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By A. H. Geisler, F. Keller

Some of the important changes that take lace in the structure of aluminum alloys are largely submicroscopic in character. This is especially true of the changes that accompany age-hardening and recrys-tallization. Although improved metal-lographic practices have been helpful in indicating some of these changes indirectly, results are limited by the resolving power of optical microscope lenses. The electron microscope, however, provides a new and important means for investigating the fine structure of metals in a range not possible heretofore. It is anticipated that this microscope will yield new and useful information to metallurgists when suitable techniques are developed to utilize its very high resolving power. Several unique methods have been devised to permit the examination of the structure of opaque samples by the electron microscope. These are all based 011 the principle of producing a very thin film that represents the prepared surface of the opaque metal sample, which can be examined in the transmission microscope; however, the available methods fall into three categories, depending on the manner in which the film is obtained. With the oxide-film method developed by Mah13-l7 a very thin surface layer of the metallographic sample is converted into oxide by a thermal, chcmical or anodic treatment. .After removal from the metal sample by one of the special techniques described by Evans,l9 this oxide film is examined in the electron microscope, and is found to portray the structure of the original metal surface. Films formed on aluminum,8,l7 nicke1,7 iron3,8,9 and a nickel-beryllium alloyl1 by heating; films formed on iron8,9 by chemical action; and films formed on aluminum3-'" by anodic oxidation, have been examined. The other two are more recent methods developed principally in this country; they consist in making the thin film in the form of a mold or replica of the surface contour of an etched sample. With the negative replica method the thin film is made directly on the sample; with the positive replica method it is made on a negative reproduction of the sample. With both methods, variations in the contour of the metal sample, caused mainly by etching, produce variations in the thickness of the surface replica. Because of the direct dependence of the amount of scattering of the illuminating electrons upon the thickness of the film penetrated, only the variations in thickness of the replica are responsible for tones in the electron image. Negative replicas are made by forming a thin film of some suitable material directly on the polished and etched metal sample, and derive their name from the fact that after removal from the sample they have the high and low points in the sample reversed, as shown in Fig. I. Nega-

Jan 1, 1944

By F. Keller, A. H. Geisler

Some of the important changes that take lace in the structure of aluminum alloys are largely submicroscopic in character. This is especially true of the changes that accompany age-hardening and recrys-tallization. Although improved metal-lographic practices have been helpful in indicating some of these changes indirectly, results are limited by the resolving power of optical microscope lenses. The electron microscope, however, provides a new and important means for investigating the fine structure of metals in a range not possible heretofore. It is anticipated that this microscope will yield new and useful information to metallurgists when suitable techniques are developed to utilize its very high resolving power. Several unique methods have been devised to permit the examination of the structure of opaque samples by the electron microscope. These are all based 011 the principle of producing a very thin film that represents the prepared surface of the opaque metal sample, which can be examined in the transmission microscope; however, the available methods fall into three categories, depending on the manner in which the film is obtained. With the oxide-film method developed by Mah13-l7 a very thin surface layer of the metallographic sample is converted into oxide by a thermal, chcmical or anodic treatment. .After removal from the metal sample by one of the special techniques described by Evans,l9 this oxide film is examined in the electron microscope, and is found to portray the structure of the original metal surface. Films formed on aluminum,8,l7 nicke1,7 iron3,8,9 and a nickel-beryllium alloyl1 by heating; films formed on iron8,9 by chemical action; and films formed on aluminum3-'" by anodic oxidation, have been examined. The other two are more recent methods developed principally in this country; they consist in making the thin film in the form of a mold or replica of the surface contour of an etched sample. With the negative replica method the thin film is made directly on the sample; with the positive replica method it is made on a negative reproduction of the sample. With both methods, variations in the contour of the metal sample, caused mainly by etching, produce variations in the thickness of the surface replica. Because of the direct dependence of the amount of scattering of the illuminating electrons upon the thickness of the film penetrated, only the variations in thickness of the replica are responsible for tones in the electron image. Negative replicas are made by forming a thin film of some suitable material directly on the polished and etched metal sample, and derive their name from the fact that after removal from the sample they have the high and low points in the sample reversed, as shown in Fig. I. Nega-

