Search Documents

PRESIDENT SIDNEY J. JENNINGS NEW YORK, N. Y. PAST PRESIDENTS L. D. RICKETTS NEW YORK, N. Y. PHILIP N. MOORE FIRST VICE-PRESIDENT C. W. GOODALE BUTTE, MONT. TREASURER GEORGE C. STONE, NEW YORK, N. Y. SECRETARY. EMERITUS ROSSITER W. RAYMOND, NEW YORK, N. Y. SECRETARY BRADLEY STOUGHTON, NEW YORK, N. Y.

Jan 5, 1918

By W. C. Leslie, R. M. Fisher, K. G. Carroll

A nitride, believed to be Si3N, has been separated from three nitrided silicon steels. Germanium nitride, Ge3N4, has been prepared from pure germanium. Comparison of the diffraction patterns indicates that the two nitrides are isomorphous; on orthorhombic structure is suggested in place of the rhombohedral structure previously reported for Ge3N4. THE possibility that a nitride of silicon may, under appropriate conditions, precipitate in silicon steels or in steels killed with silicon makes it desirable to have some positive means of identifying such a compound. One such means is the X-ray or electron diffraction pattern of the nitride. A review of the meager data in the literature indicates that the nitride most likely to form is Si3N4, a conclusion supported by the results of a study of nitrided silicon steels to be published shortly by L. S. Darken and R. P. Smith, of this Laboratory. Unfortunately, there is available no diffraction pattern for this nitride. Data have been reported, however, for Ge3N4 which, judging from the similarity between germanium and silicon, might be expected to be isomorphous with Si3N4. An effort was made, therefore, to form such a silicon nitride, to determine its composition and diffraction pattern and, if possible, its structure. To this end a series of three silicon steels was nitrided under controlled conditions with the resultant formation of nitride particles which yielded an electron diffraction pattern in situ. The particles were then extracted from the steel and an attempt was made to determine their chemical composition. X-ray and electron diffraction patterns were also obtained from the extracted particles, which indicate that the nitride is isomorphous with Ge3N4, although a complete determination of the structure has not been possible. These results show that a silicon nitride with a well-defined diffraction pattern can form in silicon steels, and they suggest that this nitride is Si3N4. Materials and Procedures The sillicon steels investigated were In the form of thin sheet or strip and had the composition shown in Table I. The 0.58 and 1.21 pct Si steels were nitrided by holding them at 1110°F in an H2-NH3 atmosphere containing 3 pct ammonia for 48 hr. The nitride particle size was increased by subsequent heating at 1500°F for 13 1/2 hr in helium. The resulting microstructure is shown in Fig. 1. The steel containing 3.20 pct Si was nitrided at 1200°F for 16 1/2 hr after which it was held in helium at 1500°F for 4 hr. Its structure as seen under the electron microscope is illustrated by Fig. 2. As would be expected from the higher silicon content and the shorter holding time at 1500 °F, the nitride particles are smaller and more numerous than those in the 1.21 pct Si steel. The ammonia-hydrogen treatment reduced the carbon content of the steels to a very low level, so no interference was encountered from carbon or carbides. In the case of the 3.2 pct Si steel, the carbon was reduced to 0.003 pct before nitriding by heating in dry hydrogen. Attempts to obtain an X-ray diffraction pattern from polished and etched surfaces of the 1.21 and the 3.20 pct Si steels were unsuccessful. However, an electron diffraction pattern was obtained from the surface of the steels. The interplanar spacings obtained from these patterns arc shown in Table 11, col. 5. The nitride particles were then extracted from all three steels by dissolving the ferrite matrix in bromine-methyl acetate, the solution used in the Beeghly method for the extraction of aluminum nitride from steel. X-ray diffraction patterns of these residues, obtained by means of a spectrometer and by a 57 mm Debye-Scherrer powder camera using filtered cobalt or chromium radiation, are given in Table II along with the pattern obtained by

