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By A. S. Nowick, C. Y. Li

It is deMonstrated that quenching from an elevated temperataupe accelerates the grain boundary relaxation in two solid solutions (aAg-Zn and a Cu-Al). This result is consistent with the proposal that, in solid solutions, grain boundary relaxation occurs by a mechanism of' self diffusion. Nevertheless, an alternative possibilitg, that quenching introduces vacancies into the boundary itself, must also be considered. THE phcnomenon of grain boundary relaxation has been well known for many years,1,2 yet the mechanism of this process is very poorly understood. One of the most interesting suggestions which relates to the mechanism of grain boundary relaxation was that of Ke,3 who claimed that the activation energy for grain boundary relaxation and for lattice self diffusion were essentially the same. The implication is therefore that the elementary step in the two processes is the same. This suggestion is particularly startling in view of the fact that activation energy for self diffusion along a grain boundary is very significantly lower than that for volume self-diffusion. Later evidence5-7 showed that there really are two grain boundary peaks, one which appears in high-purity metals, and the other (which develops at a higher temperature than the first) which appears in solid solutions beginning at solute concentrations in the range of 0.1 pct. Data for silver6 show that Kg's hypothesis is surely incorrect for the grain boundary peak in the high-purity metal, since it has an activation energy of only 22 kcal per mole, but that the hypothesis may still be correct for the grain boundary peak in various silver solid solutions, for which activation energies in the range 40 to 50 kcal per mole are observed. If the elementary step in the grain boundary relaxation process were the same as that for self-diffusion, it would be expected that the relaxation process could be hastened by quenching, 2.c. by introducing a non-equilibrium excess of lattice vacancies. Such a quenching effect has already been demonstrated in the case of another anelastic relaxation process, viz., the Zener relaxation effect. The Zener effect, which occurs in essentially all solid solutions, may be attributed to the reorientation of pairs of solute atoms in the presence of an applied shear stress,' and therefore must take place by means of a volume diffusion mechanism. The hastening of this process through quenching9 has been one way of demonstrating that atom movements in the lattice take place through a defect mechanism, presumably single vacancies. In order to see if the grain boundary relaxation is affected by quenching, it is particularly convenient to compare the grain boundary relaxation with the Zener effect, by choosing a specimen for which both relaxation effects appear. Specifically, a fine-grained sample of a solid solution shows in the curve of internal friction vs temperature, first a peak due to the Zener effect, then a second rise (and eventually a peak at substantially higher temperatures) due to the grain boundary relaxation. The same phenomena are also observable in static anelastic measurements, such as creep at very low stress levels. Thus, for the same fine-grained solid solution, the creepstrain, when plotted against log time, falls on a sigmodial curve with a sharp inflection point, due to the Zener effect, which is followed by a second rise and inflection resulting from the grain boundary relaxation. To look for a quenching effect, static measurements are preferable to the dynamic internal friction measurements, due to the fact that quenching effects tend to anneal out too rapidly at the temperatures at which the internal friction is measured.9 RESULTS AND DISCUSSION Creep experiments in torsion were carried out in an apparatus similar to that described by Ke1, whereby a wire is held under constant torque and its angular displacement is observed as a function of time. The alloy Ag-30 at. pct Znwas selected because of the large Zener relaxation that it displays. The two samples used were a "coarse grained" wire with a mean grain size about twice the diameter of the wire (diam = 0.032 in.), and a "fine-grained" wire which had several grains across the diameter. In Fig. 1 a comparison is made of the creep curves at 160°C of these two samples after they had been cooled slowly from 400°C. Curve A, which represents the coarsegrained sample, shows a unique relaxation process due to the Zener relaxation, with a relaxation time, T , in the vicinity of 100 sec. Curve B, which represents the behavior of the fine-grained sample, on the other hand, shows first the same relaxation process as that in A, followed by a turning up of the curve which corresponds to the onset of a second overlap-

Jan 1, 1962

By R. E. Lund

The design, operation, and performance of an integrated pilot plant for recovering zinc and copper from a complex sulfide ore are described. Metallurgical processing comprised selective sulfate roasting in a fluid bed, leaching in a weak sulfuring acid solution, recovering copper by cementation with scrap iron, air oxidation to remove soluble iron, more-or-less conventional purification for removal of impurities deleterious to zinc electrolysis, recovering zinc by electrolyzing solutions, and recycling spent electrolyte to the sulfating roaster. The effects of several feed preparation and roasting variables on the sulfation response of zinc, copper, and iron are set forth, together with the electrolyzing characteristics of the zinc solutions.

