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

Jan 1, 1946

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

Jan 1, 1946

By J. H. Frye, C. P. Sun

A Frimary substitutional solid solution is a solution that has the same crystalline structure as the solvent metal, and in which solute atoms have replaced, solvent atoms at random on the host lattice. This replacement usually results in an increase in hardness as measured by conventional penetration tests. The factors controlling this hardness increase have been investigated in some detail for copper and silver alloys.1-5 It has been shown that at least four factors are involved: (1) concentration of solute, (2) row of the periodic table from which the solute is taken, (3) increase in lattice parameter of the solvent produced by the solute, and (4) work-hardening produced by penetration of the hardness indenter.2,4 The last factor is of the utmost importance. An investigation of the available data2,4 leads to the conclusion that the solutes that produce large hardness increases in copper or silver do so principally because they increase the rate of work-hardening. Furthermore, it is doubtful whether any solute produces appreciable hardening in the absence of plastic deformation and hence work-hardening. Thus it is clear that an understanding of the effect of solutes on rate of work-hardening is essential to an understanding of the hardness of solid solutions. This effect of solutes is also important in forming operations such as rolling or deep drawing. The presence of elements that confer rapid rates of work-hardening will increase power consumption and may well decrease the amount of deformation possible between anneals. This paper is the report of an investigation of the factors that control rates of work-hardening in copper and silver solid solutions. The silver and copper alloys considered are those in which all solutes are from the B subgroups or second short period of the periodic table. Experience with hardness, with structure of alloys, and with electrical conductivity has proved that results of a fundamental nature are most likely to be obtained if alloys are made up on the basis of the positions of the constituent elements in the periodic table. In previous work, Meyer analysis data on high-purity copper and silver solid solutions were obtained through careful measurements with fully calibrated equipment and these data were corrected to correspond to a standard grain size. From these corrected Meyer analysis data rates of work-hardening have now been calculated. Calculation of Rates as Work- HARDENING The Meyer analyses, on which this study of rates of work-hardening is based, consisted in determining impression

Jan 1, 1944

By J. H. Frye, C. P. Sun

A Frimary substitutional solid solution is a solution that has the same crystalline structure as the solvent metal, and in which solute atoms have replaced, solvent atoms at random on the host lattice. This replacement usually results in an increase in hardness as measured by conventional penetration tests. The factors controlling this hardness increase have been investigated in some detail for copper and silver alloys.1-5 It has been shown that at least four factors are involved: (1) concentration of solute, (2) row of the periodic table from which the solute is taken, (3) increase in lattice parameter of the solvent produced by the solute, and (4) work-hardening produced by penetration of the hardness indenter.2,4 The last factor is of the utmost importance. An investigation of the available data2,4 leads to the conclusion that the solutes that produce large hardness increases in copper or silver do so principally because they increase the rate of work-hardening. Furthermore, it is doubtful whether any solute produces appreciable hardening in the absence of plastic deformation and hence work-hardening. Thus it is clear that an understanding of the effect of solutes on rate of work-hardening is essential to an understanding of the hardness of solid solutions. This effect of solutes is also important in forming operations such as rolling or deep drawing. The presence of elements that confer rapid rates of work-hardening will increase power consumption and may well decrease the amount of deformation possible between anneals. This paper is the report of an investigation of the factors that control rates of work-hardening in copper and silver solid solutions. The silver and copper alloys considered are those in which all solutes are from the B subgroups or second short period of the periodic table. Experience with hardness, with structure of alloys, and with electrical conductivity has proved that results of a fundamental nature are most likely to be obtained if alloys are made up on the basis of the positions of the constituent elements in the periodic table. In previous work, Meyer analysis data on high-purity copper and silver solid solutions were obtained through careful measurements with fully calibrated equipment and these data were corrected to correspond to a standard grain size. From these corrected Meyer analysis data rates of work-hardening have now been calculated. Calculation of Rates as Work- HARDENING The Meyer analyses, on which this study of rates of work-hardening is based, consisted in determining impression