Jan 1, 1953

Gach-Saran.—The most important development of 1937 has been the successful completion of initial exploratory wells in the Gach Saran (formerly known as Gach-i-Qaraghuli) field, about 125 miles southeast of Haft Kel. Two of these wells are rated at 33,000 bbl. per day at flowing pressures exceeding 800 lb. Drilling is proceeding with the object of delimiting the structure. Exploratory drilling is also being undertaken in several areas within the company's concession. In the producing fields the policy of controlled production has been maintained as in the past, and drilling has been limited to that required for maintenance of production and general control of the fields. Acid treatment to increase production when desired has continued to be successful in most cases. Table 1.—Crude Production in Iran Masjid-i-Sulaimana Haft Kel Total Year barrelsb Ton Barrelsb To Barrelab 1936 3,641,247 27,820,000 4,473,849 34,200,000 8,115,096 62,020,000 193P 4,375,112 33,110,000 5,693,849 43,480,000 10,068,961 76,590,000 * Net production; i.e., excluding surplus products re-injected to reservoir. 6 To nearest 10,000. " Correct to November, with an added estimated figure for December. Masjid-i-Su1aiman.—There have been no new developments in this field. The policy of returning, as and when necessary, surplus products to the reservoir has been maintained. Haft Ke1.—Drilling to explore deeper formations has been undertaken, but has not progressed far enough for conclusive results to be drawn. Gasoline retention in the crude by means of multistage pressure stabilization has been continued as in past years. Separation pressures are as follows: well-head separators, 500 lb.; central battery, 190, 85, 40, 20 and 10 lb. per sq. in., respectively. The stabilized crude is delivered to pipe line at atmospheric pressure, or ex the 10-lb. stage, in accordance with refinery requirements.

Jan 1, 1938

By H. J. Maguire

Those familiar with mill-practice understand the work required of an average bucket-elevator, but I wish to call special attention to the wear on the buckets. I have been studying in what manner the life and service of the bucket might be improved, and I feel that an adjustable lip, attachable to each bucket without the aid of rivets, will be of material advantage. For illustration, consider the feed-elevator of a typical mill in the Cæur d'Alene district. The ore is carried by water in a launder from the feed-rolls and dumped in the " boot" of the elevator, directly in front of the ascending bucket. Middlings from the return-rolls are similarly handled. Under this condition the bucket not only carries the ore, but also picks it up, and this latter requirement determines the life and service of the bucket. It might be said that it would be better practice to convey the feed to the elevator and dump it directly into the bucket, but at one mill at which this plan mas tried the results were disappointing and the rubber belt was badly worn. The wear of the bucket is confined to the lip and the corners which have to pick up the material. When the lip on a corner of a '7- by 12-in. malleable cast-iron bucket is worn down about 3 in., the bucket is of no further value as a carrier and has to be replaced. The worn bucket, containing about three-quarters by weight of the metal of the original bucket, has a scrap value of about 10 per cent. of that of a new bucket. To the cost of the bucket, however, should be added the time-

Jan 1, 1913

For the benefit of those of our members who are considerable holders of securities, but owing to their isolated situations are not in close touch with the metropolitan market and current quotations, we are publishing two very interesting graphs, showing the course of the bond and stock markets in New York over a long period. These graphs are furnished through the courtesy of the financial department of the New York Tribune.

Jan 12, 1919

By J. Parke Channing

THE growth of and profession depends on meeting and solving new problems. It is a continuous process. 'A period free from new, or hitherto unknown, questions will be a period of arrested development in the profession it affects. The present generation has witnessed a' mechanical development that has been truly marvelous: Almost every day marks the advent of a new, or the improvement of an old; process, method or machine. Wonders are now commonplace. The impossible is regularly accomplished. Yet, with all our progress in every realm of science and with our development in the engineering field, advances which have made possible the marvelous growth in industry, we have not made commensurate gains in methods affecting the human factor. Without the cooperation of the worker, we shall always fall short of our goal in a mechanical or statistical sense. If we do not make the individual members of the human family strong, healthy, happy, and ambitious for better things for themselves and their children, we will have failed utterly, for that is the real reason for our existence as men and the purpose of our organized effort as an engineering group. Thomas A. Edison

Jan 1, 1921

For the benefit of those of our members who are considerable holders of securities, but owing to their isolated situations are not in close touch with the metropolitan market and current quotations, we are publishing two very interesting graphs, showing the course of the bond and stock markets in New York over a long period. These graphs are furnished through the courtesy of the financial department of the New York Tribune.