Jan 1, 1962

By Charles Law McCabe, Lyndon H. Everett, Edna A. Dancy

It has been found that the carbide phase present at equilibrium in the system M-H2-CH4, at about 600°C, is MC for the rare-earth metals Ce and Pr. X-ray diffraction analysis showed that the monocarbides have fcc structures with lattice constants of 5.036 + 0.009Å and 5.131 + 0.001Å for CeC and PrC respectively. Gaseous equilibrium measurements were used to calculate the standard free energy of formation of the monocarbides from the elements. for the formation of (+ 1300) for the formation of PrC. THE rare-earthdicarbides, and their crystal structures, have been known for some years,l but only more recently were the carbides CeC,2,3 Ce2C3 2 and CeCS3 reported. In 1958 to 1959, Spedding et al. published work on the lanthanum-carbon system4 and other rare-earth metal-carbon systems,5 proving the existence of M2C3 and MC2, and measuring the lattice constants. They also demonstrated that tri-rare earth carbides, M3C, exist for the rare-earth metals samarium through ytterbium. However, they concluded that the cerium monocarbide reported by Brewer and Krikorian2 and by Warf,3 and given a fcc structure with a lattice constant of 5.130Å bythe former workers, was, in fact, cerium metal with carbon dissolved in it. They were also unable to find any evidence for the existence of Warf's CeC3, for which no structural details had been given. Even more recently, Palenik22 reported the existence of only M2C3 and MC2, having been unable to find any evidence for the existence of any other rare-earth carbides. There are no published experimentally derived thermodynamic data for the formation of any of these carbides, although Brewer and Krikorian6 have estimated values of for CeC, Ce2C3 and CeC2. The objective of the present investigation was; to determine experimentally the free energy of formation of any of the reported carbides of cerium and praseodymium, through a study of the rare-earth metal-hydrogen equilibrium. EXPERIMENTAL A methane-hydrogen mixture was circulated, in a closed system over previously prepared cerium or praseodymium hydride, and when equilibrium had been attained, the gas mixture was analyzed by selectively oxidizing the hydrogen and condensing out the water formed. The metal hydrides were used as starting material for convenience because, otherwise, the hydrogen in the gas mixture would immediately dissolve in the metals; in addition, the metals would not react with methane alone at the experimental temperature (around 600°C). The circulating system was based on that used by Browning, DeWitt, and Emmett7 for similar studies on iron carbides. It consisted of a quartz reaction vessel, all-glass circulating pump, analysis tube containing copper oxide that could be heated to 300" C by means of a small furnace, a solid CO2-methanol trap, and a double limb absolute manometer, Fig. 1. A cathetometer, capable of reading to 0.005 cm, was used to measure the difference in height between the two columns of mercury. In its final form, the reaction vessel was enclosed in an outer jacket, containing approximately the same pressure of hydrogen as that within, to reduce errors due to diffusion of hydrogen out through the fused silica of the reaction vessel., The circulating system was supplied with