Jan 1, 1944

By David J. Mack

A survey and critical appraisal of published information about Young'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'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's modulus. CalculatioX oP YouNg'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'enden4',~ 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

26. G. H. S. Price, S. V. Williams, and G. J.O. Garrard: Heavy alloy, its production. properties and uses. Metal Industry (1941) 599 354s 372. 394. 27. R. Kieffer and W. Hotop: p. 320 of ref 12. 28. F. R. Hensel. E. I. Larsen, and E. F. Swazy: Physical properties of metal compositions with a refractory metal base. Chap. 42, 483, Powder Metallurgy, ed. by J. Wulff (1942) Cleveland. 29. R. Kieffer and W. Hotop: p. 290 of ref. 12. 30. H. Freundlich: Kapillarchemie. 211 (1923) Leipzig. 31. W. Ostwald: Zisch. f. Phys. Chemie. (1900) 34, 503. 32. G. A. Hulett: Zisch. f. Phys. Chemie. (1901) 37. 385; and (1904) 47, 357. 33. J C. Chaston: Discussion to Price, Smithells and Williams, p. 257 of ref. 4. 34. W. Dawihl: Untersuchungen ueber die Vorgaenge bei der Abnuetzung von Hartmetallwerkzeugen. Ztsch. f. techn. Phys. (1940) 21 336. 35. W. Dawihl and J. Hinnueber: Ueber den Aufbau der Hartmetallegierungen. Kol-loidzlsch. (1943) 104, 233. 36. F. Skaupy: Dispersoidchemische und verwandte Gesichtspunkte bei Sinter-hartmetallen. Kolloidzlsch. (1942) 98, 92; and (1943) 102, 269. 37. F. C. Kellcy: Cemented tantalum car- bide tools. Trans. ASST (1932) 19, 233. 38. E. W. Engle: Cemented carbides. Chap. 39, 436, Powder Metallurgy, ed. by J. Wulff (1942) Cleveland. 39. W. Dawihl: Zlsch. f. Melallkunde. (1940) 32, 320. 40. P. M. McKenna: Tool Materials (Ce- mented Carbides). Chap. 40. 454. Powder Metallurgy, ed. by J. Wulff (1942) Cleveland. 41. G. A. Meerson. G. L. Sverev, B. Y. Osinovskaja: Zhurnal Prikladnoi Khimii. (1930) 139 66. 42. A. G. Metcalfe: The mutual solid solubility of Tunesten Carbide and Titanium carbide- Metal Trealmenl (1946) 13, 127. 43. P. Schwarzkopf: Powder Metallurgy. 196-201 and 354-356 (1947) New York. 44. H. Burden: The manipulation and sintering of hard-metals. Special Rep. No. 38, p. 78. Iron and Steel Inst.. 1947. London. 45. W. D. Jones: Principles of powder metal- lurgy. 150. (1937) London. 46. J. E. Drapeau: Sintering of powdered copper-tin mixtures. Chap. 32. 332, Powder Metallurgy, ed. by J. Wulff (1942) Cleveland. 47. H. E. Hall: Sintering of copper and tin powder. Metals and Alloys (1939) 10, 297. 48. F. Sauerwald: Present status of powder metallurgy. -.Melallwirlschafl. (1941) 20, 649. 671. 49. H. L. Wain: Powder metallurgy; influence of some processing variables on the properties of sintered bronze. Report ACA-25. Australian Council for Aeronautics (1946) Melbourne. 50. S. L. Hoyt: Constitution of copper-tin alloys. Metals Handhook, 1364. (1939) Cleveland. 51. T. Ishikawa: Studies on the interdiffusion of copper, tin and graphite powders. Nippon Kinzoku Gakkai-Si (1937) I, 226. 52. A. Carter and A. G. Metcalfe. The struc- ture of porous bronze bearings. Special Rep. No. 38, p. 99. Iron and Stecl Inst. (1947) London. 53. R. P. Koehring: Sintering atmospheres for production purposes. Chap. 25, 278. Powder Metallurgy, ed. by J. Wulff (1942) Cleveland. 54. C. G. Goetzel: Some properties of sintcred and hotpressed copper tin compacts. Trans. AIME (1945) 161, 569. 55. J. W. Lennox: The production of some non ferrous engineering components by powder metallurgy. Special Rep. No. 38. p. 174. Iron and Steel Inst., 1947, London. . P. Duwez and H. E. Martens: The power metallurgy of porous metals and alloys having a controlled porosity. TP 2343, Metals Tech. April 1948. This volume. p. 848. 57. E. A. Owen and L. Pickup: X-ray study of the interdiffusion of copper and zinc. Proc. Royal Soc., London, Series A. (1935) 149, 283. 58. C. G. Goetzel: Sintered and hotpressed compacts of copper-zinc powder. Chap. 34. 352, Powder Metallurgy, ed. by J. Wulff (1942) Cleveland. 98, R. Chadwick. E. R. Broadfield, and S. F. Pugh: Observations on the pressing. sintering, and properties of iron-copper powder mixtures. Special Rep. No. 38, p. 151, Iron and Steel Inst. (1947) London. 60. A. Squire: The properties of iron-copper compacts. Watertown Arsenal Lab. Rep. WAL No. 67101. 61. F. C. Kelley: Properties of sintered iron- comer uowder. Iron Age (Aug. 15. 193) 158 57. 62. G. H. Howe: Sinterinn of Alnico. Iron Age (Jan. 11. 1940) 14.5, 27. 63. R. Kieffer and W. Hotop: p. 359 of ref. 12. 64. W. Hotop: Permanent magnets from sintered iron-nickel-aluminum. Stahl und Eisen (1941) 61, 1105. 65. P. R. Kalischer: Some experiments in the production of aluminum-nickel-iron alloys by powder metallurgy. Trans. AIME (1941) 145, 369. 66. S. J. Garvin: Production of sintered per- manent magnets. Special Rep. NO. 38. p. 67. Iron and Steel Inst. 1947, London. 67. F. C. Kelley: Discussion to P. R. Kalischer. p. 375 of ref. 65. 68. R. Kieffer and W. Hotop: p. 357 of ret, 12. 69. C. H. Howe: Sintered alnico. Chapter 48, 530, Powder Metallurgy, ed. by J. Wulff (1942) Cleveland. Powder Metallurgy Seminar (C. G. Goetzel presiding) C. G. Goetzel—The seminar has been opened by a man who has been active in the field for over fourteen years and has made, since then, some major contributions to the advancement of the art. After having been associated with the Moraine Products Division of General Motors Corporation for over ten