Jan 7, 1919

For the benefit of those of our members who are considerable holders of securities, but owing to their isolated situations are not in close touch with the metropolitan market and current quotations, we are publishing two very interesting graphs, showing the course of the bond and stock markets in New York over a long period. These graphs are furnished through the courtesy of the financial department of the New York Tribune.

Jan 6, 1919

By C. C. Wright, R. J. Day

ALTHOUGH data on the exact tonnage of recoverable coal silt are not known, the quantity produced in 1943 was estimated to be over five million tons for the anthracite region of Pennsylvania alone. Since that time the recovery of the No. 5 buck- wheat size previously included in silt estimates has increased greatly thus reducing the total silt tonnage. As a compensating factor, however, the methods of recovering silt previously escaping into the rivers and streams have been markedly improved so that the net figure may not have changed materially. Comparable estimates for bituminous coal are lacking, but undoubtedly the silt represents a significant tonnage. With the trend toward increased wet cleaning of the smaller sizes of bituminous coal, it is to be expected that even greater quantities of silt will be available in the future. The raw silt from anthracite collieries usually contains a high mineral matter content, but technological developments in fine coal cleaning have been making rapid advances and it appears probable that more extensive use of these methods will be employed in the near future. Bituminous coal silt in many instances contains a similar high mineral matter content. As with anthracite silt, however, the cleaning of this material, where necessary, appears both technologically and economically feasible. With a view to upgrading the size and value of silt, considerable laboratory and pilot plant work has been conducted by a number of organizations on what is commonly known as pelletization. Actually the process is one of extrusion in which the moist silt is extruded from a die in the form of rods, which usually break into relatively short lengths-a few inches long-as they fall from the die. Fig I is a photograph of some extruded 3/8-in. diam pellets and of the anthracite silt from which they were produced. This technique of producing larger sized material from fines is by no means new, having been used extensively by the industrial carbon and clay industries for years.' The application of the process to coal silt appears, however, to be relatively new. The first major program of investigation dates back only to July 1945, when a group of engineers representing the Anthracite Institute, The Pennsylvania State College and the J. F. Pritchard and Co. conducted preliminary tests on the extrusion of anthracite silt at the Floridin Co. plant at Warren, Pa. Since that time these three organizations-individually, together, and in co- operation with other interested groups- have actively pursued work on various phases of the problem. Much of the early history and details of the laboratory and pilot plant work by the Anthracite Institute, has been reported by Mulcey and Eckerd.2 It is the purpose of this paper to report additional information on the process, especially with respect to the factors influencing the quality and use properties of the product, and the current develop

Jan 1, 1948

By Harry Udin

IN 1948, the writer and his associates determined the surface tension of solid copper by balancing the force of surface tension in a very fine wire against an external load.' At that time we, in common with other early workers, assumed that grain boundary energy in a pure metal is very small in comparison to the energy of an external surface. Accordingly, we neglected the internal surface energy of the coarse-grained specimens. Since that time, experimental evidence has accumulated showing that grain boundary energy, far from being small, is generally about one-third of the energy of an external surface.2-4 This is sufficient to introduce a significant error into our determination. The differential equation governing equilibrium is: wdl - yds, + y*ds2 [I] rather than wdl = yds as originally written. w is the balancing force in dynes, 1 the length of the specimen, sl the external and s2, the internal surface area, y the copper/ copper vapor surface tension, and y* the grain boundary tension. Fortunately, we had made for another purpose a careful study of the size and shape of the grains, and found that the boundaries, with rare exceptions, traversed the specimens and were perpendicular to the wire axis. For this case, eq 1 leads to w = rry -(n) r2y* [2] where r is the wire radius and (n is the number of grains per unit length. A count of some twenty 5-mil wires indicated that - n became 80 & 10 after a short anneal near the melting point, and remained nearly constant for as long as 96 hr at temperature. An assumption of y* = 1/3y leads to a defining eauation for r: [31 The term in the brackets may be considered a correction factor applied to eq 11 of ref. 1. Upon applying this factor, the surface tension of solid copper at its melting point is found to be 1650 & 100 dynes per cm, rather than 1370 as previously reported.' The new temperature coefficient is —0.55 dynes per cm per "C. Grain boundary energy is more significant than surface energy to the physical metallurgist. It is evident from eq 2 that a series of experiments with wires of different grain size can lead to an evaluation of y*. The details of such an experiment are being worked out now. References 1 H. Udin, A. J. Shaler, and J. Wulff: The Surface Tension of Solid Copper. Trans. AIME, 185, 186-190; Journal of Metals (Feb. 1949) TP 25303. 2 G. L. C. Bailey and H. C. Watkins: Surface Energies in the System Solid Copper-Molten Lead. Proceedings Physical Society. (London) (1950) 36B, 350. 3 L. H. VanVlack: Inter granular Energy of Iron and Some Iron Alloys. Ph.D. Dissertation, Univ. of Chicago, Sept. 1950. 4 . P. Greenough: Grain Boundary Energies in Silver. R.A.E. Report, No. Met. 52. (May 1950) Fan-borough, Hants, England.

