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By R. W. Fountain, W. D. Forgeng, G. M. Faulring

Precipitation of the phase Co3Ti (Cu3Au type) from a Co-5 pct Ti a11oy has been investigated using single-crystal X-ray diffraction techniques. Oscillation and transmission Laue patterns of specimens aged for short-time periods at 600" C indicate the formation of titanium-rich and titanium-poor zones coherent with the {100} matrix planes. Longer aging times at 600° C establish that the equilibrium phase also forms on the {100} matrix planes as platelets. These observations are corroborated by electron metallography; electron diffraction studies show the phase Co3Ti to be ordered. A probable sequence of the precipitation reaction is discussed. A previous publication by two of the present authors reported on the phase relations and precipitation in Co-Ti alloys containing up to 30 pct Ti.1 The results of this investigation established the existence of a new face-centered cubic inter metallic phase, ranging in composition from about 17.0 to 21.7 pct Ti at temperatures below 1000° C The decomposition of the fcc supersaturated solid solution was studied employing hardness and electrical resistivity measurements. The changes in hardness upon precipitation in alloys containing 3, 6, and 9 pct* Ti were found to be associated with an initial increase in hardness followed by a plateau and then a second, more pronounced hardness increase. Investigation of this behavior by electrical resistivity measurements suggested that two different kinetic processes were involved, which, when interpreted in terms of the kinetic relation,2-4 indicated that initial precipitation was in the form of thin plates. On continued aging, the plates impinged during the growth process. The general features of these findings have been confirmed by Bibring and Manenc,5 while, in addition, they report the phase to be ordered. The present investigation was undertaken to provide more definite information on the structural relationships between the precipitate and the matrix. EXPERIMENTAL PROCEDURE Single crystals of a (20-5 pct Ti alloy were prepared from the melt employing the Bridgman technique. Poly crystalline rod, 1/2 in. in diam, prepared from vacuum-melted material, was machined to 3/8- in. diam to remove any surface contamination that may have resulted from hot-working. The crystals were grown under a purified hydrogen atmosphere in high-purity alumina crucibles heated by induction. Considerable difficulty was encountered in attempting to grow monocrystals because of the high melting point of the alloy and the high solute concentration. However, one crystal about 6 in. long was obtained which was essentially a single crystal except for one or two very small grains around the periphery. The as-grown crystal was solution heat-treated for 24 hr at 1200°Cin a purified argon atmosphere and water-quenched. One-quarter-in. slices were taken from each end of the solution heat-treated crystal for chemical analyses, and the remainder of the crystal was mounted and oriented by the back reflection Laue Method. The chemical analysis of the crystal was as follows: Pct Ti Pct 0 Pct C Pct N Pct H Pet CO 5.29 0.08 0.004 0.002 0.0003 Balance By proper tilting of the crystal, it was possible to obtain slices 1/32 in. thick of [loo] and [110] orientation. The solution heat-treated crystal slices were sealed in silica capsules for the aging treatments, with titanium sponge placed at one end of the capsule to act as a getter. All slices were water-quenched from the aging temperatures, the capsules being broken under the water to ensure a rapid quench. Thinning of the slices for transmission X-ray studies was accomplished by a combination of mechanical and electrolytic techniques, the final thickness being about 0.1 mm. Laue patterns of the solution heat-treated crystal indicated that no strain was introduced by the thinning technique. ELECTRON METALLOGRAPHY After X-ray examination, the structural changes attending the precipitation were followed by examination of direct carbon replicas of polished and etched surfaces of the single-crystal slices and extracted phases. The earliest indication of significant structural change was observed after aging at 600°C The structure of a heavily etched, solution-treated crystal is shown in Fig. l(a). Aside from the etch pit pattern, no regularity of background structure is observed. On the other hand, in the background of the specimen heated for 500 hr at 600°C, the etching pattern shows a directionality indicating the influence of minute precipitate particles, Fig. l(b). On electrolytic dissolution of this specimen in 10 pct HC1 in alcohol, a large volume of very small, flattened cubes

Jan 1, 1962

By C. Wayne Burnham

Much has been written about hydrothermal alteration and the compositional changes induced by it in the wallrocks of mineral deposits, especially in alummino-silicate wallrocks. So much has been written and the descriptions so varied, in fact, that the casual reader frequently is bewildered by the extreme complexities and lack of uniformity, real or apparent. Certainly the mineralogy and chemistry of altered rocks are not as simple as most of us would like, but neither are they as complex in their principal aspects as pa of what has been written would lead us to believe. The trend until recently seems to have been toward greater complexity and hence greater confusion, but the straightforward presentation of Creasey (1959), it is hoped, marks a reversal in this trend.