Jan 1, 1949

By Alexander Squire

One of the principal factors that have contributed to the hesitancy of design engineers to use metal-powder parts is the difficulty experienced in the determination of the mechanical properties of compacted components. Because standard test methods cannot usually be applied in the inspection of such parts, and because adequate special test methods have not been developed, it has been considered desirable to investigate the methods that are applicable. These may then be included in specifications for metal-powder materials and components in order that the design engineer may be assured that the subject parts possess the desired mechanical properties for satisfactory performance. It is known that direct relationships exist between usually nonmeasurable properties as tensile strength and elongation and shear strength and the angle through which compacts may be plastically deformed before fracturing. These correlations are valuable in the inspection of specific parts, but it is necessary to set up standards before they may be satisfactorily employed. Apart from the use of correlations, the number and character of the inspection methods that are applicable to almost all powder parts is limited to three—chemical analysis, density, and hardness. The last of these may or may not be a pertinent characteristic, since the indentation hardness of many powdeied-metal materials is so low as to have little significance. It is, however, occasionally desirable to use hardness measurements as an indication of the uniformity of the structure of pieces of a given type. Chemical analysis reveals very little about the physical properties of metal-powder compacts, since the unpressed powder is usually of a composition almost identical with that of the finished pieces. Density determinations are simple to perform and have the advantage of being nondestructive in character. If the dimensions of a machine part are known (and usually they are), the average density may be determined by weighing a given number of pieces and dividing by the calculated volume of the parts. More accurate measurements may be made by the water-displacement method. It is recognized that mechanical properties of metal-powder materials are related to their density, but usually these relations are determined for only one type of powder, processed under a given set of conditions. Comparisons of the pioperties of compacts formed from different types of powders are made on the basis of compacting pressures instead of density, and for this reason the results obtained by using powders of different types appear widely variant.