Jan 1, 1952

By P. W. Andrews, R. B. Toombs

ECONOMIC STRUCTURE OF MODERN INDUSTRIAL ECONOMIES The role of minerals in modern industrial economies may be examined in several ways. There are relationships with the various sectors of the economy: the primary, secondary, and tertiary industrial groupings and activities. Mineral supply and demand activities can be measured in terms of national accounts criteria. The economic policy objectives of the modem industrial economy are based to a considerable extent on the needs of the nation for economic supplies of miner- al materials. There is an important role for minerals relative to national security in peace and in wartime and many national policies are directed toward ensuring adequate sup- plies of minerals. Environmental control in the modem industrial economy is increasingly concerned with matters related directly to the production and use of minerals and these matters, in turn, bear importantly on conservation in mineral supply and demand. Mineral polices include specific provision for research and development activities concerned with the production and the use of minerals. In all, national policy objectives will be shaped in considerable part by the circum- stances of mineral supply and demand: the relative degree of availability from domestic and foreign sources, the state of the mineral-processing industries, and the degree of development of the mineral-using industries, and per capita and total changes in requirements. Goods made from mineral raw materials are the basis of all advanced societies and although this is taken for granted, every country is continually dealing with problems of mineral supply and demand. Considering that in the first 50 years of this century the consumption of mineral materials in a highly Industrialized country such as the United States increased by six times while the population was doubling, it becomes apparent that if a country is to enjoy rapid economic growth it must have access to huge and ever-growing supplies of mineral materials at lowest possible cost. Adequate supplies of mineral materials and wise usage of mineral resources have always been among the most important determents of a nation's survival The importance of access to adequate mineral supplies is increasing every year and this has significant international, as well as national, implications because of the unique locational characteristics of mineral resources. It is generally acknowledged that no particular type of natural resource is essential to a high level of national income or to economic progress. A country's endowment of natural resources need not exercise a determining influence on the course of its national income over time, provided it is able to trade. What is required for economic progress is the availability of a substantial quanti-

Jan 1, 1976

By N. A. Gokcen, S. Fujishiro

THE pressures of Mn(g) in equilibrium with Mn7C3 and graphite have been measured by McCabe and Hudson' and Butler, McCabe, and paxton2 by means of graphite, zirconia, and Ta-Mo Knudsen cells. The details of corrections in their measurements were somewhat different from those of the authors;3'4 hence, further independent results at higher temperatures seemed to be warranted. The stoichiom-etry of Mn7C3 in equilibrium with graphite and its stability up to the vicinity of 1373 °K have been satisfactorily established by Kuo and persson5 (See also Hansen and Anderko).' The method of investigation has been described elsewhere in detail.3'4 The carbide was prepared in the manner described by McCabe and Hudson. In order to avoid possible reactions with refractory oxides, only graphite cells were used for the effusion experiments. The authors' results are the runs M-1, M-2 and M-3 listed in Table I, together with those of McCabe and co-workers. The heat capacity, c;, of Mn7C3 is not known; therefore McCable et al. plotted their data as log P vs 1/T and the results were only expressed first' as, and later2 as logP=- -14220+6.06 without further thermodynamic calculations. However, it is possible to estimate closely the necessary heat capacity as follows: When H; - &98 of CrC, or MnO, is plotted vs x, corresponding to various compounds, with temperature as the parameter, it is seen that the relationship is represented by a line of very small curvature. This relationship is also followed by other compounds which do not exhibit solid state phase transformations. In view of the fact that chromium and manganese have the atomic numbers of 24 and 25 respectively, it is reasonable to assume that H; - H;ae vs x for MnC, follows the same type of lines as those for CrC, for which adequate data are available.7 Similar correlations appear to be valid for oxides of two neighboring metals for which reliable data are available. The procedure is thus to move the lines for CrC, vertically (parallel to the axis of HT - H298) until they coincide with the points for MnC1/3, the only carbide of manganese whose H; - HO298 has been