Jan 1, 1944

By William A. Johnson

The mathematical analysis of diffusion curves in solid metals is carried out ordinarily by analogy with the flow of heat in a continuous medium and no account is taken of the fact that the materials involved are composed of discrete particles that move discrete distances at irregular intervals. It is possible to treat the problem on the basis of simple assumed atomic mechanisms, in which case, because of the small scale of the elementary process compared to the gross effects observed experimentally, the two procedures lead to the same expression for the variation of concentration with distance. Thus, for engineering purposes, the usual methods are quite satisfactory. If, on the other hand, our purpose is to go beyond the mere collection of data, however desirable this may be, it is necessary to recognize and understand the factors that are of fundamental importance. One factor that has not hitherto been considered when dealing with solid metals is the difference in atomic weights of the isotopes of a single metal. While all the atoms of a given element are alike chemically, their weights may vary by a small but significant amount, and atoms of different weights may have different diffusion rates. With gases this variation in isotopic weight produces a change in the rate of diffusion by a factor inversely proportional to the square root of mass. While, except for the lightest gases, this is not a large effect, it is, for example, sufficient to permit a considerable concentration of one isotope at the expense of others. If metals exhibit a similar phenomenon, some modification of the analysis of the diffusion process will be required, since the different isotopes of a given metal will have different probabilities of moving and the heat-flow analogy will contain a fundamental error. This situation cannot be rectified by using a diffusion coefficient based on the average probability of moving, and it can be shown that even when the diffusion coefficient is independent of composition, the diffusion curve will not agree with the simple theory except in the rare cases where only one isotope exists; e.g., gold. If, however, the mass effect in the solid state were no larger than in the gaseous, the errors arising therefrom in the analysis of ordinary diffusion curves would be quite negligible. Nevertheless, our desire to obtain all possible information concerning the details of the diffusion process, and the possibility of diffusion in the solid state as a means for separating isotopes are cogent reasons for undertaking an experimental study to determine whether isotopes of different masses diffuse at different rates. Experimental Procedure If isotopes of different masses diffuse at different rates, the ratio of the concentration of one relative to another will vary with the distance from the diffusion inter-

Jan 1, 1946

By William A. Johnson

The mathematical analysis of diffusion curves in solid metals is carried out ordinarily by analogy with the flow of heat in a continuous medium and no account is taken of the fact that the materials involved are composed of discrete particles that move discrete distances at irregular intervals. It is possible to treat the problem on the basis of simple assumed atomic mechanisms, in which case, because of the small scale of the elementary process compared to the gross effects observed experimentally, the two procedures lead to the same expression for the variation of concentration with distance. Thus, for engineering purposes, the usual methods are quite satisfactory. If, on the other hand, our purpose is to go beyond the mere collection of data, however desirable this may be, it is necessary to recognize and understand the factors that are of fundamental importance. One factor that has not hitherto been considered when dealing with solid metals is the difference in atomic weights of the isotopes of a single metal. While all the atoms of a given element are alike chemically, their weights may vary by a small but significant amount, and atoms of different weights may have different diffusion rates. With gases this variation in isotopic weight produces a change in the rate of diffusion by a factor inversely proportional to the square root of mass. While, except for the lightest gases, this is not a large effect, it is, for example, sufficient to permit a considerable concentration of one isotope at the expense of others. If metals exhibit a similar phenomenon, some modification of the analysis of the diffusion process will be required, since the different isotopes of a given metal will have different probabilities of moving and the heat-flow analogy will contain a fundamental error. This situation cannot be rectified by using a diffusion coefficient based on the average probability of moving, and it can be shown that even when the diffusion coefficient is independent of composition, the diffusion curve will not agree with the simple theory except in the rare cases where only one isotope exists; e.g., gold. If, however, the mass effect in the solid state were no larger than in the gaseous, the errors arising therefrom in the analysis of ordinary diffusion curves would be quite negligible. Nevertheless, our desire to obtain all possible information concerning the details of the diffusion process, and the possibility of diffusion in the solid state as a means for separating isotopes are cogent reasons for undertaking an experimental study to determine whether isotopes of different masses diffuse at different rates. Experimental Procedure If isotopes of different masses diffuse at different rates, the ratio of the concentration of one relative to another will vary with the distance from the diffusion inter-

Jan 1, 1946

By William Marsh Baldwin

TWO of the most useful and important equations available to the metallurgist for the study of plastic deformation of metals are the Huber-von Mises-Henckyl-~ and the St. Venant7-10 equations. Huber-von Mises-Hengky Equation The Huber-von Mises-Hencky equation answers the question: When does plastic flow occur in metal that is subjected to a multi-axial stress? It occurs, according to this equation, when the three principal stresses,t UI, u2, and u3 satisfy the equation: (<ri - <r2)2 + (<r2 - <rsY + (ff! - <r3)* = 2Ki [i] Here K is the yield strength of the material as determined in an ordinary tensile test. If the quantities ul, 52, andas are assigned to the coordinates of a Cartesian three-dimensional system, this expression describes a cylinder whose axis of symmetry is inclined at equal angles to the three coordinate axes4s6 (Fig. I). The radius of this cylinder is .\/%K. For the purpose of simplicity, it is sometimes advantageous to ascribe the values al/K = sl, az/K = s2, UD/K = SJ to the three coordinate axes instead of the principal stress alone. In this case, Eq. I becomes (*i - s*)1 + (s2 - S3)2 + (si - SiY = 2 [2] and the radius of the cylinder becomes \/%. In the latter method of representation, a point lying inside the cylinder indicates that the metal will react elasti-cally, whereas a point lying on the cylindrical surface indicates that the metal will behave plastically. Some of the geometric features of this cylinder are worthy of study. Let us inquire first as to what interpretation may be placed upon what we will choose to call the "circles of latitude" of the cylinder (L in Fig. I) and the "meridians" of the cylinder (M in Fig. I). Circles of Latitude Circles of latitude are formed by allowing a plane, passing perpendicular to the cylinder axis, to intersect with the cylinder. Any point, P, on this circle is presumed to have the coordinates sl, SZ, and s3. The coordinates of the point resulting from the intersection of the plane and the cylinder axis will be a, a, and a (since the cylinder axis is equally inclined to the three coordinate axes). L?t US now pass a line through the point on the circle and the point on the axis.