Jan 1, 1962

By W. A. McKinney

The segregation process consists of heating crushed oxidized or mixed oxide-sulfide copper are with a copper-volatilizing salt and carbonaceous material at about 750° C. to produce metallic copper which is recovered from the furnace calcines by conventional sulfide flotation. The Bureau of Mines made a number of bench-scale laboratory tests on two copper ores to determine the relative merits of using halogen salts, potassium chlorate, or various salt mixtures as volatilizing agents in segregation of the copper. Laboratory investigation of typical siliceous and calcareous oxidized ores revealed that sodium chloride was a better segregating agent than the other salts. Calcium chloride, magnesium chloride, sodium fluoride, or potassium chlorate gave nearly as good segregation as the sodium chloride on the siliceous ore. Segregation of the calcareous ore with calcium chloride was nearly as good as that obtained with sodium chloride, but inferior segregation resulted when magnesium chloride, sodium bromide, or potassium chlorate was employed. The use of sodium bromide or sodium iodide on the siliceous ore, and of sodium fluoride or sodium iodide on the calcareous are, gave appreciably poorer segregation than sodium chloride or the other salts. Other tests of the ores, using mixtures of sodium chloride and the other halogen salts or potassium chlorate, gave segregation approaching that obtained with sodium chloride.

Jan 1, 1962

By W. W. Weller

This report provides low-temperature heat-capacity data and entropies at 298.15° K. for magnesium metavanadate (MgV206) and magnesium pyrovanadate (Mg2V207). The work completes low-temperature measurements planned for alkaline-earth vanadates; an earlier report dealt with calcium vanadates.4 No similar data for these compounds have been published previously. Free energy of formation values at 298.15° K. were derived by combination of the present entropy values with heat of formation data. MATERIALS The materials used in the measurements were portions of the samples described in a previous Bureau of Mines publication by King, Koehler and Adami.5 Methods of preparation, chemical analyses, and X-ray examinations are covered in this paper. The indicated purity of the samples was 99.9 pct.

Jan 1, 1962

By R. W. Heckel

A method is described whereby the relationship of both the "at-pressure" powder compact density and the "zero-pressure" compact density to the applied pressure may be obtained from continuous measurements of punch movement during a single compaction operation. The rate of density increase with applied pressure for the metal powders is found to be proportional to the volume fraction of pores for pressures exceeding a lower limit which varies from 15,000 to 30,000 psi, depending on the powder. 1 HE compaction of powdered materials is carried out primarily to increase the density of the material. If the ultimate goal of the over-all process is the attainment of minimum porosity, compaction is responsible for most of the densification. For example, loose powdered metals have porosities of about 65 to 75 pct. Axial loading in a die or hydrostatic pressure may effectively reduce the porosity of most powders to 20 pct or lower with pressures of 50,000 psi and greater. The relationship between the density of a powder compact and the pressure needed to achieve that density is most commonly obtained by pressing several compacts, each at a different pressure. Measurement of the densities of the individual compacts when they are removed from the die then provides the density-pressure relationship. However, this method suffers from several disadvantages. Because a large number of compacts and pressing operations are required, it is inherently slow. Furthermore, since density measurements are made after the specimens are removed from the die, data obtained refer only to pressures greater than those necessary to form a coherent compact. The third disadvantage is the inability of this method to provide information about the compact density at the applied pressure in the die. Because the determination of density-pressure relationships has been a slow, tedious process, investigators have sought to express the compaction behavior of powders by other means. The general terms "comparability" and L'compressibility" have been used to rank powders qualitatively according to their compaction characteristics. To restore a quantitative nature to the subject and to prevent confusion, Schwarzkopf1 has proposed that compac-tibility be defined as the minimum pressure needed to produce a given green strength, while compressibility should be used to indicate the extent to which the density of a powder is increased by a given pressure. Probably the most widely used of the compaction parameters is the "compression ratio,'' which is generally defined as the ratio of the compact density obtained by pressing at a given pressure to the apparent density of the loose powder.2 However, the description of the compaction behavior of a powder by these parameters provides only limited information about the process because of their applicability to just one specific condition such as a given green strength or a given pressure. The method of obtaining density-pressure relationships which will be described in the present paper was designed to eliminate the shortcomings of the previous techniques while maintaining equivalent accuracy and precision. EXPERIMENTAL TECHNIQUES The general principle employed makes use of the fact that the linear movement of the punch during a