Jan 1, 1963

By C. S. Land

Relative permeability functions are developed for both two- and three-phase systems with the saturation changes in the imbibition direction. An empirical relation between residual nonwetting-phase saturation after water imbibition and initial nonwetting-phase saturations is found from published data. From this empirical relation, expressions are obtained for trapped and mobile nonwetting-phase saturations which are used in connection with established theory relating relative permeability to pore-size distribution. The resulting equations yield relative permeability as a function of saturation having characteristics believed to be representative of real systems. The relative permeability of water - wet rocks for both two- and three - phase systems, with the saturation change in the imbibition direction, may be obtained by this method after properly selecting two rock properties: the residual nonwetting-phase saturation after the complete imbibition cycle, and the capillary pressure curve. INTRODUCTION Relative permeability is a function of saturation history as well as of saturation. This fact was first pointed out for two-phase flow by Geffen et al. 1 and by Osaba et a1.2 Hysteresis in the relative permeability-saturation relation also has been reported for three-phase systems.3 Since saturations may change simultaneously in two directions in a three-phase system, four possible relationships arise between relative permeability and saturation for a water-wet system. The four saturation histories of this system were given by snel14 as 11, ID, DI and DD. I and D refer to the direction of saturation change (imbibition and drainage), with the first letter of the symbol indicating the direction of change of the water phase. As used in this paper, the second letter of the symbol refers to the direction of saturation change of the gas phase, i.e., D and I indicate an increase and decrease, respectively, in gas saturation. Only a few three-phase relative permeability curves have been published. Leverett and Lewis5 published three-phase curves for unconsolidated sand, and Snell4 reported results of several English authors for both drairrage and imbibition three-phase relative permeability of unconsolidated sands. Three-phase relative permeability curves for a consolidated sand were published by Caudle et a1.3 for increasing water and gas saturations (ID). Corey et a1.6 reported drainage (DD) three-phase relative permeability for consolidated sands. Recently, Donaldson and Dean7 and Sarem8 calculated three-phase relative permeability curves from displacement data on consolidated sands, also for saturation changes in the drainage direction. The only published three-phase relative permeability curves for consolidated sands with saturation changes in the imbibition direction (11) are those of Naar and Wygal.9 These curves are based on a theoretical study of the model of Wyllie and Gardner 10 as modified by Naar and Henderson.11 Interest in three-phase relative permeability has increased recently due to the introduction of new recovery methods and refinements in calculation procedures brought about by the use of large-scale digital computers. The scarcity of empirical relations for three-phase flow, and the experimental difficulty encountered in obtaining such data, have made the theoretical approach to this problem attractive. RELATIVE PERMEABILITY AS A FUNCTION OF PORE-SIZE DISTRIBUTION Purcell used pore sizes obtained from mercury-injection capillary pressure data to calculate the permeability of porous solids.12 Burdine extended the theory by developing a relative permeability-pore size distribution relation containing the correct tortuosity term.13 The works of Purcell and Burdine were combined by Corey14 into a form that has

Jan 1, 1969

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 com¬mercial 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.1 When reduction of tungsten oxides by H2 was introduced commercially, 2.1 several investigators became concerned with the equilibria between tungsten metal and its several oxides in an atmosphere of hydrogen and water vapor.4-13 While these many investigations were in fair agreement on the equilibria there arose considerable controversy as to the chemical composition of the oxide between W03 and W02, 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 10o years. Thus Malguti,14 in 1835, decided it was W02.56. In 1857, Riche" proposed the formula W308. Usler,16 in 1865, confirmed the existence of W308 and further proposed W4O11. In 1897, Desi17 agreed upon W308 but also found W5014.

