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By W. G. Lidman, H. J. Hamjian

' I HE fabrication of many materials from powders involves a sintering process. A mass of powder will sinter because of the excess free energy over the same mass in the densified state caused by the higher total surface area of the powder. An understanding of the kinetics and mechanism of sintering should assist in improving the properties of such materials. The present investigation conducted at the NACA Lewis laboratory deals with the sintering of chromium carbide. Dry sintering (sintering at a temperature below the melting point) was divided into two stages by Shaler:' the first stage, during which the particles preserve much of their original shape and the voids are interconnected, and the second stage, during which densification occurs and the pores are isolated. The mechanism of forming interfaces between particles, or welding together of particles, has been investigated by Kuczynski2 and may be described by any one or a combination of the following mechanisms: viscous flow, evaporation and condensation, volume diffusion, or surface diffusion. The mechanism by which pores are closed or eliminated (densification) during sintering, is of interest. Grain growth observed during sintering may be attributed to the variation in the surface energies of individual grains, causing some grains to grow at the expense of others. Grain boundary migration occurs presumably by a diffusion process, therefore the rate of grain growth would be expected to increase exponentially with increasing time and temperature. Thus, for practical sintering times of less than 1 hr, a certain minimum temperature may exist at which major structural and property changes will occur. Densification and kinetics of grain growth during sintering under pressure of chromium carbide were investigated to provide additional information which will aid in describing more accurately the sintering process and the mechanisms involved. This material was selected for this study because of the current interest in high strength, oxidation resistant refractory materials, such as carbides, which are sintered to produce solid, dense materials from powders. Sintering under pressure is a process where the heat and pressure are applied to the compact simultaneously, specimens for this work were prepared by sintering under pressure at different temperatures and for various time periods. Experimental Procedure Preparation of Specimens: Chemical analysis of the commercial chromium carbide used in this investigation was as follows: Cr 86.19 pct, C 12.14 pct, and Fe 0.2 pct. X-ray diffraction powder patterns gave characteristic diffraction lines of Cr3C2 crystal structure. Powder particle size was determined microscopically and the average initial particle size was 6 microns with 85 pct between 2 and 10 microns. Specimens sintered under pressure were formed in graphite dies3 heated by induction. Sintering temperatures were measured with an optical pyrometer by sighting into a 3/8-in. hole drilled 1 in. deep at the midsection of the graphite die. A load of approximately 1 ton per sq in. was applied to the powder. The die assembly was heated in 20 min to the highest temperature (2500°F') at which no increase in grain size could be observed, and less than 2.5 min were required to heat from this temperature to the maximum temperature (3000°F). Sintering temperatures and times for the specimens of this investigation are indicated in Table I. Analysis of Specimens: Specimens polished with diamond abrasives were etched to reveal the grain boundaries with a 1:1 mixture of 20 pct potassium hydroxide and 20 pct potassium ferricyanide heated to 160°F. Representative areas of each sample were photographed at 1000 diameters. The largest diameters of all well-defined grains were measured, but only the measurements of 15 of the largest grains were averaged in order to determine an index of grain size on the assumption that they were among the first to begin growth. Densities were determined from differential weighing of the samples in air and water. The reported density values are considered correct within ±0.01 g per milliliter. Results and Discussion Metal compacts have exhibited grain growth when sintered at temperatures about two-thirds of the absolute temperature of their melting point.' Grain growth also occurs during the sintering of chromium carbide and is illustrated by the micrographs shown in Fig. 1. These micrographs were prepared from specimens sintered for 90 min at temperatures ranging from 1371°C (2500°F) to 1648°C (3000°F). Average grain size and density measurements of specimens investigated are presented in Table I. The relationship between grain size and sintering tem-

Jan 1, 1954

By W. H. Bassett

W H. BASSETT was elected first vice-president at . the executive session of the new Board on Tues- day afternoon. Karl Eilers, H. Foster Bain, Thomas T. Read, and H. A. Maloney were respectively re-elected as treasurer, secretary, assistant secretary and assistant treasurer. The new Executive Committee will consist of W. H. Bassett, Chairman, and Richard Peters, Jr., H. C. Bellinger, E. De Golyer, Edgar Rickard. The Finance Committee will be J. V. W. Reynders, Chair- man, Henry Krumb and H. G. Moulton. George D. Barron was reappointed Chairman of the Admissions Committee, and F. Julius Fohs put in charge of the Papers and Publications Committee.