Jan 1, 1947

By Alexander Squire

One of the principal factors that have contributed to the hesitancy of design engineers to use metal-powder parts is the difficulty experienced in the determination of the mechanical properties of compacted components. Because standard test methods cannot usually be applied in the inspection of such parts, and because adequate special test methods have not been developed, it has been considered desirable to investigate the methods that are applicable. These may then be included in specifications for metal-powder materials and components in order that the design engineer may be assured that the subject parts possess the desired mechanical properties for satisfactory performance. It is known that direct relationships exist between usually nonmeasurable properties as tensile strength and elongation and shear strength and the angle through which compacts may be plastically deformed before fracturing. These correlations are valuable in the inspection of specific parts, but it is necessary to set up standards before they may be satisfactorily employed. Apart from the use of correlations, the number and character of the inspection methods that are applicable to almost all powder parts is limited to three—chemical analysis, density, and hardness. The last of these may or may not be a pertinent characteristic, since the indentation hardness of many powdeied-metal materials is so low as to have little significance. It is, however, occasionally desirable to use hardness measurements as an indication of the uniformity of the structure of pieces of a given type. Chemical analysis reveals very little about the physical properties of metal-powder compacts, since the unpressed powder is usually of a composition almost identical with that of the finished pieces. Density determinations are simple to perform and have the advantage of being nondestructive in character. If the dimensions of a machine part are known (and usually they are), the average density may be determined by weighing a given number of pieces and dividing by the calculated volume of the parts. More accurate measurements may be made by the water-displacement method. It is recognized that mechanical properties of metal-powder materials are related to their density, but usually these relations are determined for only one type of powder, processed under a given set of conditions. Comparisons of the pioperties of compacts formed from different types of powders are made on the basis of compacting pressures instead of density, and for this reason the results obtained by using powders of different types appear widely variant.

Jan 1, 1947

By Richard Paul Seelig

The following review covers published information on pressing of metal powders at room temperature. Only those operations are considered which occur between the time the powder is filled into the cavity and the compact is ejected from the die. Thus, this review does not concern hot pressing, coining or sizing feed or flow problems, commercial presses nor designs. It was also necessary to disregard to a large extent the effect of pressing on subsequent operations and on properties after sintering. 'The pressing operation is considered independently in its function to compact loose metal powder into useful shapes which can subsequently be handled. There are some comments by the writer in connection with a few of the findings quoted in the literature in order to stimulate thought and discussion. The selection of references quoted in the text is in some cases arbitrary although an attempt was made to favor papers containing novel ideas, techniques or results which mag stimulate future research. In order to enable the reader to check further into the subjects mentioned, the original, rather extensive, bibliography is appended even though not all the references are touched on in the printed version of this review. The equipment used by various workers, for example a die design created by Bridgman,22 is very interesting. 'The die insert has a conical external surface. The vertical pressure exerted on the punch transmits itself to the die which in turn is pushed harder into its tapered retainer. Thus, the higher the pressure exerted on the punch, the higher also the pressure exerted inwards on the die inserts. Inasmuch as this pressure counteracts the internal pressure from the compact the two stresses balance each other so that it is possible to obtain tremendous pressures without breaking the die. The die collar was made from an oil hardening tool steel, heat treated to a tensile strength of some 300,000 psi. The die was closed at the bottom by a plug made from special tool steels. Bridgman found that there is no steel which will withstand a com-pressive stress of 700,000 psi without continuous slow flow or immediate fracture. Therefore, the only material suitable for use in the pressing punch was sintered carbide. In view of the ingenious design it was possible to use special tool steel as die material. Jones22 raises the question whether this method of pressing has practical application in powder metallurgy. Although these tremendous pressures cannot readily be utilized without many special precautions, the tapered die and retainer idea is believed to be useful even for lower pressures. Bridgman, himself," alls attention to the fact that the properties