Jan 1, 1962

By J. C. Uy, A. A. Burr

IN the primary solid solutions of zirconium-base alloys, there is a striking regularity of the effect of solute valence on the stabilization of the allotropic phases.1 The valences derived by pauling2 are for elements as they are bonded in the solid metallic state. Effects of variations in isotopes, alloying elements, and allotropes on their valences are difficult to determine and such data are presently unavailable. Pauling's values are somewhat empirical and approximate, but if some definite correlations can be found between those values and experimental observations, this will lend support to the tacit assumption that the possible variations in valence mentioned above are small. Pauling has amassed a large amount of evidence of such correlations. It is the purpose of this technical note to show another application of the Pauling valences and to offer a possible explanation for this observation. The relationship between the Pauling metallic valence of the solute and the stabilization of allotropic phases in zirconium is shown in Table I, which has been compiled from available data in the literature3 plus the results of work done at Rens-selaer Polvtechnic Institute.' The chemical valences are included for comparison. It can be seen that a solute whose metallic valence is lower than that of the solvent tends to stabilize the a phase while one whose metallic valence is higher than that of the solvent tends to stabilize the 0 phase. It should be noted that, inasmuch as the Pauling valences are periodic with atomic number, this is tantamount to saying that the elements in groups I-A, 11-A, III-A, III-B, IV-B, V-B, and VI-B are a stabilizers while those in groups IV-A, V-A, VI-A, VII-A, VIII-A, I-B, and 11-B are ß stabilizers. The chemical valences do not show such consistency. Although the zirconium-rich end of the Zr-Au diagram is not available, it call be expected that gold, having a metallic valence of 5.56, would stabilize the ß phase. At absolute zero, the Fermi energy level is the criterion of equilibrium, i.e., the structure having the lower Fermi level will be more stable. Conse- quently, allotropic transformation occurs in a metal when thermal excitation raises the Fermi level to a point at which the atoms can be better accomodated by a different structure which yields a lower Fermi level.4-6 Thus in allotropic transformation, a change in structure occurs as a result of the change in the energies of the bonding electrons. Since the Pauling valence is the number of bonding electrons per atom, and these are the only electrons whose energies are affected by thermal excitation,* it can be inferred that the introduction of a solute which has a higher Pauling valence than that of the solvent raises the initial Fermi level; consequently, the transformation temperature is lowered. The converse is also true. The fact that at the transformation temperatures this statement is still fairly valid implies that the contribution due to the difference in specific heat terms of the two allotropes is comparatively small.

Jan 1, 1962

With the exeption of the United States, Canada and Russia, oil has not been around in quantity near world centres of population. Production: in Western Europe is insignificant. Japan is without production as are Australia, Southern Africa, India; Brazil, Chile, New Zealand and China. The United States is, however, a large importer of crude oil. The very fact that oil is produced generally away from centres of population means that it has to be carried by sea to the area in which it is required. There is, therefore, a constant flow of oil around the world in very definite channels.

Jan 1, 1962

By J. P. Wiser

THIS paper discusses testing and quality control of milled asbestos fibre. It has been composed with the intention of: (I) Summarizing past, present and probable future methods of testing and classifying the various grades of commercial asbestos produced by the Quebec asbestos industry. (2) Acquainting those unfamiliar with the methods used for evaluating, testing and controlling the grading and the quality of Quebec chrysotile asbestos fibres with some of the physical and chemical procedures currently used for that purpose. (3) Discussing some of the complications facing the producers, such as variations in the orebody and special requirements of asbestos manufacturers. ( 4) Detailing some of the present quality control methods. SUMMARY OF PAST, PRESENT AND PROBABLE FUTURE TESTING METHODS Past During the first years of production of commercial asbestos in the Province of Quebec, fibre testing and quality control were based principally on dry screen analysis and visual inspection. These methods were gradually expanded during the period from 18, 90 to 1932. In 1932, standardization