Jan 1, 1946

By J. B. Warriner

S. A. TAYLOR, Pittsburgh, Pa.-What was the distance of haul? J. B. WARRINER.-There is practically no limit to the haul. The length is determined entirely by the feasible location for a dump. -I have known of hauls up to 2 miles in length. R. V. NORRIS, Wilkes-Barre, Pa.-This paper was originally presented to the Anthracite Section as the result of the appointment of Mr. Warriner as the Chairman of the committee to study this matter and present this paper. As he has stated, he obtained data very freely from all the stripping operations in the region, and it is a type of paper of which we should have more in the Transactions. Two or three things in it strike me as particularly valuable. The two tables, 1 and 2, showing the coal remaining, have been the result of a great amount of study, as it is not an easy matter to obtain data as to the amount of coal left in mining. As an example, one of the, anthracite mines was mined and robbed out in 1850, so the maps show. That mine is today producing 250,000 tons of coal, over 50 per cent. from the bed which on the maps is marked as exhausted. What actually happened is that the seam was on a light pitch inconvenient to mine. There was ample thickness of coal and the chambers were driven at a convenient pitch through this 30,-ft. bed, leaving top and bottom, taking out about 10 ft. The pillars were removed and the working caved and marked as gone. That is the type of area that is now being stripped, which explains the reason for the enormous amount of coal left in, and the fact that Mr. Warriner has worked out the actual results from a large number of strippings is of great interest to the operators in any region handling thick coal which has been mined over in the past, generation. The modern mining, of course, is different. We do not have all the coal we want in big veins, and we do not mine it that way. Another interesting feature of the paper to me was the study of losses. It is not uncommon to assume that after you have stripped off the overburden all the coal goes to market. Mr. Warriner has shown that there is a loss ranging up to 10 or 15 per cent. that does not go, so 'that estimates made on stripping, figuring on all the coal, are subject to this very material correction.

Jan 4, 1917

By E. W. Dewing

ROLIN1 in 1961 published a phase diagram for the CaF2-Na3AIF6 system in which substantial (-20 wt pct) solid solubility of CaF2 in Na3A1F6 at the eutectic temperature (945°C) was indicated. The evidence was that the halt in cooling curves associated with the eutectic was lowered progressively on the Na3AlF6 side. H olm2 has recently confirmed the experimental fact, but attributes it to evaporation losses shifting the composition into the ternary NaF-CaF2-Na3A1F6 system with a consequent lowering of the eutectic temperature

Jan 1, 1970

By C. G. Durdaller, W. H. Robinson, G. M. Pound

The nucleation rate of the a (pay) to 0 (white) tin transformation was measured as a function of temperature and a tin particle size using an X-ray diffraction technique. The powder specimens of a tin were essentially monodisperse and the small dinzension of the particles of these specimens was varied from 13 to 75 p. Several types of nucleation sites of differing potency were fbund to be operative in the nucleation process, but it could not be determined whether these sites were on the free surface of the tin particles or within the volume. Assuming that they were on the free surface, the average density of the most potent sites was calculated to be 2.5 to 5.3 x 10' sites per sq cnz through the application of a Poisson distribztion finction to the isothermal data. Analysis of the temperature dependence' of the rate constmts at a given fraction transformed suggests that the active sites are regions of higher free energy and not catalytic interfaces. Appreciable induction periods were observed at the lower temperatures of transformation. Experimental studies1 of solid-solid phase transformations have led to the belief that the new phase nucleates at structural imperfections. The purpose of the present work was to learn more about the mechanism of nucleation in solids and the nature of the singularities at which nucleation occurs. In this investigation nucleation rates in the isothermal transformation of gray to white tin were measured by an X-ray diffraction technique using essentially monodisperse powders of gray tin. This particular phase transformation was chosen for study because it presented fewer experimental difficulties than most others. The experimental temperature-control problems were minimal because the two phases coexist in equilibrium at 13.3"C, and measurable transformation rates occur at temperatures only slightly above room temperature. The growth rate of the P phase into the a2 is sufficiently fast to make the measured transformation rate equivalent to the nucleation rate, provided that the particle size of the samples is small enough; for the experimental temperatures used in this study, the particle diameter must be less than 100 p. EXPERIMENTAL TECHNIQUE The P tin used in this study was obtained from Capper Pass and Son Ltd., North Ferriby, Yorkshire, England, and was of 99.999 pct purity. It was transformedS to the a phase and ground into a fine powder in an agate mortar. This powder was separated by a Roller air classifier into seven fractions whose dimensions, as determined by microscopic measurement of many thousands of particles, are given in Table I and whose distribution of size within each fraction is given in Figs. 1 and 2. The shape of the particles was roughly that of an oblate spheroid,