Jan 1, 1946

By William Marsh Baldwin

TWO of the most useful and important equations available to the metallurgist for the study of plastic deformation of metals are the Huber-von Mises-Henckyl-~ and the St. Venant7-10 equations. Huber-von Mises-Hengky Equation The Huber-von Mises-Hencky equation answers the question: When does plastic flow occur in metal that is subjected to a multi-axial stress? It occurs, according to this equation, when the three principal stresses,t UI, u2, and u3 satisfy the equation: (<ri - <r2)2 + (<r2 - <rsY + (ff! - <r3)* = 2Ki [i] Here K is the yield strength of the material as determined in an ordinary tensile test. If the quantities ul, 52, andas are assigned to the coordinates of a Cartesian three-dimensional system, this expression describes a cylinder whose axis of symmetry is inclined at equal angles to the three coordinate axes4s6 (Fig. I). The radius of this cylinder is .\/%K. For the purpose of simplicity, it is sometimes advantageous to ascribe the values al/K = sl, az/K = s2, UD/K = SJ to the three coordinate axes instead of the principal stress alone. In this case, Eq. I becomes (*i - s*)1 + (s2 - S3)2 + (si - SiY = 2 [2] and the radius of the cylinder becomes \/%. In the latter method of representation, a point lying inside the cylinder indicates that the metal will react elasti-cally, whereas a point lying on the cylindrical surface indicates that the metal will behave plastically. Some of the geometric features of this cylinder are worthy of study. Let us inquire first as to what interpretation may be placed upon what we will choose to call the "circles of latitude" of the cylinder (L in Fig. I) and the "meridians" of the cylinder (M in Fig. I). Circles of Latitude Circles of latitude are formed by allowing a plane, passing perpendicular to the cylinder axis, to intersect with the cylinder. Any point, P, on this circle is presumed to have the coordinates sl, SZ, and s3. The coordinates of the point resulting from the intersection of the plane and the cylinder axis will be a, a, and a (since the cylinder axis is equally inclined to the three coordinate axes). L?t US now pass a line through the point on the circle and the point on the axis.

Jan 1, 1946

By S. E. Maddigan, B. R. Zimmerman

Most metallurgists are well acquainted with the contributions already made to the study of metals by the use of X-rays. On the one hand, the radiographic method is constantly becoming of increasing importance as a nondestructive testing procedure, while on the other hand the techniques of X-ray diffraction have made important contributions to the fundamental knowledge in studies of phase diagrams, stress conditions, and so forth. A new, and as yet insufficiently appreciated, tool exists in the application of microradiography to alloy structures. This new procedure in many respects bears the same relation to microscopic investigations as does macroradiography to the gross inspection of metal surfaces. However, where macroradiography is used ordinarily to determine the soundness of the metal structure, this new method can be used not only to investigate micro-un-soundness but also to examine the distribution of the constituent elements within the body of the alloy. When combined with the normal procedures of microscopy, this offers a technique of great potential power. It is intended in this paper to present a few examples of copper-base alloys demonstrating the additional knowledge obtained from the microradiographic method. The detection of micro-unsoundness is demonstrated in Fig. I for a sample of cartridge brass as cast. The sample ap- peared quite sound when viewed under the microscope, but in reality was thickly populated with minute voids. This application of the method conforms in every way to conventional large-scale radiography and has been used to facilitate production of metal for vacuum devices.&apos; The true potentialities of the technique are revealed by comparison of Figs, 2a and 2b, which are respectively a photomicrograph and a microradiograph of a cast alloy of 80 per cent Cu, 10 per cent Sn, 10 per cent Pb. The remarkable difference in appearance provides some concept of the additional information this method may yield when used as an auxiliary to microscopic studies. Fig. 2a shows two phases of the copper-tin system plus segregated_ lumps of lead. Fig. 2b, on the other hand, shows with exceptional clarity the actual dendritic growth of the metal crystals during solidification. The practice of microradiography depends upon the laws of absorption of X-rays. This subject has been reviewed thoroughly in recent papers,l,2,3 but for clarity a brief resume will be given here. As is well known, when a beam of X-rays is transmitted through a, layer of homogeneous material, the intensity is reduced according to the relation: where Il is the transmitted intensity, I0 is the incident intensity, µ1 is the linear absorption coefficient of the material, t1 is the thickness of the material.

