. The time will come when supplementary and replacement reserves of magnetic taconite will be required. One way these can be obtained is by underground mining of the down-dip extension of the Mesabi magnetic taconites, especially those layers averaging well over 25% recoverable iron. A key point in such a proposal is the possibility of realizing substantial savings by beneficiating an ore of 30% magnetic iron at 2.5 to 1 ratio of concentration. This contrasts with current practice in Mesabi commercial taconite plants, where the ore averages 22 to 25% magnetic Fe, with concentration ratios of about 3.0 when producing 61% Fe pellets. Two factors which favor the eventual development of underground taconite mining are: 1) the desirable physical structure and high grade of taconite pellets in general and 2) the improved engineering techniques in underground mining. Experience in large scale room and pillar mines demonstrates that, given strong rock strata immediately above a high grade mining

Jan 1, 1963

THE slag performs two useful functions in open-hearth steel- making. First, it is the means of disposal of all the impurities, save carbon, which are removed from the charge materials in refining the steel, so it must be suited to receiving and retaining as much as possible of undesirable elements with minimum loss of iron and useful alloying elements. Second, the slag serves as a buffer between the flame and the bath and transfers oxygen to the metal at a measured pace contrasted with the violent and difficultly controlled oxidation of the bessemer process. At the same time, the slag is a thermal insulator that limits the rate at which heat can be delivered to the metal from the flame, and a heavy slag blanket thereby serves as a brake on production rates. It has been said with justification that the secret of good steel- making is to make a good slag and the steel will take care of itself. In a broad sense, the subject of slag control includes not only the adjustment of the composition of the slag but also of its relative weight in terms of percentage of the metal-bath weight. The slag is made up essentially of: (1) oxides formed by oxidation of silicon, manganese, phosphorus, and iron in the charge, (2) Si02, MnO, MgO, and other oxides charged as such or introduced incidentally with ores or fluxes or by refractory erosion, and (3) lime charged or fed to the heat to neutralize the "acidic" oxides present (Si02 and P205). Obviously, if practically perfect control were possible over the composition of the charge as well as over the oxidation process during the melting period, both slag weight and composition would be very nearly predetermined; and the control problem would be solved. Unfortunately, only a somewhat imperfect control over these factors is possible, so the operator must begin during the lime boil and continue through the refining period to discover and correct departures from the normal pattern of slag development. To do this as the heat progresses, the first helper must be able to make quick estimates of the composition and physical state of develop-

Jan 1, 1964