Jan 1, 1947

By Richard Paul Seelig

The following review covers published information on pressing of metal powders at room temperature. Only those operations are considered which occur between the time the powder is filled into the cavity and the compact is ejected from the die. Thus, this review does not concern hot pressing, coining or sizing feed or flow problems, commercial presses nor designs. It was also necessary to disregard to a large extent the effect of pressing on subsequent operations and on properties after sintering. 'The pressing operation is considered independently in its function to compact loose metal powder into useful shapes which can subsequently be handled. There are some comments by the writer in connection with a few of the findings quoted in the literature in order to stimulate thought and discussion. The selection of references quoted in the text is in some cases arbitrary although an attempt was made to favor papers containing novel ideas, techniques or results which mag stimulate future research. In order to enable the reader to check further into the subjects mentioned, the original, rather extensive, bibliography is appended even though not all the references are touched on in the printed version of this review. The equipment used by various workers, for example a die design created by Bridgman,22 is very interesting. 'The die insert has a conical external surface. The vertical pressure exerted on the punch transmits itself to the die which in turn is pushed harder into its tapered retainer. Thus, the higher the pressure exerted on the punch, the higher also the pressure exerted inwards on the die inserts. Inasmuch as this pressure counteracts the internal pressure from the compact the two stresses balance each other so that it is possible to obtain tremendous pressures without breaking the die. The die collar was made from an oil hardening tool steel, heat treated to a tensile strength of some 300,000 psi. The die was closed at the bottom by a plug made from special tool steels. Bridgman found that there is no steel which will withstand a com-pressive stress of 700,000 psi without continuous slow flow or immediate fracture. Therefore, the only material suitable for use in the pressing punch was sintered carbide. In view of the ingenious design it was possible to use special tool steel as die material. Jones22 raises the question whether this method of pressing has practical application in powder metallurgy. Although these tremendous pressures cannot readily be utilized without many special precautions, the tapered die and retainer idea is believed to be useful even for lower pressures. Bridgman, himself," alls attention to the fact that the properties

Jan 1, 1947

By Alexander Squire

A brief study of the effects of material and processing variations upon the tensile properties of steel formed from mixtures of iron and carbon was made in order to provide information regarding the properties obtainable in iron-carbon compacts as influenced by forming pressure, sintering temperature, and graphite particle size. Sintered steels formed from mixtures of iron and graphite have been studied by Stern,' who investigated the effect of various percentages of graphite on compacts formed from electrolytic iron that were repressed and heat-treated after sintering. A further study, by Stern and Greenberg,l is concerned with the heat-treatment of steels formed by the car-burization of iron compacts, and Margolies3 has reported work on the simultaneous sintering and carburization of iron-powder parts. Glauch4 investigated the effect of various types of graphite on the properties of iron-carbon powder alloys but did not determine the effect of different particle sizes of the same graphite alloyed with different types of powder. In the investigation reported in this paper, powders typical of those produced by electrolytic deposition and the decar-burization of shotted steel scrap were used. The powders were mixed by tumbling in a jar mill with graphite powder ground to an average particle diameter of 2, 4, 6, and 16 microns (as determined by microscopic measurement). The properties of the iron and graphite powders are presented in tabular form as Table I. In order to obtain the maximum information from a minimum number of test specimens, the study was divided into two sections with one set of specimens treated identically in each section as a basis for comparison. In the first section, iron powder produced by the shotting and subsequent decarburization of scrap steel was mixed with 2-micron graphite powder, pressed at 50,000, 100,-000, and 200,000 psi, and sintered in hydrogen at 1200°C for the periods of time ranging from 15 to 120 minutes. In the second section of the investigation, electrolytic iron powder was mixed with graphite of an average particle diameter of 2, 4, 6, and 16 microns, pressed at 100,000 psi, and sintered at temperatures ranging from 1000° to r200°C'. for periods of time of 30 to 180 minutes. By following this procedure an indication of the effect of the following variables upon the density and tensile properties of iron-carbon powder compacts was obtained: (I) forming pressure, (2) sintering time, (3) particle size of graphite powder, (4) sintering temperature, (4) type of iron powder.