Jan 1, 1944

By S. E. Maddigan, B. R. Zimmerman

Most metallurgists are well acquainted with the contributions already made to the study of metals by the use of X-rays. On the one hand, the radiographic method is constantly becoming of increasing importance as a nondestructive testing procedure, while on the other hand the techniques of X-ray diffraction have made important contributions to the fundamental knowledge in studies of phase diagrams, stress conditions, and so forth. A new, and as yet insufficiently appreciated, tool exists in the application of microradiography to alloy structures. This new procedure in many respects bears the same relation to microscopic investigations as does macroradiography to the gross inspection of metal surfaces. However, where macroradiography is used ordinarily to determine the soundness of the metal structure, this new method can be used not only to investigate micro-un-soundness but also to examine the distribution of the constituent elements within the body of the alloy. When combined with the normal procedures of microscopy, this offers a technique of great potential power. It is intended in this paper to present a few examples of copper-base alloys demonstrating the additional knowledge obtained from the microradiographic method. The detection of micro-unsoundness is demonstrated in Fig. I for a sample of cartridge brass as cast. The sample ap- peared quite sound when viewed under the microscope, but in reality was thickly populated with minute voids. This application of the method conforms in every way to conventional large-scale radiography and has been used to facilitate production of metal for vacuum devices.&apos; The true potentialities of the technique are revealed by comparison of Figs, 2a and 2b, which are respectively a photomicrograph and a microradiograph of a cast alloy of 80 per cent Cu, 10 per cent Sn, 10 per cent Pb. The remarkable difference in appearance provides some concept of the additional information this method may yield when used as an auxiliary to microscopic studies. Fig. 2a shows two phases of the copper-tin system plus segregated_ lumps of lead. Fig. 2b, on the other hand, shows with exceptional clarity the actual dendritic growth of the metal crystals during solidification. The practice of microradiography depends upon the laws of absorption of X-rays. This subject has been reviewed thoroughly in recent papers,l,2,3 but for clarity a brief resume will be given here. As is well known, when a beam of X-rays is transmitted through a, layer of homogeneous material, the intensity is reduced according to the relation: where Il is the transmitted intensity, I0 is the incident intensity, µ1 is the linear absorption coefficient of the material, t1 is the thickness of the material.

Jan 1, 1944

By Shueling Woo, Charles S. Barrett, Robert F. Mehl

When one solid phase is generated from another, fixed and rational orientation relationships are observed to subsist between the parent and the new crystal. The principle has been proposed1 that the relationships obtaining between the same two phases are identical whatever the type of phase change involved, or whichever of the phases may act as parent. Many types of phase changes have been studied: allotropic transformations in pure metals, precipitation from solid solutions, eutectoid decompositions, peritectic reactions, the formation of oxide layers, and others2 Phase layers generated by diffusion of one metal into another constitute an additional type of reaction. This report provides new data on the orientation relationships occurring between phase layers formed by diffusion, in the Cu-Zn system,§ and furnishes further evidence in support of the principle. Materials and Methods The Cu-Zn system is especially suitable for these studies since the high vapor pres- sure of Zn provides an opportunity readily to create one phase poorer in Zn upon a parent phase richer in Zn by removing Zn by vaporization, or to reverse this process by adding Zn from Zn vapor; e.g., the beta phase can be found as a layer upon gamma by dezincing, or gamma can be found on beta by addition of Zn from Zn vapor. Since orientation relationships are to be sought, requiring crystals large enough for orientation determinations, it is convenient to prepare single crystals or large grains of the parent phase. The samples were prepared from oxygen-free high-conductivity copper and Horse Head zinc by melting under a borax flux in a graphite crucible. Large crystals of beta brass were grown by the strain-anneal method, in plates sectioned from the cast ingots, by the following procedure. Rockwell-hardness indents were made at I cm. intervals and with various loads, then the plates were annealed for 4 days at 700°C. in Nichrome boxes packed with beta-brass chips and graphite. Surface layers were removed by grinding and etching to a depth of about 1.0 mm., and individual grains were cut out. Crystals of alpha and gamma brass were prepared by freezing, by lowering a graphite crucible at speeds less than one inch per hour through a furnace held at a constant temperature above the melting point. Single crystals were cut out with a jeweler&apos;s saw, ground, polished and etched. Care was taken to remove cold-worked layers from the finished crystals

Jan 1, 1944

By Charles S. Barrett, Robert F. Mehl, Shueling Woo

When one solid phase is generated from another, fixed and rational orientation relationships are observed to subsist between the parent and the new crystal. The principle has been proposed1 that the relationships obtaining between the same two phases are identical whatever the type of phase change involved, or whichever of the phases may act as parent. Many types of phase changes have been studied: allotropic transformations in pure metals, precipitation from solid solutions, eutectoid decompositions, peritectic reactions, the formation of oxide layers, and others2 Phase layers generated by diffusion of one metal into another constitute an additional type of reaction. This report provides new data on the orientation relationships occurring between phase layers formed by diffusion, in the Cu-Zn system,§ and furnishes further evidence in support of the principle. Materials and Methods The Cu-Zn system is especially suitable for these studies since the high vapor pres- sure of Zn provides an opportunity readily to create one phase poorer in Zn upon a parent phase richer in Zn by removing Zn by vaporization, or to reverse this process by adding Zn from Zn vapor; e.g., the beta phase can be found as a layer upon gamma by dezincing, or gamma can be found on beta by addition of Zn from Zn vapor. Since orientation relationships are to be sought, requiring crystals large enough for orientation determinations, it is convenient to prepare single crystals or large grains of the parent phase. The samples were prepared from oxygen-free high-conductivity copper and Horse Head zinc by melting under a borax flux in a graphite crucible. Large crystals of beta brass were grown by the strain-anneal method, in plates sectioned from the cast ingots, by the following procedure. Rockwell-hardness indents were made at I cm. intervals and with various loads, then the plates were annealed for 4 days at 700°C. in Nichrome boxes packed with beta-brass chips and graphite. Surface layers were removed by grinding and etching to a depth of about 1.0 mm., and individual grains were cut out. Crystals of alpha and gamma brass were prepared by freezing, by lowering a graphite crucible at speeds less than one inch per hour through a furnace held at a constant temperature above the melting point. Single crystals were cut out with a jeweler&apos;s saw, ground, polished and etched. Care was taken to remove cold-worked layers from the finished crystals