Jan 1, 1929

By E. R. Kaiser

COAL research during 1941 had a marked increase in activity on problems bearing directly on furthering the increased and improved use of coal in homes and industry. Coal producers and fuel engineers expressed a greater interest in its practical possibilities and the coal laboratories have shown an increased interest in applied research, of value at once or in the near future to industry and the public. A large volume of accomplishment in mining, coal analysis, and the fundamentals of coal constitution and coal chemistry also continued to fill the storehouse from which applied research and fuel engineering of the future can draw valuable data.

Jan 1, 1942

By M. J. Hordon, M. A. Wright

ReCENT work has indicated that the substantial decrease in the rate of fatigue crack propagation for aluminum observed below a critical vacuum level can be attributed to the depletion of oxygen or water vapor from the vicinity of the fatigue crack opening.' At reduced gas pressures, generally below 10-2 Torr with fatigue strain amplitudes in the range *1 to 2 x 10-3 and cyclic loading rates of 25 to 50 cps, estimated rates of oxide or hydroxide monolayer adsorption on newly formed crack surfaces can fall behind the actual rate of crack extension. Changes in the critical pressure required for the transition in fatigue behavior with changes in temperature, strain amplitude, and cyclic frequency can be interpreted from variations in the adsorption and crack growth rates.'" Although the adsorption model generally appears to explain the enhanced fatigue resistance of reactive metals in vacuum, the specific adsorbing gas species and nature of the adsorption mechanism are uncertain. In addition to the direct dissociation and adsorption of O2 on the metal surfaces,3 the dissociation of H20 and subsequent adsorption of H ions have been advanced for aluminum alloys.4 The present note describes some measurements of the fatigue behavior of 1100 aluminum in reduced partial pressures of specific gases including O2, H2O, and H2 in order to provide additional experimental data. Cantilever-type specimens of 1100-H14 aluminum were fatigued in cyclic reverse bending at constant strain amplitude using a multispecimen vacuum apparatus and procedure described previously.' After initial vacuum evacuation to 1 x 10-7 Torr, the appropriate gas species was bled into the system through a calibrated leak valve. The input rate was adjusted to maintain the desired pressure level under continuous evacuation, thus minimizing possible changes in gas composition during testing. High-purity input gases including 99.9 pct O2, 99.999 pct H 2, and water vapor from triply distilled H 2 O were used to provide residual pressures. Trace amounts of contaminant species were limited by passing the Oz and H 2 input gases through liquid-nitrogen-cooled copper coils prior to entry to the test chamber. Care was taken to repeatedly flush the gas lines and valves before testing to minimize the effect of adsorbed contaminants. Residual gas pressures in the range 10-6 to 5 x x3 Torr were monitored by an NRC ionization gage corrected for each gas species. In the higher-pressure range, 5 x 1CT3 to 5 x 10' Torr, an NRC alphatron gage was used. In operation, eight simultaneous fatigue tests were conducted at a constant strain amplitude of *1.2 x 10 at cyclic bending rates of 25 and 50 cps to give an average fatigue life of 6.5x 105 cycles-to-fracture at standard atmosphere and 3.3 x 106 cycles in 1 x 10"7 Torr vacuum. Representative results for the effect of residual O2, H2O, and H2 contents on the fatigue life are shown in Fig. 1 for tests performed at 50 cps. It is apparent that the presence of either O2 or H2O gas in the system at partial pressures greater than 10"3 Torr was noticeably detrimental to the fatigue life. In contrast, the enhanced fatigue resistance typical of high-vacuum environments was retained with pure H 2 through the pressure range up to 1 Torr. For partial pressures of H2 gas above 1 Torr, the fracture life noticeably decreased. The critical Hz