Jan 1, 1962

By John H. Schemel

Large Zircaloy-2 hammer or press forged bars did not exhibit the uniform excellent corrosion resistance to steam normally expected of the alloy in wrought form. Weight gains of coupons cut from forged bars were 40 to 60 mg per sq dm compared to the 28 mg per sq dm obtained on hot rolled sheet and strip. The mechanism of this corrosion and its relation to microstructure is discussed. After these observations, a solution heat treatment followed by rapid cooling was tried on coupons from eight heats of forged bars. The basket-weave structure resulting from the quench did not show agglomeration of intermetallic compounds. These coupons showed uniformly good corrosion resistance with weight gains very close to the 28 mg per sq dm expected of Zircaloy-2 after the 14-day steam test. A large forging was solution heat-treated and tested for structure, mechanical properties, and corrosion resistance. Corrosion resistance was excellent and uniform throughout the section. The normally anisotropic mechanical properties were changed to completely iso-tropic. Strength levels were raised while there was a small loss in ductility at the service temperature. Tempering of the quenched structure below the ß transus did not improve the ductility at the test temperature of 600°F. ZIRCALOY-2 end caps for nuclear fuel elements Zircaloy-2 is an alloy of 1.5 pct Sn, 0.1 pct Fe, 0.1 pct Cr, and 0.05 pct Ni, balance hafnium-free zirconium patented by Westing-house Electric Co. used in pressurized water reactors are machined from large hammer-finished forged bars. The bars forged for this application range from 3 1/2 in. to 7 1/2 in. squares. One of the tests used to evaluate Zircaloy-2 for this service is a 14-day exposure to very high-purity steam at 75oF and 1500 psi pressure. Normally wrought products will exhibit a black lustrous film of zirconium oxide after the test and show a weight gain of approximately 28 mg per sq dm. Coupons representing the forged bars exhibited a wide variety of corrosion results ranging from acceptable black coupons to some covered with white crystals of zirconium oxide that had weight gains of nearly 100 mg per sq dm. One of the most common effects was a white corrosion product that looked like a stain to some observers and the outline of massive metal grains to others. Very careful specimen preparation prior to the corrosion test did not affect the result and metallographic examination did not reveal a structural feature of a size and shape that would correlate with the corrosion product. In addition to the relatively poor corrosion resistance, the forged product was not as ductile as desired. The problem of obtaining uniform and more acceptable properties in these heavy-forged sections seemed to be a function of the microstructure of the metal and, in particular, the distribution of the intermetallic compounds. None of the four alloying elements however are appreciably soluble in a zirconium and are present as compounds which usually appear scattered randomly throughout the structure. Moudryl showed that the distribution of these intermetallic compounds in Zircaloy could be related to a ostringero corrosion failure. Grozier et al. discussed another structural defect that causes a similar corrosion effect. In this case, an elongated gas-void was determined to be the cause. M. L. Picklesimer held in his discussion of the Grozier paper that at least a part of the observed =stringersn were caused by the distribution of the intermetallic compounds. He proposed a

Jan 1, 1962

By Thomas M. Garland

Reports that set forth the pertinent facts of existing secondary-recovery operations are an integral part of the work of the Bureau of Mines in promoting conservation and efficient utilization of the petroleum resources of the Nation. Knowledge of the success or failure of waterflood projects in an area is very useful to other operators. Although projects will not have identical results, information concerning the flood performance, method of operation, and difficulties encountered on one project will help operators to determine the feasibility of flooding a similar sand and to select the methods of operation most likely to prove successful. The increasing cost of discovering and developing new oil reserves, as well as the unending effort to reduce operating costs and increase ultimate oil recovery from known petroleum reservoirs, has required the petroleum industry to evaluate continuously the performances of various secondary-recovery methods. Waterflooding was recognized early by the petroleum industry as a possible means of increasing oil recovery. From the early accidental floods in Pennsylvania and through many haphazard attempts to inject eater into oil-bearing formations, waterflooding emerged as one of the more important methods of oil recovery. Waterflooding is important not only to the oil industry but also to the economy of the area concerned.