Jan 1, 1944

By David J. Mack

A survey and critical appraisal of published information about Young&apos;s modulus was originally made by the writer because of a complete lack of information about this very important quantity in works on. mechanics, physical metallurgy, physics, and other sciences. It was felt that a comprehensive summary of such information about Young&apos;s modulus might be of general interest and may suggest new problems or lines of attack on other problems that involve E. Hence this paper has been prepared even though it is only a review, with no new ideas or experimental data. The references are only those used in assembling the paper. No attempt was made to compile a complete bibliography on the subject of Young&apos;s modulus. CalculatioX oP YouNg&apos;s Modulus from Theoretical or Empirical CoNsidera-tions Many attempts have been made to compute E from theoretical considerations. The earliest calculations were probably those of Tomlenson (1883) and Souther-land (1891), but Fess&apos;enden4&apos;,~ made extensive calculations a few years later and arrived at the relationship: £ = 78.TOw(i)* where V is the atomic volume. In 1923, Peczalski, working from the same standpoint but with more information available on atomic structure, arrived at an identical relationship, which he expressed as: where B is a constant of value about 8 . 107, p is density and mis atomic weight; the atomic volume, of course, being ml p. Portevind4 immediately pointcd out that while the equations of Fessenden and Peczalski were true of the common metals, they gave low values for the refractory metals with high moduli (Fig. I). He showed (Fig. 2) that much better concordance was obtained by means of an empirical equation of the form: F- KT" where K is a constant; T the absolute melting point; V, atomic volume, and a and b constants of value approximately I and 2 respectively. This constant K in the Portevin equation is not necessarily the same for all elements, as shown by Thompson. Other equations for E based upon theoretical considerations have been derived by Honda and Yamada49 and Lasareff.50 The most recent calculations of elastic moduli based upon quantum mechanics are probably those of Fuchs He extended the method of Wigner and Seitz for calculating the lattice energy and compressibility of monovalent metals and computed the elastic constants of lithium, 18

Jan 1, 1946

By Walter V. Knopp, Laurence Delisle

The aim of this work was the preparation of nickel-steels from elemental metal powders by powder metallurgy techniques. It was known that plain carbon steels could be made from a mixtufe of iron powder and graphite and that the effect of carbon on iron in powder form was of the same nature as that produced in fusion metallurgy. The problem in making nickel steels from elemental powders consisted therefore in finding out whether sufficient diffusion of the nickel and other incidental metals . normally present in such steels could be induced in the solid state to modify the properties of plain carbon steels made from powders and produce the beneficial effect of alloying. The composition selected originally was that of an S.A.E. 2330 steel. Metal powders, in the proportion correspending to that composition, were mixed with graphite, pressed, and heated at different temperatures for different periods of time, to produce bonding of the metal particles and mutual diffusion of the various elements without melting. Temperatures up to 1325°C and sintering periods as long as 6 hr were first investigated because it was expected.that such conditions would produce maximum diffusion with an accompanying improvement in the properties of the alloy. It was found that, although diffusion proceeded to a large extent under the conditions investigated, it would not be complete unless sintering were carried out at a high temperature for much longer than 6 hr. Relatively high temperatures and long sintering times are objectionable from a practical point of view, particularly when a low COSt material is to be produced, because they necessitate the use of special, costly equipment. Work could be done to improve the diffusion of iron and nickel by changing conditions other than the sintering temperature and time, that is, finer primary or alloy powders could be used. However, a marked change in the properties of the steel had been observed even with only partial diffusion. It was thought, therefore, that instead of trying to improve the diffusion, advantage might be taken of its incompleteness to produce a special structure consisting, in the unquenched condition, of a hard constituent, rich in nickel, dispersed in a tough pearlitic matrix. Steels with such a structure, not readily obtainable by fusion, should have desirable mechanical properties. Besides, it should be possible to prepare them from elemelltal powders under economical conditions. This latter alternative was therefore adopted for the second phase of this work. This report is divided into four parts: I. General Procedure. 2. Effect of Sintering Temperature. 3. Effect of Varying the Nickel Content. 4. Effect of Alloying Elements. General Procedure The general technique of cold pressing as used in powder metallurgy was applied.