Jan 1, 1969

Organization Place Date 1917 Mine Inspectors Institute of U. S. A Indianapolis, Ind. July 9-11 American Society of Sanitary Engineers Grand Rapids, Mich. Aug. 1-3 National Association of Stationary Engineers... Evansville, Ind. Sept. 10-15 National Exposition of Safety and Sanitation.. New York City Sept. 10-15 American Iron, Steel & Electrical Engineers.... Philadelphia, Pa. Sept. 10-14 American Institute of Metals Boston, Mass. Sept. 24-29 American Foundrymen's Association Boston, Mass. Sept. 24-29 Chemical Industries, Third National Exhibition. New York City Sept. 24-29 American Electro-Chemical Society Pittsburgh, Pa. Oct. 3-6

Jan 7, 1917

By Andy B. Wallace

Veins in the Pyramid district of northwestern Nevada occur along steep fractures in Oligocene and Miocene quartz latite tuffs. The vein mineralization is zoned from a central enargite-pyrite zone outward through a complex polymetallic pyrite-tetrahedrite-sphalerite-galena-chalcopyrite-bornite-chalcocite zone, and finally to an outer zone of pyrite and galena. Wall rock alteration includes advanced argillic and sericitic envelopes along veins superimposed on district-wide propylitization. The ore distribution and alteration patterns were probably produced by an increase in pH, a decrease in sulfur fugacity, along with cooling of the migrating hydrothermal fluid.

Jan 1, 1981

By C. A. Heiland

IN the third year of war, geophysical oil exploration broke all records to keep pace with the demand for increased reserves. Geophysical prospecting for strategic and other minerals also grew in scope. The trend of geophysical oil exploration throughout the war is indicated in Fig. 1. This figure resembles the one presented in the last annual review issue of M&M (February 1944, p. 62), corrected for data on-operations in the last months of 1943 and extended into 1944. The average number of geophysical oil prospecting crews in the field in 1944 was 451, whereas the total in 1943 was 340. An upward trend in the use of all geophysical methods is clearly evident throughout the year. Seismic operations were 67 per cent, gravimeter surveys 28 per cent, and other methods 5 per cent of the total. Seismic reflection and refraction crews increased 181/2 per cent over the 1943 average, gravimeter operations increased 73 per cent, and other methods gained 92 per cent. The increase in seismic and gravimeter operations, particularly the latter, is probably due to an increased production of equipment and the organization of new service companies. Miscellaneous methods gained largely through a revival of magnetometer work, and an increase in the use of torsion balances and electrical equipment. In comparison with the prewar average of 1941, it is noteworthy that seismic operations increased 58 per cent, gravimeter operations 88 per cent, and miscellaneous other methods gained as much as 283 per cent. Unfortunately the expansion in the number of geophysical crews does not indicate a proportionate increase in efficiency or in areal coverage, as will be brought out later.

Jan 1, 1945

By R. W. Raymond

(Chattanooga Meeting, October, 1908.) THE immense commercial value of the Gayley dry-blast process has been established beyond controversy. The testimony of practical blast-furnace managers, on both sides of the Atlantic, agrees that it reduces the cost of pig-iron about $1 per ton; but from the same testimony it appears that this direct economy does not by any means cover its commercial advantages-in fact, that under conditions frequently encountered in practice, it presents other benefits of even greater immediate financial importance. To this point I shall recur in a later part of the present paper. The history of the reception given to this invention, especially on the other side of the Atlantic, has repeated an experience familiar to American engineers. First, the reports of our practice were rejected as theoretically impossible, according to generally accepted notions and formulas; then the figures were reluctantly accepted ; and finally the attempt has been made to explain how they could have been obtained. As to the Gayley dry blast, we Americans have been for several years in the last stage of the discussion, and the rest of the professional world is rapidly coming to it. Meanwhile, the remark has been repeatedly made that, whatever Mr. Gayley's process may turn out to be worth, it was not an invention on his part, but simply the energetic and persevering execution of a procedure already proposed by others. This question I wish to discuss first in the present paper. I. WHAT DID MR. GAYLEY INVENT Realizing that this is not the place for detailed argument on an issue of patent law, I shall not undertake to quote and criticise the publications prior to Mr. Gayley's first patents. It may be admitted, without such critical analysis, that the possi-