Jan 1, 1962

By Charles Smeal, Robert J. Schafer, Max Quantinetz

Normally metal powders cannot be ground to sub-micron sizes because of welding and agglomeration phenomena. Through the use of selected grinding aids and grinding fluids, nickel and other metal powders have been ball-milled as fine as 0.1 It was found that certain inorganic salts are more effective grinding aids for metal powders than conventionally used surfactants. METAL and alloy powders are used to produce reagents, pigments, coatings, solders, brazes, and parts for industry by powder metallurgy techniques. They are also combined with refractory compounds to produce cermets and dispersion-hardened products. One of the interests at the Lewis Research Center has been to explore the potentialities of the dispersion strengthening process. Since the work of Ir-mann, many investigators have shown that the strength of dispersion-hardened products may increase with decreasing interparticle spacing.24 One approach to achieving small interparticle spacing is to combine fine refractory compounds and metal powders, preferably below 1 in size. In attempting to obtain fine metal powders, it was found that until very recently the best that could be obtained from commercial suppliers, particularly of ductile metals, was about 1.0 . Interest was therefore developed in providing finer metal powders for dispersion-hardening studies. Information obtained from the literature, from others working in the field, and from prior experimental work performed at NASA, led to a consideration of ball-milling as a technique to produce the desired materials. Some of the variables associated with ball-milling are the size, material, and nature of construction of the grinding container; the nature and amount of the grinding material and material to be ground; and the nature and amount of the grinding liquid and grinding aid, if employed, and the grinding time. In all ball-milling, welding and agglomeration can oc- cur as well as grinding. Because of the tendency of ductile metals to weld together, they are difficult to grind.5 The ultimate particle size obtained on grinding is generally the one at which the rate of grinding becomes equal to the rate of welding. To help delay welding and thus obtain smaller particle sizes, grinding aids are often employed. The principal objective of this investigation was to produce submicron metal powders by ball-milling the powders with selected grinding aids and grinding fluids. A secondary objective has been to attempt to explain the variations observed in grinding behavior by considering possible grinding mechanisms and correlating various parameters with grinding effectiveness. Three groups of ball-milling experiments were run; one in which the grinding aid was varied, a second in which the grinding fluid was varied, and a third in which the material being ground was varied MATERIALS, APPARATUS, AND PROCEDURE In the first group of experiments in which the grinding aid was varied Inco Carbonyl Grade B nickel powder initially 2.5 (all sizes refer to average particle size as measured by Fisher Sub -sieve Sizer) was used as the material being ground and 200-proof ethyl-alcohol as the grinding fluid. Surfactants, representative of typical organic structures, were selected as grinding aids. Inorganic salts used as grinding aids were chosen on the basis of the size and valence of their ions. Water soluble salts were used in order to facilitate their removal from the slurry after grinding. In the second set of experiments, grinding of the 2.5- Ni powder was tried in four different grinding liquids; water, cyclohexane, n -heptane, and methy-lene chloride. In this study seven grinding aids selected from those tried in the first group of experiments were employed. In the third group of experiments 200-proof ethyl alcohol was again used as the grinding fluid to mill Cu, Cr, Fe, Ag, and Ni powders of various initial particle sizes' All mill charges contained 300 ml of grinding liquid and 3000 g of 1/2 in. stainless steel balls. When inorganic salts were used as the grinding aid, 70 g of salt and 210 g of metal powder were employed, and with surfactants 6 g of grinding aid and 300 g of

Jan 1, 1962

By Charles B. Kenahan

Vanadium is subject to only light corrosion in phosphoric acid at temperatures up to 60° C. and has a moderate corrosion rate in this acid at 100° C. It is relatively corrosion resistant in sulfuric and hydrochloric acids up to 60° C, but corrodes rapidly at 100° C. It corrodes rapidly in dilute nitric acid at 35° C. Vanadium is almost inert in 10-percent solutions of formic, acetic, lactic, tartaric, and citric acids; in 9-percent oxalic acid it corrodes slowly up to 60° C. and rapidly at 100° C. Vanadium is resistant to corrosion in substitute ocean water, tapwater, and in 3-percent sodium chloride and 10-percent sodium hydroxide solutions. It is readily attacked, however, by 20-percent ferric chloride, 20-percent cupric chloride and 5-percent mercuric chloride solutions. Vanadium is protected by contact with magnesium, aluminum, and steel SAE 4130 in substitute ocean water, by magnesium and aluminum in 3-percent sodium chloride solution, and by magnesium in tapwater. Vanadium protects copper in substitute ocean water. When vanadium and stainless steel are coupled in sulfuric acid solutions, both metals are usually unaffected by contact, whereas the corrosion rate of titanium in sulfuric acid is greatly reduced by contact with vanadium.

Jan 1, 1962

By H. E. Powell

A series of alkyl-dithiocarbamic acid amine salts was prepared and tested as collector for slimed lead minerals contained in the waste material from a commercial lead ore concentrator. The reagents, members of a homologous series differing only in the number of alkyl radicals in their structure, were prepared by reacting stoichiometric amounts of primary amines and carbon disulfide in a cold alcohol solution. Subsequent purification was by recrystallization from absolute ethyl alcohol solution. Evaluation was through froth flotation of a mill tailing containing 0.2 percent lead. Results show that maximum recovery (38 percent) was obtained with the reagent containing 8 alkyl radicals, but that maximum rougher concentrate grade (4.8 percent) was obtained with the reagents of intermediate number of radicals.