Jan 1, 1949

By Bernard Kopelman

The particle size of tungsten metal powder used to make tungsten wire for use in radio tubes and incandescent lamps must be closely controlled if the highly desirable feature of nonsagging is to be achieved. Our knowledge of factors affecting the particle size of tungsten powder has been limited by lack of any extensive literature on the subject. There are no publications in the English language discussing this problem in any but the most general terms. In this paper the published experimental information on this subject is reviewed. Based on the published data and some experimental data obtained by the author, a general theory of factors affecting the particle size of tungsten metal powder obtained by reduction of the oxides in hydrogen is offered. The various forms of the tungsten oxides and tungsten metal used in the experiments described were those prepared by commercial processes, so that the experimental results obtained on a laboratory scale would be more directly applicable to actual commercial reduction conditions. The effects of time of reduction, temperature. and concentration of water vapor in the hydrogen were observed by counting microscopically the particle distribution obtained. Such a method is very time-consuming, but the data obtained by this method are more reliable and more fundamental than those obtained by any of the several instruments available for measurement of particle size. Review of the Literature Until the year 1912, tungsten powder was prepared commercially by reducing tungstic oxide in the presence of carbon or one of its compounds (such as glycerin or ethylene glycol), usually by firing the mixture in a closed fire-clay crucible. The resultant powder contained about 95 per cent tungsten.&apos; When reduction of tungsten oxides by H² was introduced Commercially,²,³ several investigators became concerned with the equilibria between tungsten metal and its several oxides in an atmosphere of hydrogen and water vapor.4-l3 While these many investigations were in fair agreement on the equilibria WO³ + H2 = WO2 + H2O and WO2 + 2H2 = W + 2H2O there arose considerable controversy as to the chemical composition of the oxide between WO³ and WO², because of very poor agreement on the equilibrium constant of this intermediate oxide reduction reaction. The controversy on this intermediate oxide has been in progress for more than 100 years. Thus Malguti,14 in 1835, decided it was WO2.56 In 1857, Riche15 proposed the formula W³O8. Usler,16 in 1865, confirmed the existence of WsO8 and further proposed W1O1l. In 1897, Desil7 agreed upon W²O8 but also found W5O14.

Jan 1, 1947

By Bernard Kopelman

The particle size of tungsten metal powder used to make tungsten wire for use in radio tubes and incandescent lamps must be closely controlled if the highly desirable feature of nonsagging is to be achieved. Our knowledge of factors affecting the particle size of tungsten powder has been limited by lack of any extensive literature on the subject. There are no publications in the English language discussing this problem in any but the most general terms. In this paper the published experimental information on this subject is reviewed. Based on the published data and some experimental data obtained by the author, a general theory of factors affecting the particle size of tungsten metal powder obtained by reduction of the oxides in hydrogen is offered. The various forms of the tungsten oxides and tungsten metal used in the experiments described were those prepared by commercial processes, so that the experimental results obtained on a laboratory scale would be more directly applicable to actual commercial reduction conditions. The effects of time of reduction, temperature. and concentration of water vapor in the hydrogen were observed by counting microscopically the particle distribution obtained. Such a method is very time-consuming, but the data obtained by this method are more reliable and more fundamental than those obtained by any of the several instruments available for measurement of particle size. Review of the Literature Until the year 1912, tungsten powder was prepared commercially by reducing tungstic oxide in the presence of carbon or one of its compounds (such as glycerin or ethylene glycol), usually by firing the mixture in a closed fire-clay crucible. The resultant powder contained about 95 per cent tungsten.&apos; When reduction of tungsten oxides by H² was introduced Commercially,²,³ several investigators became concerned with the equilibria between tungsten metal and its several oxides in an atmosphere of hydrogen and water vapor.4-l3 While these many investigations were in fair agreement on the equilibria WO³ + H2 = WO2 + H2O and WO2 + 2H2 = W + 2H2O there arose considerable controversy as to the chemical composition of the oxide between WO³ and WO², because of very poor agreement on the equilibrium constant of this intermediate oxide reduction reaction. The controversy on this intermediate oxide has been in progress for more than 100 years. Thus Malguti,14 in 1835, decided it was WO2.56 In 1857, Riche15 proposed the formula W³O8. Usler,16 in 1865, confirmed the existence of WsO8 and further proposed W1O1l. In 1897, Desil7 agreed upon W²O8 but also found W5O14.

Jan 1, 1947

By A. J. Shaler, J. Prieto Isaza, J. Wulff

Tantalum metal has a number of unique properties which give it widespread application in modern technology and in research. In electronic apparatus involwing high temperatures in vacuo some of the refractory metals 6ecome brittle. Tantalum retains its ductility at elevated temperatures, and this property, together with its low vapor pressure and its ability to absorb gases, make it important in this field. Its chemical inertness in the presence of acids, halogens, and other corrosive media, makes it useful in chemical apparatus and in neuro and orthopedic surgical applications. As an addition to tungsten carbide in steel-cutting grades of cemented-carbide tools, the carbides of tantalum and of its sister element colum-bium have found considerable use. The present-day method1 of manufacturing tantalum is to sinter a powder compact of the metal in vacuo. Because tantalum-columbium alloys are difficult to work and since tantalum ores almost always contain columbium, the two metals must be separated chemically, the products of the separation being generally in the form of potassium tantalum fluoride and potassium columbium oxyfluoride. These salts are used in fused-salt electrolytic baths from which coarse metallic powder is deposited as a sponge at the cathode. Finer powder can be made from the coarse product or from tantalum scrap by first submitting it to an embrittling heat treatment in hydrogen and then crushing it. The fine hydrogen-containing powder may subsequently be degassed in vacuo at a high temperature. Prompted by the success of others2,3 in the magnesium reduction of titanium and zirconium halides; one of the authors undertook4 an investigation of the thermochemistry of the reaction between solid magnesium and gaseous tantalum penta-chloride, a subject which had not previously been studied. He found that the heat of formation of tantalum pentachloride is approximately 364,250 cal per mol at temperatures lower than the melting point of magnesium. A value of 83 units was found for the standard entropy at these temperatures. With these values, it was shown that magnesium and tantalum pentachloride are capable of reacting exo-thermically at temperatures less than the melting point of magnesium, and that no great violence is to be expected when these substances are heated together. The exothermic nature of the reaction indicated that the Drocess should be efficient and should not require much externally applied energy. Tantalum pentachloride is not commonly made commercially, and any process using it therefore involves the subsidiary problem of producing and handling this substance. A series of experiments was carried out in which dried chlorine saturated with carbon tetrachloride was passed over heated tanta-