Jan 1, 1909

WALTER P. JENNEY, Rapid City, S. Dak.: This paper is the first publication, I believe, of the fact that traces, up to two or three ounces to the ton, of tellurium have been found in the gold ores of the Black Hills occurring in the Potsdam formation. There are two great classes of ore-deposits in the Black Hills. First, the gold-ores in the Archæan, of which the great Homestake lode, extending from Lead City to Central, in the northwest section of the Hills, may be taken as a type; second, the refractory gold-ores found in the Potsdam sandstone over a

Jan 1, 1897

By Mrs. V. J. DeCarlo, G. P. Salvo, H. W. Schadler, L. M. Osika

The lattice parameter of the inlerrnetallic compound Nb3Sn has been measured as a function of temperature from 80° to 1290°K. The results are compared with published data on the thermal ex- ThE recent interest in the intermetallic compound, Nb3Sn, as an engineering material for the production of superconducting devices has necessitated that certain engineering data be obtained. Because of the difficulty encountered in producing bulk pansion of niobium and indicate that the compound when made by diffusion of tin into niobium at 1000°C, would be subjected to a tensile strain of about 0.1 pct when cooled to room temperature. material which is single phase, the coefficient of thermal expansion has not been measured by dilata-tional methods. Therefore the lattice parameters of fine-grained samples of Nb3Sn produced on the surface of a niobium sheet by heating in molten tin at 950°C have been obtained as a function of temperature. The results are compared with published data on niobium2 and Nb3Sn3 and with lattice-parameter measurements made on small single crystals of Nb3Sn.

Jan 1, 1964

By Cyril Stanley Smith

Jan 1, 1949

By Cyril Stanley Smith

Jan 1, 1949

MARCEL R. DALY (communication to the Secretary?).-The fundamental disagreement between Eugene Coste and the writer proceeds essentially from the contradictory views they hold on the origin of petroleum. This difference cannot be bridged, nor can inorganic and organic theories be discussed here. The writer has suggested that the proper thing in such a case would be to agree to disagree. Coming to the detailed objections further presented by Mr. Coste, the writer feels that, in the main, they take their source in a wrong interpretation of the theory, and the writer is sometimes too generously invested with views that are not his own. 1. The only requirement for the theory is that the oil proceeding from organic remains be distributed in a water-laden sediment, and that this sediment be submitted to the increasing compression due to the continuous accumulation of superimposed strata, which would tend to squeeze out the liquid contents (p. 1152). This squeezing out would be further aided by the distortion of the strata (p. 1148, a). Nothing here makes impossible the slow formation of the oil, if this is considered necessary, as the piling up of the strata in the syncline would require by itself a protracted length of time, and, further, the squeezing-out process is a slow one. Possibly the formation of the oil may even continue during part of the process of distortion. But the mode of formation of the oil and the time and temperature required for it are left to the chemist to decide. The diastrophic theory, which is essentially a theory of motion and accumulation dependent on the laws of mechanics, is not directly concerned with them, provided the general points heretofore outlined be agreed upon. Perhaps it would be wise not to claim too many "eons" for the formation of the hydrocarbons, if the statement made by Sir Boverton Redwood is correct that "the coral reefs of the Red Sea are charged in places with recent petroleum, formed in that torrid climate from the swarming organisms occupying the shallow pools."1

Jan 5, 1917

For $100 a month plus expenses, Thomas A. Edison in 1879 hired a colorful adventurer named Frank McLaughlin to go west as a prospector. A few months later, McLaughlin triumphantly returned to the inventor's laboratory in Menlo Park, N. J. "On his shirt bosom and fingers sparkled glittering stones," recalled one of Edison's associates. These were only the tangible parts of his new trappings. In addition, McLaughlin "now wore the title of major which he acquired somewhere west of Omaha."