Jan 1, 1962

By John D. Roach

DURING an investigation of the yttrium-hydrogen system aimed at producing solid yttrium hydride specimens containing various amounts of hydrogen, it was observed that yttrium containing approximately 2 wt pct H exhibited a tendency to crack and crumble to a powder on standing in air at room temperature. It was also observed that longer hydriding times, at a given temperature, increased this susceptibility to powdering without an increase in hydrogen content, also that moisture in the air is necessary for the observed effects to occur. Even if cracking did not occur, there was a continual formation of a light gray powder on the as-treated surface of the hydrided yttrium and this reaction continues until the entire hydrided piece has been reduced to a powder. Storing the hydrided specimens in the absence of air or removing the surface either by machining or grinding were effective means of preventing this disintegration of hydrided yttrium. In an attempt to determine the reason for this powdering phenomenon, the surfaces of a number of as-hydrided yttrium specimens were examined by X-ray techniques. In all cases the X-ray pattern obtained showed the major phase to be yttrium hydride (YH2) as would be expected since the specimens contained 2 to 2.2 wt pct H. In some cases a trace of yttrium oxide was observed. There was also a third phase present on the surface of these hydrided specimens which could not immediately be identified. This unknown phase was a face-centered cubic material, NaC1-type structure, with a lattice parameter of 4.855 and a calculated density of 5.914 g per cc. Very slight hand polishing of the surface of the hydrided yttrium specimens completely removed both the unknown phase and the traces of oxide so that only the yttrium hydride pattern remained. Based on the X-ray patterns the quantity of the unknown phase on the surface of the hydrided yttrium appeared to be directly related to the susceptibility of the material to powdering. Work at the Denver Research Institute on the yttrium-nitrogen binary system showed that yttrium nitride (YN) is a face-centered cubic material with a lattice parameter of 4.878A and a density of 5.890 g per cc. They also noted that this compound rapidly disintegrated to a powder on standing in air. The unknown pattern observed in the above specimens corresponds very closely to that of the nitride—fcc structure, 4.885 parameter, and density of 5.914 g per cc. The presence of this thin film of nitride on the surface of the hydrided specimens probably accounts for the observed powder formation and crumbling. The nitride reacts with the water vapor in the air (verified by private communication from Dr. C. Huffine, General Electric Co.) to yield yttrium oxide and ammonia. Ammonia is readily detected when hydrided yttrium specimens were allowed to stand in bottled moist air. The powder formed on the surface of the hydrided specimens was shown by X-ray analysis to be yttrium oxide. This reaction appears to occur primarily at the grain boundaries since discrete particles of yttrium hydride separate from the specimens during this powdering process. The reaction of yttrium nitride with water vapor is believed to be as follows: 2YN + 3H2O - Y203 + 2NH3. Despite the fact that this nitride is present only as an extremely thin surface film, if the above reaction is not prevented by removing this film from the surface either by machining or grinding, the reaction continues until the entire hydrided piece has been reduced to a powder. To account for this continuation of the reaction, it is believed that the following reactionalsooccurs: 2YH2 + 2NH3 -2YN + 5H2. The nitride produced by the latter reaction reacts in turn with water vapor. The reaction therefore becomes autocatalytic and continues until the hydride has been consumed and the entire piece reduced to oxide powder. The amount of nitride required to initiate this reaction is quite small and this nitrogen contamination can occur from a number of sources—hydrogen gas employed, minute leak in the hydriding apparatus or even from degassing of the reaction vessel itself. Longer hydriding times increase the possibility of nitrogen contamination and this is especially true when a dynamic gas system is employed in the hydriding process. The production of stable, solid hydrided yttrium is dependent on the complete absence of nitrogen contamination during processing. If such contamination does occur, powdering of the hydrided product can be prevented by removing the nitride from the surface e.g. grinding or by preventing access of air to the pieces e.g. sealing in wax or plastic. The author wishes to express his appreciation to General Electric Co. for sponsoring this research and for permission to publish the results of work under Subcontract AT-93.

Jan 1, 1962

By D. I. Cameron

A graphical method has been developed and tested for separating the effects of grain boundary and lattice diffusion in polycrystalline materials. The method is based on the assumptions that for unidirectional diffusion from a plane source of radioactive material, the penetration of activity far into the specimen from the source is due solely to grain-boundary effects, and 2) pure grain-boundary penetration is described by a linear plot of log activity vs the perpendicular distance x from the source. The former is based on the fact that at any temperature the grain-boundary diffusion coefficient is always very large relative to the lattice diffusion coefficient; and the latter is based on the derivation of Fisher.1 Using these criteria along with appropriate penetration data (in this case, data for the diffusion of Cb95 in pressed and sintered UO2) one first plots the data as log activity vs x2 and as log activity vs x, as shown by curves 1 and 2, respectively, in Fig. 1. A tangent line to curve 2 for large x (curve 3) is then transferred to the x2 plot as curve 4. The subtraction of curve 4 from curve 1 yields curve 5 which represents only lattice diffusion and may therefore be related to the diffusion coefficient by using the appropriate solution to Fick's second law. It should be noted that the method has inherent inaccuracies for small and large values of x2 and only the subtraction at intermediate values can be used. For the illustrated specimen the calculated diffusion coefficient is 3.4 X 10-11 sq cm per sec at 1445°C while data using a single crystal of UO2 at the same temperature yielded a value of 2.9 x 10-11 sq cm per sec.2 The same method of subtracting grain-boundary diffusion effects to obtain lattice diffusion coefficients has been successfully used to determine self-diffusion coefficients of Th230 in polycrystal- line thoria.