Jan 1, 1962

By H. A. Dierks

Implementation of the joint Federal-State control program established in 1955 to cope with the mine water problem in the Pennsylvania anthracite region is described in this report. The increasing severity of the water problem in the anthracite mines has necessitated major adjustments as this continuing program has progressed. Since 1941 the Federal Government has recognized the mine water problem as an important factor in the worsening economic condition of the anthracite region by initiating scientific and technologic investigations and establishing the Anthracite Flood-Prevention Section in the Bureau of Mines in 1948. On the basis of comprehensive investigations and studies, the results of which were published in numerous reports and bulletins, the Anthracite Mine Drainage Commission of the Commonwealth of Pennsylvania formulated a plan that served as a background for legislative action in 1955, resulting in Public Law 162, 84th Congress (Act of July 15, 1955 (69 Stat. 352; 30 U.S.C. 571-576)), for the Federal Government, and Act No. 82 of the General Assembly, July 7, 1955, for the Commonwealth of Pennsylvania. The report covers 29 mine flood control projects approved and executed in implementing the aforementioned legislative acts. Essential engineering and cost details for each project are given, together with an evaluation of the effect that the installed facilities have on alleviating the mine water problem as it concerns individual mines and the anthracite industry as a whole.

Jan 1, 1962

By J. E. Castle

The essential foundation upon which to build an effective marketing program in industrial minerals is the ability to produce competitively mineral products meeting precise customer specifications and to ship them promptly and on schedule. Without this prerequisite, all the other factors in a second marketing program-creative sales management, energetic solicitation, advertising, technical service, new products, etc.are without meaning. The primary image to be created in the mind of customers is that of the reliable and prompt supplier of mineral products at competitive prices and of standard, uniform quality. With this favorable image implanted, it becomes possible to integrate the other essential factors into a strong marketing program; and without this image, little can be accomplished. After having .made provision for the basic product ion position outlined, there are then two fundamental considerations in the design of a successful marketing program for industrial minerals. The first of these is that the number of potential customers for the typical industrial mineral product is, relatively small, and indeed compared to the number of customers for consumer products, the number is actually minute. The second consideration is that the customers for industrial minerals are manufacturers and producers rather than consumers. These two factors lead to a necessity that the marketing program be specifically and uniquely tailored to fit the individual mineral product to be sold and to conform to an existing pattern of distribution.

Jan 1, 1962

By T. N. McVay

The Bureau of Mines has developed a field test for detecting the presence of columbium in a variety of minerals containing the clement. The test consists of fusing the mineral or rock powder with potassium pyrosulfate in a porcelain crucible, digesting the melt with hot dilute hydrochloric acid to release the columbium oxide (Cb205), and subsequently reducing the columbium oxide to a lower oxide by adding tin, which gives a blue color to the contents of the crucible. The method will detect 1 percent of contained columbium oxide (Cb205) in a mineral sample provided no tungsten is present. If a mineral containing appreciable titanium is test,-!d in the same manner, the solution in the crucible becomes violet. In the presence of columbium, titanium at first causes a violet coloration of the solution, which after a few minutes is masked by the stronger blue of the reduced columbium oxide. Although tantalum oxide (Ta205) does not interfere with the columbium test, tungsten gives a blue color that is indistinguishable from the color obtained with columbium. A simple method is available to detect the presence of columbium in the absence of tungsten, but when the presence of tungsten is suspected, the sample must be subjected to somewhat more elaborate chemical tests to determine the presence or absence of columbium. Although these latter tests can be made in the field, several steps are involved that arc best performed in the laboratory with simple equipment.

Jan 1, 1962

By Goode RA

It is-assumed that a pipeline system is economically justified as a means of transportation.. The terms "True Life" and "Economic Design Life" are defined. The most usual design alternatives to be considered from both physical and economic -viewpoints are listed and a summary is given of the main factors to be costed in assessing the relative economics of each alternative. A brief statement of the recor mended method af economic. assessment is given and an example is included. The paper aims to present a reasonably accurate, simple and practical method of considering the main economic factors which govern design.

Jan 1, 1962

By E. A. Sigworth

Our interest in metallurgical applications for activated carbon was thoroughly aroused when laboratory studies indicated that each dollars worth of carbon could retain as much as four dollars worth of tin. Since then other data was developed suggesting many Potential uses in the metallurgical field it is hoped that, the information presented in this paper may encourage studies by knowledgeable individuals in metallurgical operations. Activated Carbon accomplishes its results by adsorption which involves selective removal of materials from solution by holding the compounds on the carbon surface at the active areas. An example of adsorption is the dyeing of cloth where the dye is selectively held on the cloth surface and the concentration in the dye solution is thereby reduced. Many theories exist on, adsorption, but the predominant factors involved in metallic ion adsorption probably are that adsorption is indirectly proportional to solubility and is benefited by high concentrations acting to squeeze out molecules in smaller amounts.