Jan 10, 1961

Executive DEGOLYER, Chairman SIDNEY H BALL RICHARD PETERS, JR WILLIAM H BASSETT J V W REYNDERS Finance GEORGE D BARRON, Chairman H A GUESS GEORGE OTIS SMITH Membership J M CALLOW, Chiarman FRANK L ESTEP WILBER JUDSON GEORGE D BARRON H N SPICER Alternates P A MOSMAN EDWARD B STURGIS

Jan 1, 1923

By T. MacDONALD

ATHOUGH flotation has been a commercial process for over twenty years, the last two years have witnessed a sudden and phenomenal increase in our knowledge of how to separate minerals heretofore not considered amenable to flotation at all. As remarked by Professor Locke in the January issue. "Either commercial or laboratory flotation is reported on zircon, ilmenite, carnotite, kyanite, scheelite, chromite, fluorite, feldspar, cassiterite, wolframite, barite, and clay. Attractive patents on soap flotation are U. S. Nos. 2,000,656 and 2,040.187. A survey by Ralston in the February E. & M. J. adds many other minerals to this impressive list. The simple but pregnant fact is that any mineral can be coated, directly or indirectly, with a water-repellent coating, and since this is true, it follows that any mineral can be floated. Fundamentally, this is no new discovery, where, for instance, is the mineral that cannot he washed from a pair of dirty hands by means of soap and water, given the absence of refractory greases or oils which would have no proper place in flotation ?

Jan 1, 1937

By T. A. Rickard

The question of the original extent of the anthracite-beds of Pennsylvania has often been raised; and even discussed with reference to the probability of their present existence under the New Red, a matter of immense practical importance. So high an authority as my revered master, J. P. Lesley, Honorary

Jan 1, 1903

By O. K. Riegger, L. H. Van Vlack

The median angle of relatively few two-dimensional observations provides a satisfactory value for dihedral angle determinations. Those data that contain bimodal or non-equilibriated dihedral angle distributions are readily detected. THIS paper is concerned with a statistical simplification for determining dihedral angles in solids. Microstructures are partially controlled by relative energies of interphase boundaries and grain boundaries. smith1 has shown rather conclusively that such boundaries may be equilibrated to give a vectorial balance at grain and phase edges. Thus if an accurate measurement is made of the dihedral angle associated with grain and phase edges, an accurate calculation of the relative energies may also be made. The accurate measurement is difficult because the dihedral angle involves two planes in three dimensions, and only a two-dimensional cut through the dihedral angle is usually observed. Such a two-dimensional cut is statistically random provided there is no preselection or orientation. Harker and parker2 have shown that the mode of the frequency distribution of observed angles is within 5 deg of the true angle if the true dihedral angle is 120 deg. smith1 had calculations made to show that the same generalization could apply to dihedral angles of 30, 60, 90, and 150 deg. This procedure of requiring the determination of the statistical mode is time consuming because experience has shown that more than 200 angle observations are necessary before the mode is clearly indicated. It is possible to determine the dihedral angle with equal accuracy with only 25 angle observations if the median angle is used in place of the mode angle. Use is made of Harker and parker's2 basic equation tan =2 sin x cos