Jan 1, 1949

By Clarence Zener

It is customary to regard the stress-strain relation as consisting of two parts, thc elastic region and the plastic region. The essential attribute of the plastic region is the presence of a permanent set, which remains upon removal of all stresses. The essential attribute of the elastic region is the absence of such a permanent set. Absence of a permanent set does not imply a linear relation between stress and strain, nor even a single valued relation. In fact, in no real metal is stress a single valued function of strain in the elastic region. The property of a solid in virtue of which stress and strain are not uniquely related in the elastic range will be called "anelasticity." The purpose of the present article is to review and correlate the past work upon the anelasticity of metals. The following paper by W. A. West124 describes investigations upon anelastic properties of iron. Many manifestations of anelasticity have been observed, the first as early as 1835 by Weber.l,2 In his experiments Weber subjected a specimen to a constant load (or deformation) for a given time, and then suddenly removed the load. He observed that most of the deformation suddenly disappeared, but that there remained a residual deformation, which disappeared only gradually with time, as is illustrated in Fig. I. The occurrence of a residual deformation which only gradually disappeared, Weber called the elastic after-effect (Elastische Nackwir-kung). An extensive review of the early work upon elastic after-effects has been given by Auerbach.3 Another manifestation of anelasticity is the dependence of the elastic constants---e.g., Young&apos;s modulus— upon the method of measurement. Thus, if dynamic methods are used, the measured value will depend upon the frequency of oscillation. Still another manifestation is dissipation of energy attending vibration, called damping or internal friction. One objective. of metallurgical science is the understanding of the plastic and fracture properties of metals in terms of their microstructure. Through such an understanding will come the ability to design microstructure to give the desired mechanical properties. A study of anelasticity will furnish an invaluable aid in the attainment of this objective. Such studies, when properly guided, yield information regarding the relation between stress and strain in the individual components of the microstructure. In order, however, that this type of information may be obtained, it is necessary that the experimental studies of anelasticity be interpreted by the appropriate mathematical analysis. This article, therefore, starts with the mathematical formulation of anelasticity.

Jan 1, 1947

By Clarence Zener

It is customary to regard the stress-strain relation as consisting of two parts, thc elastic region and the plastic region. The essential attribute of the plastic region is the presence of a permanent set, which remains upon removal of all stresses. The essential attribute of the elastic region is the absence of such a permanent set. Absence of a permanent set does not imply a linear relation between stress and strain, nor even a single valued relation. In fact, in no real metal is stress a single valued function of strain in the elastic region. The property of a solid in virtue of which stress and strain are not uniquely related in the elastic range will be called "anelasticity." The purpose of the present article is to review and correlate the past work upon the anelasticity of metals. The following paper by W. A. West124 describes investigations upon anelastic properties of iron. Many manifestations of anelasticity have been observed, the first as early as 1835 by Weber.l,2 In his experiments Weber subjected a specimen to a constant load (or deformation) for a given time, and then suddenly removed the load. He observed that most of the deformation suddenly disappeared, but that there remained a residual deformation, which disappeared only gradually with time, as is illustrated in Fig. I. The occurrence of a residual deformation which only gradually disappeared, Weber called the elastic after-effect (Elastische Nackwir-kung). An extensive review of the early work upon elastic after-effects has been given by Auerbach.3 Another manifestation of anelasticity is the dependence of the elastic constants---e.g., Young&apos;s modulus— upon the method of measurement. Thus, if dynamic methods are used, the measured value will depend upon the frequency of oscillation. Still another manifestation is dissipation of energy attending vibration, called damping or internal friction. One objective. of metallurgical science is the understanding of the plastic and fracture properties of metals in terms of their microstructure. Through such an understanding will come the ability to design microstructure to give the desired mechanical properties. A study of anelasticity will furnish an invaluable aid in the attainment of this objective. Such studies, when properly guided, yield information regarding the relation between stress and strain in the individual components of the microstructure. In order, however, that this type of information may be obtained, it is necessary that the experimental studies of anelasticity be interpreted by the appropriate mathematical analysis. This article, therefore, starts with the mathematical formulation of anelasticity.