Jan 1, 1962

By S. E. Haszko

SEVERAL new XGa2 intermetallic compounds, Table 1, where X is a rare earth, having the AlB, structure were prepared as part of a continuing study of the magnetic and structural properties of rare-earth alloys.' In this note, the crystallographic results of these compounds are presented. Chart, Eq. 121 for the data in Fig. 1 can be adequately represented by The corresponding standard free-energy change is AF; = -4.576 T log K = -20,900 + 10.20T [5I At low nitrogen concentrations the ratio of mole fraction to weight percentage is a constant so that the mole fraction X of nitrogen is given by X = 0.0392 [%NJ. At low values of X, the activity and the concearation approach each other, hence K, = 0.0392 K,, where K, is expressed in terms of the mole fraction of nitrogen. Hence Eqs. [4]. and [5] become

Jan 1, 1962

By B. D. Cullity, K. S. Sree Harsha

When a copper or aluminum single crystal is swaged into wire, the resulting deformation texture depends on the original orientation of the crystal. The<100> and <111>orientations me essentially stable, while <110> is unstable. The greater the <100> content of the deformation texture, the stronger the wire is in torsion. the greater the<111>content, the stvonger it is in tenszotz. The preferred orientation (texture) of fcc wires, either after deformation or recrystallization, is usually a double fiber texture in which some grains have <100> parallel to the wire axis and others have <111>. The relative amounts of these two texture components, as reported by different investigators for the same metal, vary considerably. Previous work in this laboratory&apos; has shown that the starting texture of a wire, i.e., the texture which it has before deformation, can have a decided influence on the texture produced by deformation. In particular, it was found that the deformation texture of copper wire is essentially a single <100> texture, if the wire before deformation contains only a <100> component. This is true even when the deformation is carried to more than 98 pct reduction in area. This paper reports on further studies of the role played by the starting texture. Copper and aluminum single crystals of various orientations have been cold swaged into wire, and quantitative measurements of the resulting deformation textures have been made. The tensile and torsional properties of the deformed wires have also been measured, and the relation between these properties has been correlated with the texture of the wire. These measurements were made in order to demonstrate that a cold-worked wire can be made relatively strong in torsion and weak in tension, or vice versa, by proper selection of the texture before deformation. MATERIALS The copper was of the tough-pitch variety, containing, by weight, 99.962 pct Cu, 0.003 pct Fe, 0.025 pct 0, and 0.0021 pct Si. The aluminum contained more than 99.99 pct .&apos;41; the only reported impurities were 0.001 pct Fe, 0.001 pct Si, and 0.003 pct Zn, by weight. Large single crystals of these metals were grown by the Bridgman method in graphite crucibles and a helium atmospliere. Cylindrical specimens of predetermined orientation, about 1.5 in. long and 0.36 in. in diameter, were machined from the as-grown crystals and then etched to 0.25 in. to remove the effects of machining. Their orientations were checked by back-reflection Laue photographs, and they were then swaged to a diameter of 0.050 in. (96 pct reduction in area). 111 order to study the "inside texture" of the deformed wires, they were etched, after swaging, to a diameter of 0.040 in. before the texture measurements were made. TEXTURE MEASUREMENTS The fiber texture which exists in wire or rod can be represented by a curve showing the relation between the pole density I, for some selected crystal-lographic plane, and the angle $ between the pole of that plane and the wire axis (fiber axis). Such a curve will show maxima at particular values of , and these values disclose the texture components which are present. The relative amounts of these components can be determined2&apos;3 from the areas under the maxima on a curve of I sin F vs F. It is seldom necesszlry to measure I over the whole range of F from 0 to 90 deg, since the existence of maxima in the low-F relgion can be inferred from measurements confined to the high-F region. The X-ray measurements were made with a General Electric XRD-5 diffractometer and filtered copper radiation, according to one or the other of the following procedures: 1) A method developed in this laboratory,4 involving diffraction from a single piece of wire. 2) A modification of the Field and Merchant method.5 This method was originally devised for the examination of sheet specimens, but it can easily be adapted to the measurement of fiber texture. Three or four short lengths of wire are held in grooves machined in the flat face of a special lucite specimen holder. The axes of the wires are parallel to the plane defined by the incident and diffracted X-ray beams, and the holder to which the wires are attached can be rotated step-wise about the diffractometer axis for measurements at various angles 9.