Jan 1, 1962

By R. V. Lundquist

The work described in this report, part of the Bureau of Mines long-range program to develop methods of utilizing submarginal domestic sources of aluminum, was undertaken to investigate the effects of iron in the lime soda sinter process, The approximate Fe2O3 content in a sinter for maximum alumina and soda recovery was 8 to 9 percent. Fe2O3 appears to inhibit gelation, and 15.5 percent Fe2O3 produces effects similar to those produced by 1 percent sucrose. In the lime soda sinter process, aluminum silicates are sintered with limestone and soda ash to yield dicalcium silicate and sodium aluminate. The sodium aluminate is extracted by leaching in caustic solution. The solution is purified by heating in an autoclave with lime to remove silica, and alumina trihydrate is precipitated with carbon dioxide. The reactions involved in sintering and leaching are complex. A number of studies by the Bureau of Mines4-9 and others1 indicate that the iron content of sinters influenced the recovery of alumina and soda and the gelation characteristics.

Jan 1, 1962

By Norman Brown

It is suggested that the difference in ease of cross-slip among the fcc metals determines the relative amounts of [111] and [100] wire texture which occur in each metal. Since the ease of cross-slip is controlled by the stacking fault energy, it turns out that the amount of [111] texture should increase as the stacking fault energy increases. Arguments and existing data are presented to support the above suggestion. THE fcc metals generally have a dual texture, [11 and [loo], after wire drawing. As yet no fundament explanation exists concerning the variation of the amounts of each texture among the metals. Barrett&apos; has compiled data which show how the relative amounts of each texture vary from 100 pct [Ill] in the case of aluminum to 25 pct [l1] for silver. In this paper it is suggested that the value of stacking fault energy plays a major part in determining the amount of each type of texture. The double texture has its origin in the classical rotation of a single crystal under tension. An equilibrium position of the crystal is one in which three or more equivalent slip systems are operating simu taneously. Most crystals, initially, tend to rotate toward the [1ll] or the [l00] pole depending upon its initial orientation. This single-crystal behavior is essentially the same as the rotational behavior of the polycrystalline metal as worked out by Taylor.2 The next point to consider is whether the [Ill] or [100] orientation is more stable. There have been many discussions of this question3&apos;" which, in general, have lead to the conclusion that 11111 is most stable. For example, Pickus and Mathewson 4 suggested that a [Ill] texture produces more effective flow becake the [ 110] slip direction makes a smaller angle with the [111] than with the [loo]. A crude statistical argument will be presented which again favors the (1111 orientation. In order to maintain a pure [loo] wire texure, slip must occur in equal proportions in four of the six possible <110>slip directions. In order to maintain a pure [Ill] texture, slip must occur in equal proportions in only three of the six <110>directions. Since the <110> directions are the only slip directions in a fcc metal and if it is assumed that each of these six directions is equally probable, then the relative probability of a [1ll] texture vs a [l00] texture may be calculated. The statistical weight of a particular texture is the multiplicity of a texture times the probability of obtaining any one. The statistical weight for [Ill] is