Jan 1, 1964

By H. M. Otte, A. L. Esquivel

A new leasl-squares method is Presented for determining lattice parameters of hexagonal or tetragonul structures. The method is adapted for use on electronic computers and involves a reiterative procedure. The correction factor employed raries linearly with the lattice parameter, a (determined from the Brag, angle). In contrast, Cohen's method and recent modifications of it use a correction factor that varies incersely as the squure of the lattice paramneter, a. While the recent modifications attempt to improve the precision of the extrapolated lattice parameter, a, (or-cu). by stressing the importance of the weighting factor. the present approach emphasizes the need for choosing the correct extrapolation function. A comparison between the present method (the Linear method) and Cohen's method indicates that the Linear method may be more appropriale in certain cases. through a priori no critertion appears to he available for making a chorce between the methods. The size of hexagonal and tetragonal crystal lattices is determined by two parameters, a, and c,. Although in principle the two lattice parameters can be determined independently from reflections for which h - k = 0 and 1 = 0, respectively, in practice this may be inconvenient (because of the angular positions at which these reflections may occur) or not easily possible (because of low intensity). Furthermore, if a high precision or accuracy is required, the limited number of reflections of this type available, particularly in the high-angle region, is not sufficient for the necessary corrections (mainly due to absorption) to be determined with accuracy. Several methods1-7,11-13 have been proposed employing all reflections, to obtain the optimum values, a. and co, either by a trial and error procedure or a least-squares fit. Of the latter method, cohen's5 is the best known one since it provides explicit expressions for the optimum a. and c,. However, Cohen's method is only strictly valid if an extrapolation function is used that varies linearly with l/a2 or lie2 (see Section 3), a requirement that does not appear to be generally appreciated. On the other hand, all the better known and more widely used A recent trial and error method was proposed by Massalski and King8,7 who computed extensive auxiliary tables of axial ratios vs the functions A = [(4/3)(h2 + hk +k2) + l2+(a/c)2] and C = A(c/a)2 used in computing a and c values from the observed Bragg angles. These values of a and c were then plotted against a function which permitted linear extrapolation. As a criteria; for the "optimum" values, Massalski and King rely upon a visual fitting of the line through points representing reflections of low 1-index points to compute the extrapolated value of ao and high 1-index reflections to obtain CO. The successive computations and graphical plotting required to reach the "optimum" value are quite lengthy and tedious even on a desk calculator and no quantitative assurance is obtained of having in fact selected the optimum value.* If the method of Massalski and King is used on an electronic computer, then their published tables become redundant and a least-squares fit becomes a natural selection for the choice of optimum values. Such an approach will be called the Linear method. For work now in progress on the effect of certain physical variables on the lattice parameters of hexagonal crystals, it has become essential to determine the confidence limits of small changes in the lattice parameters. Since extrapolation functions that varied linearly with a and c actually also appeared to vary linearly with l/a2 or l/c2 when tested against published as well as our data, a comparison of Cohen's method and the Linear method was considered desirable (Sections 3 and 4). For the latter method an electronic computer was required since a reiterative procedure to obtain the optimum ao and co values had to be employed. The purpose of this paper is to describe the principles of the Linear method, illustrate its application, and compare it with Cohen's method. 1) THE LINEAR METHOD The standard practice in obtaining the lattice parameters in the Debye-Scherrer method is to