Jan 1, 1962

By N. M. Parikh, T. J. Koppenaal

The strengthening mechanism of fiber-reinforced silver has been investigated as a function of fiber density and fiber material. Stress-strain curves were determined in the range 2 x 10-6 to 2 x 10-3 plastic styain and slip lines were examined. The yield strength at 0.2 pct permanent strain is markedly dependent upon fiber density but the stress necessary to initiate plastic deformation is independent of fiber density. The strengthening mechanism of the fibers is shown to be malogous to grain boundary strengthening in poly crystalline metals. The variation in strengthening with different types of fibers is also noted and discussed. In recent years, considerable progress has been made in the understanding of the mechanical properties of two-phase systems, particularly in the classical dispersed-phase alloys where the separation between the dispersed phases is 0.01-0.1µ. However, little work has been done on fiber-reinforced metals where the dispersed-phase separation is considerably larger than this. Parikh1 investigated the mechanical properties of many fiber-reinforced metals and found that two general relationships are always observed, as follows: 1) A fibrous network incorporated into a second weaker metal strengthens the latter, and the amount of strengthening increases with fiber concentration. 2) At a corrstant fiber concentration, the amount of strengthening in a given matrix can vary considerably, depending upon the type of fiber employed. The object of the present investigation was to examine the fuiidamental factors controlling these two observations. procedure: Fig. 1 shows the initial step in the fabrication of the specimens. The sieve is shaken so that the fibers fall into a mold with the longitudinal axes of most fibers in the X-Z plane. The fibers are then compressed to a predetermined density, thus forming a "felt", and the necessary amount of matrix metal is added to the top of the felt. The mold is heated, in vacuum or hydrogen, to above the melting point of the matrix metal; the molten metal flows into the felt, and the entire assembly is cooled. This produces a "composite" that is essentially free of voids. A number of composites were prepared in this manner using 1/4-in. kinked lengths of mild steel

Jan 1, 1962

By Robin O. Williams

The increase in internal energy as the result of deformation has been measured for lead, aluminum, silver, nickel, iron, and zirconium by using rapid, adiabatic compression. The stored energy increase is roughly Proportional to the strain; the propor-tionality constant increases rapidly with increasing melting point. The fraction of the mechanical energy which is stored increases more slowly, since the strength of the metals also increases with melting point. The values of the stored energy are considered accurate to about 10 pet. The present values appear about 50 pet larger than the more reliable published results where comparisons are possible. It is possible that this difference is due to the high strain rate used in this investigation. Immediately after deformation all these metals release energy at a rate roughly proportional to (time)-&apos;. This release is considered to be associated with dislocation motion but in aluminum (and copper) some additional process seems to be present. This release can represent 20 pet or more of the stored energy. WHEN pure metals are plastically deformed, most of the mechanical energy is converted into heat. The energy remaining within the metal is significant in that it is the energy of the disorder produced and thus detailed knowledge of this energy is a powerful tool in understanding the nature of deformational disorder. While much effort has been expended on this problem, the amount of information available is limited. The situation as of 1958 has been carefully reviewed by Titchener and ever.&apos; The present results have been obtained by a new experimental approach to this problem. The method necessitates high-strain rates which make comparisons with published results less certain, but a high-strain rate is an advantage in that the energy release immediately after deformation can be followed. EXPERIMENTAL PROCEDURE In the experimental method used, the internal (stored) energy is given as the difference between the mechanical work used in deforming the sample and the heat which is released (the first law of thermodynamics). The work is supplied by two identical hammers swinging freely from a fixed height, the available energy being the product of the mass, the gravitational constant, and the distance through which the center of gravity moves. The initial temperature rise of the sample represents the heat produced by the deformation. The sample temperature is determined by a small thermocouple embedded in and supporting the sample. This process can be repeated over and over to produce increased strains. Most samples are run through about five cycles to a total strain of around 0.7. Further details are covered elsewhere. The determination of the heat is dependent upon the sample weight, its specific heat, the rise in temperature, and any gains or losses to the surroundings. One is dependent on published results for specific heals (the values were taken from a collection).3 The values must be accurate to about 0.1 pet in order that they not affect the results. The best values thus do not contribute to the uncertainty, but this is probably not always the case. The accuracy of the temperature rise is limited primarily by knowledge of the thermocouple characteristics over short temperature intervals, but careful calibration eliminates this as an important factor. One can calculate readily the heat flow between the sample and hammers if the time of contact and the sample temperature are known and if there were no oil at the interface. Assuming the maximum temperature difference, upper values for this interchange have been calculated (the time of contact is determined from the decrease in sample length) and it may or may not be significant. However, no correction is colnsidered necessary because of the presence of a thin oil film which has a thermal conductivity much less than the metals. Except for the possible uncertainty in specific heat, the heat is considered to be adequately known. The mechitnical losses which are recognized as important are: 1) friction between the sample and the hammer:;, 2) the kinetic energy in the hammer suspension system which may not be entirely usable, 3) the rebound energy of the hammers, and 4) the vibration of the hammer heads. All these have been covered in detail elsewhere2 and only the more significant points are made here. The friction turns out to be small except for soft materials (lead)