Jan 1, 1947

By Alexander Squire

A brief study of the effects of material and processing variations upon the tensile properties of steel formed from mixtures of iron and carbon was made in order to provide information regarding the properties obtainable in iron-carbon compacts as influenced by forming pressure, sintering temperature, and graphite particle size. Sintered steels formed from mixtures of iron and graphite have been studied by Stern,' who investigated the effect of various percentages of graphite on compacts formed from electrolytic iron that were repressed and heat-treated after sintering. A further study, by Stern and Greenberg,l is concerned with the heat-treatment of steels formed by the car-burization of iron compacts, and Margolies3 has reported work on the simultaneous sintering and carburization of iron-powder parts. Glauch4 investigated the effect of various types of graphite on the properties of iron-carbon powder alloys but did not determine the effect of different particle sizes of the same graphite alloyed with different types of powder. In the investigation reported in this paper, powders typical of those produced by electrolytic deposition and the decar-burization of shotted steel scrap were used. The powders were mixed by tumbling in a jar mill with graphite powder ground to an average particle diameter of 2, 4, 6, and 16 microns (as determined by microscopic measurement). The properties of the iron and graphite powders are presented in tabular form as Table I. In order to obtain the maximum information from a minimum number of test specimens, the study was divided into two sections with one set of specimens treated identically in each section as a basis for comparison. In the first section, iron powder produced by the shotting and subsequent decarburization of scrap steel was mixed with 2-micron graphite powder, pressed at 50,000, 100,-000, and 200,000 psi, and sintered in hydrogen at 1200°C for the periods of time ranging from 15 to 120 minutes. In the second section of the investigation, electrolytic iron powder was mixed with graphite of an average particle diameter of 2, 4, 6, and 16 microns, pressed at 100,000 psi, and sintered at temperatures ranging from 1000° to r200°C'. for periods of time of 30 to 180 minutes. By following this procedure an indication of the effect of the following variables upon the density and tensile properties of iron-carbon powder compacts was obtained: (I) forming pressure, (2) sintering time, (3) particle size of graphite powder, (4) sintering temperature, (4) type of iron powder.

Jan 1, 1947

By Robert Steinitz

Soft iron parts for magnetic applications, particularly pole shoes, constitute a major portion of the ferrous products of powder metallurgy. The residual pores in pressed and sintered parts reduce values such as the magnetic permeability but service experience extended over a number of years has proven beyond doubt that in many instances the lower density of powder parts is not prohibitive to their use as replacement of machined magnetic parts. The magnetic requirements for pole shoes, particularly the permeability, vary within wide limits, especially with the relative size of the air gap in the finished assembly. The overill permeability of an assembly, is given by the formula where is the permeability of the core material, I the total length of the magnetic path, and a the length of the air gap. Fig I shows the variation of the overall permeability with the permeability of the core material, calculated according to Eq I for an air gap of I pct of the total length of the magnetic circuit. It is readily recognized that to use core materials hav- A