Jan 1, 1965

By B. G. Reisdorf

This paper describes the microstructural changes that occur when quenched ultrahigh-strength steels containing OA pet C and various amounts of nickel, silicon, and cobalt are tempered. The changes that occur in hardness, yield strength, and martensite diffraction-peak widths when these steels are tempered are related to the precipitation of the carbide phases. An unea$ectedly high silicon content (about 30 pct) was found in the E -carbide phase in a steel containing only 1.5 pct Si. TEMPERED martensitic steels have such wide-spread utility that they have been the subject of numerous investigations, and a sizable amount of literature has developed on this subject.M This investigation, which is a part of a larger program to correlate microstructure with mechanical properties at a variety of strength levels, is limited to the microstructural changes that occur when a quenched 0.40 pct carbon steel (USS Airsteel X-200 steel) is tempered, and to the effects of the alloying elements—nickel, cobalt, and silicon—on these microstructures. Used in this investigation were electron microscopy, electron-diffraction identification of the carbide phases, electron-probe micro-analysis of the carbides, X-ray determinations of retained austenite, and measurements of martensite X-ray diffract ion-peak widths. MATERIALS AND METHODS The chemical analyses of the eight heats examined eats No. 30 through 37) are shown in Table L Heat No. 30 has the chemical com~osition of Airsteel X-200, and the remaining seven heats contain various amounts of nickel, chromium, cobalt, and silicon. The heats were air-melted in an induction furnace and cast into 8 by 8 in. ingots that were subsequently heated to 2300 and rolled to 1-in.-thick plate. Oversize 0.505-in.-diam tensile specimens were rough-machined from the plates and austenitized in air at 1700° F for half an hour and oil-quenched. The specimens were then tempered in air at temperatures of 400° to 1000 for tempering times of 1, 4, and 16 hr, and finish-machined to 0.505-in.-diam tensile specimens. Electron micrographs were prepared from Formvar replicas of the midthickness of tensile-specimen shanks that had been electrolytically polished and etched in nital. Electron-diffraction patterns were obtained from carbon-extraction replicas. The replicas were prepared by etching the sample surface in the same manner as for microscopy, evaporating carbon on the etched surface, and re-etching the sample to free the carbon film and the precipitate particles. Electron-probe microanalysis was performed on some of the extraction replicas. To obtain adequate fluorescent X-ray intensities, several thicknesses of replica were exposed to the electron beam so that the results represent an average composition of the extracted particles rather than an analysis of single precipitate particles. The retained austenite contents of the specimens were determined by an empirical X-ray diffraction

Jan 1, 1963

By R. W. Raymond

(Cleveland Meeting, October, 1912.) UNDER the names of Conservation, Social Justice, the New Nationalism, and Progressive Democracy, many earnest reformers are calling for a new system of Federal government to replace the one which they ascribe to our fathers, and declare to have been outgrown. They are proposing the lease by the United States of certain natural resources on the public domain, for the profit of the U. S. Treasury, instead of the sale of such resources to private citizens or associations of citizens. In the present paper, I shall try to show that this notion is neither new nor good. It is clear that the United States is owner, as well as sovereign, of public lands acquired through conquest or purchase from other nations, as it was owner of the public lands expressly ceded to it by the original thirteen States. Its policy with regard to such lands involves, therefore, two entirely distinct questions: What shall it do as owner ? and, What shall it do as sovereign ? The latter question, it must be confessed, has played but a small part in our history. All the prerogatives of sovereignty which were not explicitly conferred upon the Federal government by the original States were retained by them. The ownership or control of precious or other metals or minerals in the earth, for instance, was thus reserved to the several sovereign States. New York, South Carolina, and other States have passed laws on this subject, without regard to Federal authority. As new States have been successively admitted to the Union, the tacitly accepted theory has been,. that they thereby acquired all the reserved rights of the original States. These newer States largely outnumber the first. thirteen; and it is inconceivable that they would submit to any deprivation of sovereignty based on historical grounds. One of them-Texas-came into the Union by its own voluntary

Oct 1, 1912