Jan 1, 1962

By J. B. Clark, A. S. Yue

The zone-melting technique can be adapted for the de-termination of the eutectic composition in complex metal systerrzs. The application of this method is demonstrated in a simple eutectic system, Mg-AE, in which the eutectic composition is known and in a complex ternary system, Mg-Al-Zn, in which the literature is uncertain as to the composition of the ternary eutectic. The advantages and limitations of this unique approach for the determirution of the eutectic composition are discussed. ThE eutectic composition in phase diagrams is usually determined by thermal analysis of a series of arbitarily selected alloy compositions. The temperatures of the liquidus and eutectic arrests for each alloy are plotted and the eutectic composition is estimated by extrapolation to the entectic temperature of the curve formed by the liquidus arrest temperatures for the series of alloys. Although this approach readily yields the eutectic temperatures, several dekrminations are needed to estimate the eutectic composition, even in a simple system. In a complex ternary system, a great many determinations are often necessary to estimate, even approximately, the ternary eutectic composition. Thus, the conventional method is inherently tedious and time consuming. The application of zone melting provides a relatively efficient method of determining the eutectic composition.&apos; As an illustration, consider the zone melting of an alloy composition C, in the simple eutectic system A-B, shown in Fig. 1, under the ideal conditions of infinitely rapid diffusion in the liquid, no diffusion in the solid, and ease of nucleation of both phases. As the zone moves along the bar, the composition of the zone is enriched by solute rejected during the freezing of the a phase and the zone composition approaches the eutectic composition CE.Once the zone composition attains the lowest melting composition, i.e., the eutectic composition, it remains at this composition as the zone moves along the bar and finally freezes as such at the end of the bar. Chemical analysis of the end of such a zone-melted bar then should yield the eutectic composition CE of the system A-B. A corresponding analysis can be made for a ternary eutectic system. Under the ideal conditions noted above, only one pass of the molten zone is required to yield the eutectic composition. Experimentally, however, a solute-rich layer forms at the solid-liquid interface2 and the composition of the zone does not attain the eutectic composition as rapidly or as uniformly as in the ideal case outlined above. But with agitation of the melt, the ideal conditions can be approximated experimentally. Also, as shown below, zone melting permits a cumulative build-up of the solute at the end of the bar to the eutectic composition. The purpose of this paper is to demonstrate this unique method for determining the eutectic composition. The method is here applied to two systems: first, to the binary Mg-A1 system, in which the composition is well established, and second, to the complex Mg-Al-Zn system in which there is doubt concerning the composition of the ternary eutectic. EXPERIMENTAL PROCEDURE The zone-melting apparatus used in this study is described in detail elsewhere.3 Briefly, the binary alloy rods (5/8 in. in diam and 9 in. long) and the ternary alloy rods (5/8 in. in diam and 6 in. long), with the compositions given in Table I, were zone

Jan 1, 1962

By R. L. Gall

This report describes Bureau of Mines experiments in gasifying coal in a helium-heated tube-coil reactor. The purpose of this work was to investigate helium as a medium for transferring heat from a nuclear reactor to gasify coal or for use as high-temperature process heat. A laboratory-scale system was designed and constructed to demonstrate feasibility. In preliminary tests with this system, in which the coal was fed as a water slurry, the helium-heating and recycling equipment operated well. Considerable difficulty was experienced, however, in preheating coal slurry to the desired range of 400° - 1,000° F. without plugging the preheaters. Five different preheaters plugged with coke or with salts leached from the coal. The longest operating period wan 12 hours. These difficulties were partly due to the relatively small equipment and flow rates. The gasifier processed l pound per hour of low-rank coal at 300 p.s.i.g. and 1,800° F., with the carbon conversion limited to 20 to 30 percent by the short residence time and slow heat-transfer rate.