Jan 1, 1962

By A. Szirmae, Hsun Hu

The early stages of recrystallization in a 70 pct cold-rolled Si-Fe crystal of the (110) (0011) orientation were studied with a Siemens electron microscope. Orientation studies based on electron-diffractzotz. patterns confirm the results of previous texture analysis. The driving energy for recrystallizatior and the critical radius for growth were calculated from the dislocation energy and the energy of the subgrain bourzdaries, and it was found consistent with the observed size of the recrystallized grains. The recrystallization characteristics of crystals with different initial orientations are discussed. The recrystallization of cold-rolled (110)[001] crystals of Si-Fe has been widely studied by various investigators.1-4 Their results on both deformation and annealing textures are in good agreement. The rolling texture after 70 pct reduction consists mainly of two crystallographically equivalent (111) [112] type textures and a minor component of the (100) [011] type. The latter is derived from the deformation twins, or Neumann bands, which are formed during the early stages of deformation and later rotate to the (100) [011] orientation upon further rolling reduction. Between the two main (111) [112] type textures, there is some orientation spread, because of which very low intensity areas appear in the pole figure. If these very low intensity areas are considered to be a very weak component in the texture, then a (110) [ 001 ] orientation may be assigned to them. When this rolled crystal is annealed at a sufficiently high temperature for recrystallization, the texture returns to a simple (110) [001]. The purpose of the present investigation was primarily to seek a better understanding of the recrystallization process by using the electron transmission technique. The (110) [0011 type of crystal was selected because orientation data for it are well known from previous studies with conventional techniques. Direct observations on the recrystallization of such a crystal have also been made by using a hot-stage inside the electron microscope, and the results will be reported in another paper. MATERIAL AND METHOD A single-crystal strip of the (110) [001] orientation was prepared from a commercial grade 3 pct Si-Fe alloy by the strain-anneal technique.= The strip was approximately 0.014 in. thick, and was rolled 70 pct at room temperature to a thickness of 0.004 in. Specimens were cut from the rolled strip and were annealed in a purified hydrogen or argon atmosphere. They were then electrolytically polished in a chromic-acetic acid solution to very thin foils. Best results were found by polishing first between two narrowly spaced flat cathodes with the specimen edges coated with acid-resisting paint, followed by polishing between two pointed electrodes until a hole appeared in the center as described by Bollmann.6 It was found that a thin transparent film always formed along the thin edges of the polished specimen. This film was then removed by rinsing the specimen very briefly in a solution of alcohol with a few drops of HF or HCl. RESULTS AND DISCUSSION 1) The Deformed Crystal. From the electron-diffraction patterns taken at various areas of an as-rolled specimen, the texture components as deduced - from ordinary pole-figure analysis were confirmed. Over most of the areas where orientation was examined, a (111) pattern with a [112] direction parallel to the rolling direction was obtained. This corresponds to the main deformation texture of the (111) [112] type. In a few areas the diffraction pattern was (100) [Oil], corresponding to the minor-texture component derived from the Neumann bands. The (110) [001] orientation, which corresponds to the very weak intensity area in the pole figure, was found infrequently. A typical example of the deformed matrix having the (111) type main texture is shown in Fig. 1, where (a) is the microstructure and (b) is the diffraction pattern taken from that area. It was also frequently observed that in other areas more or less continuous rings of weaker intensity were superimposed on the simple (111) diffraction pattern, suggesting the presence of a wide range of additional orientations. Other evidence indicated that the recrystallization characteristics are different in these two different types of areas. The hot-stage observations which provide this evidence will be discussed in another paper. AS shown in Fig. l(a), numerous dislocation-free areas of very small size are embedded in the "clouds" of high-dislocation density. This indicates that the deformation of a single crystal, even after a rolling reduction of 70 pct, is far from uniform on a micro-

Jan 1, 1962

By John T. Norton, Matthew J. Donachie

Residual lattice strai?zs were produced in 2024 aluminum and ingot iron by uniaxial tensile deformation. These strains were rneasured on the original surface and ulith depth below the surface. The strains conformed approximately to those from a macroscopic stress distribution but they were not truly macroscopic in nature. The exact mechanism which apparently causes the coherently difi9,acting region of each grain to behave as if macroscopically stressed was not determined. MACROSCOPIC stresses in metals produce strains in the lattice which result in X-ray line broadening and line displacements. The latter effect can be utilized in a technique for determining stresses in metals as first shown by Lester and born.&apos; Subsequent advances in technique have enabled the X-ray method of stress measurement to be satisfactorily applied to many problems involving residual stresses of a macroscopic nature, such as those due to welding, grinding, shot-peening, and so forth. In the case of stresses such as those described above, the correlation of X-ray- and mechanically determined data has been generally good. However, plastically extended polycrystalline metals have sometimes been reported2 to show line displacements upon release of the applied tensile load, yet the nature or origin of the residual lattice strains, rls, producing these displacements has never been clear. As will be pointed out, this lack of clarity regarding the macroscopic or microscopic nature and origin of these stresses casts doubt on the validity of results achieved by the commonly accepted techniques of X-ray stress measurement. This anomalous behavior requires clarification to remove the doubts concerning X-ray stress measurement. The present paper is the result of an investigation of the interesting behavior of such plastically extended polycrystalline metal bodies. The studies were originated to carry out the following tasks: 1) Observe whether a residual lattice strain is produced as a result of plastic extension and show whether any residual lattice strains produced can be related to the usual concept of a macrostress. 2) Examine the origin of any residual lattice strains observed. 3) Consider the implications or consequences of the existence of such residual lattice strains on the problem of X-ray stress measurement. THEORY 1) Lattice Strains. The theoretical developments necessary for the treatment of lattice strains and their relation to stresses follow from the classical theory of elasticity and have been adequately covered by arrett. For an isotropic solid under homogeneous deformation, it can be shown that, for uniaxial stresses where Dl is the macrostress acting in the longitudinal direction; E$L is the lattice strain in the plane defined by the surface normal and the longitudinal direction at an angle, , from the surface normal; ET is the similar strain in the transverse plane; E is Young&apos;s modulus; and v is Poisson&apos;s ratio. Eq. [2] is independent of angle + and Eq. [I] is a linear function of sin2, see Fig. 1, and can be solved analytically for DL if E and u are known and EL is measured. Thus, a uniaxial macrostress will be indicated by a linear E,L vs sinZ plot and a