Jan 1, 1961

By John L. Ham, Robert M. Parke

The melting point of molybdenum is 2625° + 50°C. Heretofore the metal has been considered too refractory to be melted in commercial quantities; hence, it has been formed into rod, wire, and sheet by the methods of powder metallurgy, wherein the temperatures do not exceed 90 per cent of the melting temperature. The manipulation of liquid metals at temperatures of about 2000°C. and above presents some difficult problems in heat transfer, in purification, and in container materials. For metals melting at such high temperatures, it is generally regarded as expedient to circumvent the more common melting and casting process by resorting to powder metallurgy. This circumvention is not accomplished without some penalties, the more notable of which are the relatively high cost of the powder metallurgy method and particularly the size limitations of its product. In an effort to overcome the inherent disadvantages of the powder metallurgy method, especially in respect to the limit of size, a project was begun in 1943 at the Climax Molybdenum Co. laboratory to develop a method of melting and casting molybdenum capable of producing larger bodies of molybdenum than were then obtainable. Later, from Feb. I, 1944, to Aug. 31, 1945, the project was under the supervision of the National Research Committee, Division One. In peacetime, too, there are needs for molybdenurn, which make consideration of another process desirable; for example, large parts for heat engines generally, the omnipresent demand for metal of higher quality and lower cost, and the development of molybdenum-base alloys. This paper describes methods for melting and casting molybdenum, with details of the special process needed to make molybdenum castings ductile, and reports some of the properties of what may be regarded as a new, or at least modified, form of the metal. First Process for Melting and Casting Molybdenum The maintenance of a temperature greater than 2625°C. in a 'pace large enough to melt several pounds of molybdenum may involve the loss of heat at a Very considerable rate. For melting molybdenum, therefore, the source of heat must be of high potential and of fairly high power. Evidently, also, the source of heat must not impair the purity of the product. The electric arc operating in vacuum appeared to meet these requirements and was accordingly the first choice as a source of energy. A number of arc devices for melting molybdenum were examined, and several were tried. In the first experiment, a 20-kw., 60-cycle-per-second alternating-current arc was operated between two horizontal and opposed electrodes of molybdenum- In this arrangement the falling droplets of molybdenum solidified below the arc in an irregular mass. This experiment did not produce a useful casting, but the data obtained indicated that

Jan 1, 1947

By John L. Ham, Robert M. Parke

The melting point of molybdenum is 2625° + 50°C. Heretofore the metal has been considered too refractory to be melted in commercial quantities; hence, it has been formed into rod, wire, and sheet by the methods of powder metallurgy, wherein the temperatures do not exceed 90 per cent of the melting temperature. The manipulation of liquid metals at temperatures of about 2000°C. and above presents some difficult problems in heat transfer, in purification, and in container materials. For metals melting at such high temperatures, it is generally regarded as expedient to circumvent the more common melting and casting process by resorting to powder metallurgy. This circumvention is not accomplished without some penalties, the more notable of which are the relatively high cost of the powder metallurgy method and particularly the size limitations of its product. In an effort to overcome the inherent disadvantages of the powder metallurgy method, especially in respect to the limit of size, a project was begun in 1943 at the Climax Molybdenum Co. laboratory to develop a method of melting and casting molybdenum capable of producing larger bodies of molybdenum than were then obtainable. Later, from Feb. I, 1944, to Aug. 31, 1945, the project was under the supervision of the National Research Committee, Division One. In peacetime, too, there are needs for molybdenurn, which make consideration of another process desirable; for example, large parts for heat engines generally, the omnipresent demand for metal of higher quality and lower cost, and the development of molybdenum-base alloys. This paper describes methods for melting and casting molybdenum, with details of the special process needed to make molybdenum castings ductile, and reports some of the properties of what may be regarded as a new, or at least modified, form of the metal. First Process for Melting and Casting Molybdenum The maintenance of a temperature greater than 2625°C. in a 'pace large enough to melt several pounds of molybdenum may involve the loss of heat at a Very considerable rate. For melting molybdenum, therefore, the source of heat must be of high potential and of fairly high power. Evidently, also, the source of heat must not impair the purity of the product. The electric arc operating in vacuum appeared to meet these requirements and was accordingly the first choice as a source of energy. A number of arc devices for melting molybdenum were examined, and several were tried. In the first experiment, a 20-kw., 60-cycle-per-second alternating-current arc was operated between two horizontal and opposed electrodes of molybdenum- In this arrangement the falling droplets of molybdenum solidified below the arc in an irregular mass. This experiment did not produce a useful casting, but the data obtained indicated that

Jan 1, 1947