Jan 1, 1947

By William A. West

One manifestation of anelastic properties in solids is the mechanical elastic aftereffect, which may be described briefly as follows: If a stress is applied to a solid body, a deformation or strain is produced. On removal of the stress, this deformation disappears, at least in part. As a first approximation, this appearance or disappearance of deformation usually has been considered instantaneous. Actually, however, for a very wide variety of substances, on application of stress the instantaneous deformation is followed by a further slow yielding, which continues, although at a rapidly diminishing rate, for as long as the stress is applied. Similarly, on removal of the stress, the instantaneous recovery from deformation is followed by a further slow recovery, which continues, although at a rapidly diminishing rate, often for a long time. This latter phenomenon has been called the "elastic after-effect." Experiments upon the elastic after-effect in metals, when properly designed and when properly interpreted, are capable of giving quite precise information regarding the relation between stress and strain in the various constituent parts of the metal. For example, if certain parts of the metal, such as grain boundaries or slip bands, behave in a viscous manner—that is, if therein—the relaxation spectrum will contain lines or bands associated with the relaxation of shear stress within these parts. No attempts have heretofore been made to utilize elastic after-effects for obtaining such detailed information. The purpose of the present paper is to explore the possibilities of properly designed and interpreted experiments on the elastic aftereffect in metals. Since new procedures and principles are employed in this study, an attempt has been made to record each step taken. Elastic after-effect observations are susceptible of simple interpretation only when the stress level employed is so low that all effects are linear with the stress. Just how low the stress level must be can he determined only by experiment. An advnntage, other than simple interpretation, is associated with low stress levels. When all effects are linear, derived quantities, such as the relaxation spectrum, are independent of the stress distribution. It is, furthermore, possible to employ the type of deformation that is most convenient from the experimental standpoint; for example torsion. It appears that in experiments involving both loading and unloading the following would be observed: I. Instantaneous deformation, recoverable instantaneously in whole, or in part. 2. Delayed deformation, recoverable slowly in whole, in part, or not at all. 3. Permanent deformation, the difference between total deformation and total recovery. In the work here described, unloading experiments only were made. Wires were

Jan 1, 1947

By William A. West

One manifestation of anelastic properties in solids is the mechanical elastic aftereffect, which may be described briefly as follows: If a stress is applied to a solid body, a deformation or strain is produced. On removal of the stress, this deformation disappears, at least in part. As a first approximation, this appearance or disappearance of deformation usually has been considered instantaneous. Actually, however, for a very wide variety of substances, on application of stress the instantaneous deformation is followed by a further slow yielding, which continues, although at a rapidly diminishing rate, for as long as the stress is applied. Similarly, on removal of the stress, the instantaneous recovery from deformation is followed by a further slow recovery, which continues, although at a rapidly diminishing rate, often for a long time. This latter phenomenon has been called the "elastic after-effect." Experiments upon the elastic after-effect in metals, when properly designed and when properly interpreted, are capable of giving quite precise information regarding the relation between stress and strain in the various constituent parts of the metal. For example, if certain parts of the metal, such as grain boundaries or slip bands, behave in a viscous manner—that is, if therein—the relaxation spectrum will contain lines or bands associated with the relaxation of shear stress within these parts. No attempts have heretofore been made to utilize elastic after-effects for obtaining such detailed information. The purpose of the present paper is to explore the possibilities of properly designed and interpreted experiments on the elastic aftereffect in metals. Since new procedures and principles are employed in this study, an attempt has been made to record each step taken. Elastic after-effect observations are susceptible of simple interpretation only when the stress level employed is so low that all effects are linear with the stress. Just how low the stress level must be can he determined only by experiment. An advnntage, other than simple interpretation, is associated with low stress levels. When all effects are linear, derived quantities, such as the relaxation spectrum, are independent of the stress distribution. It is, furthermore, possible to employ the type of deformation that is most convenient from the experimental standpoint; for example torsion. It appears that in experiments involving both loading and unloading the following would be observed: I. Instantaneous deformation, recoverable instantaneously in whole, or in part. 2. Delayed deformation, recoverable slowly in whole, in part, or not at all. 3. Permanent deformation, the difference between total deformation and total recovery. In the work here described, unloading experiments only were made. Wires were

Jan 1, 1947

By E. A. Nesbitt

A new permanent-magnet material has been developed with unusual mechanical as well as magnetic properties. Specimens that have been cast or subjected to a small amount of hot reduction by rolling or swaging may be machined, punched, tapped or drilled. The composition range of the alloys is 30 to 52 per cent iron, 36 to 62 per cent cobalt and 4 to 16 per cent vanadium. After being either quenched, annealed or given the usual cold finishing passes and then heated for 2 hr. at 600°C., such materials have a magnetic energy product of 1.0 X 106 gauss-oersteds. This product is equivalent to that of the well-known Honda steel (36 per cent Co, 4W, 2 Cr, 0.8 C. 0.3 Mn, balance Fe). Material handled in the manner just described does not depend on cold-working for its magnetic properties, and is known as Vicalloy I. The preferred composition for Vicalloy I is 38.5 per cent iron, 52 per cent cobalt and 9.5 per cent vanadium. When the alloys are first hot-worked, then considerably reduced in area by cold-swaging, drawing or groove rolling and then heat-treated, the magnetic energy product measured in the direction of previous extension is increased to 2.0 to 3.5 X 106 gauss-oersteds. These higher values have been obtained only after cold reductions in area of 75 to 95 per cent. Material handled in this manner is known as Vicalloy II and the preferred composi-

Jan 1, 1947