Jan 1, 1962

By O. J. Malacarne, D. G. Millenbruch

The use of a series of thickeners for washing of the slime fraction of a leached ore is not uncommon in the uranium industry; however, few ore processing mills have used a thickener circuit for washing leached total ore. The common practice is to wash the sand fraction in classifiers and the slime fraction only in thickeners. At the Uravan mill of Union Carbide Nuclear Co., a total ore acid leach is employed to extract uranium values from sandstone ores. These leached ores are then washed at a nominal rate of from 1000 to 1300 tpd in a series of washing thickeners. A typical screen analysis of the ore being washed in these thickeners is: 25 pct, -200 mesh; 3 pct, +35 mesh; and about 1 pct, +14 mesh. The amount of slimes (-200 mesh) will vary from 20 to 30 pct as the mill receives ore from 150 different mines. The washing liquor is acidic, from a pH of about 2 in the first thickener to 0.6 pH in the last thickener and, of course, all acid duty equipment must be used. The Uravan mill of Union Carbide Nuclear Co. is located in Montrose County, Colo. and is physically located on a canyon wall along the San Miguel River. The thickeners referred to in this paper are located on top of the mesa above the canyon. For purposes of identification, these thickeners are numbered 1 through 8 from south to north. GENERAL DESCRIPTION OF CIRCUIT The circuit utilized consists of eight wooden fir tanks, 60-ft diam by 12-ft deep, set in a line and staggered in elevation by approximately 3 ft. The washing water flows through the thickeners by gravity, while the ore pulp is pumped uphill from thickener to thickener. Adequate piping and pumping capacity are available so that any of the thickeners can be bypassed in the circuit. All the controls for the

Jan 1, 1962

By Michael G. Zabetakis

Limits of flammability of normal propyl nitrate (NPN) vapor were investigated at ambient and elevated temperatures. Minimum spontaneous ignition and decomposition temperatures were determined with laboratory apparatus over the pressure range from 0 to 4,000 p.s.i.g. Flame speeds and the detonation susceptibility of NPN vapor were measured at elevated temperatures. Stable detonation was obtained with liquid NPN at elevated temperatures, and the detonation velocity was determined to be between 4,700 and 5,100 m./sec.

Jan 1, 1962

By K. E. Doud

An unusually pure grade of rutile and several grades of aplite rock are produced in a unique mining and mineral dressing operation in Hanover County, Virginia. The ore body is an aplite rock of gnessic structure, having a sari ace exposure extending over several hundred acres, heavily leathered and containing rutile, ilmenite, and other titanium and iron minerals. The physical nature and mineral composition of the ore body has permitted the use of a relatively economical and unusual processing circuit. The flowsheet was designed to take full advantage of the remarkable liberation of the minerals at relatively coarse rinds. It permits flexibility in changing the product mix, and maintains high levels of purity in both rutile and aplite rack. The mineral processing is discussed in some detail below.

Jan 1, 1962

By W. N. Poundstone, W. M. Merritts, B. A. Light

A joint investigation by the Bureau of Mines and the Christopher Coal Co. at the Humphrey No. 7 mine, operating in the Pittsburgh coalbed in northern West Virginia, was undertaken to gain more insight concerning the hazardous emission of methane gas in mining. This report describes the equipment, procedure, and results. Horizontal bleeder holes drilled in the faces drained large quantities of methane, eliminating downtime of mining equipment. Also, larger quantities of methane were removed by forcing 14 to 25 g,.p.m. water at 25 to 200 p.s.i. 5 pressure into the bleeder holes. In one infusion test a fluorescein dye was added to the infusion water; in later mining operations, the infusion water was traced for a distance of 1,500 feet. With vacuum pump applied to the horizontal hole the gas-flow rate increased, and the methane content decreased. Tests indicated that methane and water infused in bleeder holes traveled along the bedding planes of the Pittsburgh coalbed at a faster rate than across the planes. Methane associated with coalbeds is produced by the slow decomposition of carbonaceous material in the absence of air and the presence of water. It is lighter than air and, depending on its concentration, forms an inflammable or explosive mixture with air. It is believed that methane is entrapped in and around the pores of the coal and adjacent strata--often under great pressure. In many cases where the strata have been disturbed by geologic movements the

Jan 1, 1962