Jan 1, 1962

By R. I. Jaffee, R. W. Wood, H. R. Ogden, D. N. Williams

D. W. Morgan, D. H. Polonis,and R Taggart (Uuivevsity of Washington)—Dispersion hardening in titanium-copper alloys is of particular interest to us in view of our current research activities in phase transformations in this system. We should like to raise questions concerning several points in the paper. The flow sheet for fabrication and heat treatment (Authors&apos; Fig. 2) indicates that 0.045 in sheet is treated in air for a period of 30 min at 1625&apos; F. Were any surface coatings used to reduce oxygen contamination at this stage? One might ask the same question about the 8-hr annealing at 1400F. Contamination during fabrication and heat treatment of such thin sections could be considerable without some protection. Although the authors state that no analyses were made, they note that contamination masks the distinction between base strengths of the different alloys. In this connection, what fabrication and heat-treatment procedures were used in obtaining the comparison specimens of unalloyed titanium? It would seem that oxygen contamination must cast doubt on the reliability of the proposed strength-mean free path relationship deduced from the data (Authors&apos; Fig. 5). It is usual to evaluate dispersion hardening on the basis of yield strength rather than ultimate tensile strength, and accordingly we have replotted the authors&apos; Fig. 1 to include yield strength. The yield strength data do not justify a discontinuity of 3 p at either 70" or 1000 OF. Can the authors substantiate their conclusion 1) with additional evidence? Otherwise it seems that they have succeeded only in pointing out the possibility of a linear relationship between yield strength (or Uts) and the logarithm of the nleall free path, comparable with that demonstrated for iron-carbon alloys (Authors&apos; Ref. 2). Work in our own laboratories has shown that the hardness of the phase Ti,Cu is 235 Vpn, and that of a 1.5 pct (at.) (2 pct wt) supersaturated solid solution of copper in titanium is 190 Vpn. This small difference in hardness would suggest that Ti2Cu should not be a very effective dispersion-hardening phase. D. N. Williams, R. W. Wood, H. R Ogden, RI. L Jaffee (authors&apos; reply)— This discussion brings out some interesting points with respect to the interpretation of our results, and also raises some questions regarding the experimental technique. We shall consider the latter questions first. Contamination during heat treatment was prevented by performing all heat treatments in argon-filled Vycor capsules. Fabrication was done in air, with the usually observed scaling. Scale was removed

Jan 1, 1962

By Paul Gordon, A. S. Iyer

Apreliminary investigation has been carried out on the annealing behavior of explosively deformed copper as compared to that of conventionally deformed copper, using hardness, stored energy, and the sharpening of X-ray spots on Debye rings as the measures of annealing. Some metallographic observations were also made. Two purities of copper were studied. The first was tough pitch copper obtained as a small piece from the guard ring of a sample explosively deformed to approximately 500 kbars.* The second consisted of mentedand deformed these samples quite badly so that only a few small fragments were available for the annealing experiments. As a result, little in the way of quantitatively significant data was gleaned from the measurements. However, several important qualitative differences between the annealing of explosively deformed and conventionally deformed copper have been observed. It is these effects which are described in this report. Fig. 1 presents the results of hardness and stored energy measurements during the annealing of the high-purity copper after explosive and after conventional deformation. The data for the conventionally deformed copper were taken from the work of Gordon;&apos; in this copper it is evident that most of the stored energy is released concommittantly with the hardness drop. As shown in orddon&apos;s&apos; investigation, these effect:: are definitely associated with recrystal-lization. In the case of the explosively deformed copper, on the other hand, a large fraction of the stored energy is released before any appreciable hardness change takes place. At 160°C about 40 pct, and at 170°C about. 80 pct, of the stored energy appears to have been released prior to the onset of softening, i.e., undoubtedly prior to recrystallization. In view of the facts that the hardness and energy measurements were made on separate samples and that there is reason to suspect that the intensity of the explosive deformation from sample to sample may not have been uniform, a check run was carried out in which both energq release and hardness changes were measured cnn the same sample. The results of this run, shown in Fig. 2, confirm the conclusion that much of the stored energy is released before the hardness begins to change appreciably. In an effort to obtain some idea of the activation energy associated with the early release of energy, a single callorimetric sample was annealed in two steps, first at 149.5"C and then at 159.5"C, Fig. 3.

Jan 1, 1962

By Thomas P. Meloy

Floating "fines" differs from floating "sands" because the fines have a much larger surface area compared to their mass. The forces that arise from this large specific surface the key to understanding the behavior and treatment of fine particles. Though the nature of these forces is not thoroughly understood, enough work has been done to give a qualitative picture of what is happening in a flotation cell. It is the purpose of this chapter to re-examine some of the more, recent theoretical work and-to indicate its importance.

Jan 1, 1962