Jan 1, 1949

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 F. V. Lenel

Two years ago in Chicago a seminar was held on the theory of sintering of pure metal powders. As an introduction to this seminar D,.. Rhines1 gave an excellent survey of the literature on this subject, His method of presentatioll was to summarize the experimental observations on sintering and from them to develop a composite theory of sintering in which he combined all the important contributions to the theory into one organic whole. In contrast to the mechanism of sintering of pure metal powders, which, of course, al\vays takes place in the solid phase, sintering j,, the presence of a liquid phase, cannot be treated as one unified mechanism, such as the sintering mechanism of pure metals. The reason is that there are really several mechanisms depending upon the type of alloy system which is sintered and the field of its con. stitutional diagram ill which the sintering takes place, Two mechanisms have heen investigated and will be reviewed in this paper. Ill the first lnechanism the liquid is presellt during the entire time while the compacts are at the sintering temperature, In other words they are sintered between the liquidus and the solidus of the alloy system and are ~e~erogelleous during the entire sintering cycle. The second mechallism applies to alloys in which the liquid phase is formed during the sintering process, but disappears before the sintering process is completed through diffusion and formation of a solid solution. These alloys are therefore homogeneous at the end of the sintering cycle. This second mechanism is more complicated because of the two stages of sintering, the liquid and the solid, as they may be called. It is therefore not surprising that the few detailed investigations of sintering in the presence of a liquid phase have been concerned with heterogeneous sintered alloys, namely the tungsten-nickel-sinter ing which is the so-called "heavy alloy," and the cemented carbides. The mechanism of sintering of these systems is characterized by the fact that theoretical or near theoretical density is attained during sintering, while simultaneously a distinct grain growth takes place through solution of the smallest grains of the solid phase in the liquid phase and reprecipitation on the larger grains. In the first part of the survey this sintering mechanism which is called for short the heavy alloy mechanism is treated in detail. In the second part Of the survey experimental observations for the sintering of homogeneous sintered alloys where the liquid phase disappears before the completion of sintering are discussed. Much less systematic work has been done on these alloys to which the conlmercially important Porous bronzes and the iron-nickel-aluminum permanent magnet alloys belong. Emphasis will be laid throughout this survey upon the microstructural and density changes during sintcring because the Sintering mechanism can usually be described directly by these changes. Other

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.' 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.' 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 Pol Duwez, H. E. Martens

The high temperatures encountered in the operation of jet engines have imposed most drastic requirements upon the materials used in their construction. There are two different approaches to the materials problem connected with the design of parts in contact with high temperature gases. The first approach is to use a material which will perform satisfactorily at a temperature comparable to that of the gas. The second approach is to use a cooling system so that the material is maintained at a temperature appreciably lower than that of the gas. Besides the conventional method of cooling by means of a liquid in contact with the material exposed to a high rate of heat transfer, a less orthodox method consists of making the part to bc cooled of a porous material', so that the cooling fluid can be forced through the pores, In this scheme, the temperature of the coolant moving in a direction opposite to that of the heat flow increases gradually while passing through the porous material, and the coolant forms a protective layer on the surface exposed to heat, This method, referred to as ((sweat cooling," was pro- posed at the Jet Propulsion Laboratory in September 1944, and the experimental work on the preparation of porous metals was started early in 1945. The sweat cooling method opens new lines of research in powder metallurgy by extending the field of application of porous metals. The porous metals available at the present time are used mostly as bearings or filters, and a rather limited number of alloys are made for these applications. In addition, the fabrication of bearings or filters does not require a very close control of the permeability, while in the case of sweat cooling such a control is of primary importance. In designing a sweat cooled part it is imperative to assure a given rate of flow of coolant under certain conditions of Pressure drop. Generally, the Proper pressure drop and the rate of flow of coolant are deduced from heat transfer and design considerations, and consequelltl~ the Permeability of the Porous metal to be used is also determined. It is therefore necessary for the designer to have available a continuous series of porous metals covering a range of permeability as wide as possible. Contrary to the requirements established in the fabrication of filters, the actual pore size of a porous metal intended for sweat cooling is of little consequence, except for its effect on permeability. The tensile strength is likely to be of great importance for some applications. Since the tensile strength of a porous alloy decreases with increasing porosity, an important problem is to develop porous alloys having the maximum permeability with minimum porosity.

Jan 1, 1949