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Discussion of the paper of Robert R. Abbott, presented at the New York Meeting, October, 1913, and printed in Bulletin No. 82, October, 1913, pp. 2389 to 2400. ALBERT SAUVEUR, Cambridge, Mass.:-Mr. Abbott has certainly made a strenuous effort to ascertain the influence of the various elements on the absorption of carbon by steel-a subject of great importance to those dealing with the case hardening of that metal. Because of the extensive and careful character of Mr. Abbott's experiments, one is all the more disappointed that his results, as he himself recognizes, are not more satisfactory; for, indeed they leave us just about where we were,-still entertaining uncertain views in regard to the carbon-absorbing power of various alloy steels. It might be asked whether Mr. Abbott's method of estimating the amount of carbon absorbed-namely, by weighing the specimens before and after the carburizing treatment-was the best one to select. Are not serious sources of error. inherent to such procedure because of the difficulty of satisfactorily removing the earburizing material attached to the specimen ? The method of least squares has certainly failed to solve the problem satisfactorily. By manipulating Mr. Abbott's results in a different manner I have obtained the following expression: P = 100 - 50 C - 7 Ni + 20 Cr, in which P represents the carbon-absorbing power; C, the percentage of carbon; Ni, that of nickel; and Cr, that of chromium. It is assumed that the carbon-absorbing power of pure iron, or what might be called its carburizability, is represented by 100. Applying the formula, for instance, to a steel containing 0.15 per cent. C, 3 per cent. nickel, and 0.50 per cent. chromium, its carbon-absorbing power would be 100-50X0.15-7X3+20X0.50=81.50; that is, 81.50 per cent. of the carbon-absorbing power of pure iron.

Jan 12, 1913

By T. P. Floridis, J. H. Young

The need for close control of the phosphorus content of steels has led to numerous investigations on the equilibria of the dephosphorization reactions. Winkler and chipman1 have established the general conditions for effective dephosphorization of steel. They are high slag basicity, high oxygen potential, and low temperature. Other investigators have made additional contributions to the understanding of the dephosphorization process. The current status of the understanding of the dephosphorization of steel is concisely presented by Bodsworth2 and by Ward. The investigation reported in this communication was undertaken with the purpose of establishing the effect of additions of barium oxide and calcium fluoride on the dephosphorizing capacity of slags. Esin and Gel'd4 proposed that barium oxide, being more basic than calcium oxide, should cause an increase in dephosphorizing capacity when added to steelmaking slags, or when used as a substitute for calcium oxide. Derge5 has also proposed that in the future conventional slags might be replaced by BaO-Al2O3 slags. There is, however, no experimental evidence confirming the effect of barium oxide on the dephosphorizing capacity of slags. The effect of calcium fluoride on the dephosphorization of steel is not clearly understood. It is generally recognized that additions of calcium fluoride are beneficial. It is not clear, however, whether calcium fluoride affects the equilibrium of the dephosphorization reaction, or whether it simply causes an increase in the fluidity of the slag and, consequently, faster approach to equilibrium. The experimental procedure consisted in equilibrating synthetic molten slags with liquid copper at 1550°C under a gas stream containing argon, hydrogen, and water vapor. In all experiments the argon to hydrogen ratio was approximately 4:1, and the hydrogen to water ratio was 5.42:l. Molybdenum crucibles were used as containers for the slag and metal. Under the above-described conditions of temperature and composition of atmosphere, there was no observable attack of the crucibles by the metal, slag, or atmosphere. Copper was used instead of iron, because iron attacks molybdenum. The equilibration was made in a tubular furnace consisting of a recrystallized alumina tube. The alumina tube was heated by electrical resistance. A Pt-40 pct Rh wire winding was used for most runs. A silicon carbide tubular resistor was also used for some runs. Temperatures were measured with a Pt-Pt-Rh (10 pct Rh) thermocouple and kept constant within ±5°C. Equilibrium was approached from both sides, i.e., by adding the phosphorus either as oxide in the slag or as a phosphorus-rich alloy of phosphorus and copper. The holding time at the equilibrium temperature was 6 hr. At the end of each run the crucibles were rapidly cooled and removed from the furnace. The slag and metal were separated and analyzed. The experimental results are shown in Table I. The phosphorus content of the slag is expressed both as percent phosphorus pentoxide and as percent phosphorus. The basicity ratio is computed by dividing the number of moles of basic oxides-oxides of barium, calcium, magnesium, and sodium—by the number of moles of acidic oxides- oxides of aluminum, phosphorus, and silicon. Calcium fluoride is not included in the computation of the basicity ratio; i.e., calcium fluoride is assumed to be neither basic nor acidic. The distribution ratio of phosphorus—percentage of phosphorus in the slag divided by the percentage of phosphorus in the metal- is plotted in Fig. 1 against the basicity ratio. The results indicate that slags containing barium oxide have greater dephosphorizing capacity than slags containing calcium oxide. The high dephosphorizing capacity of slags containing sodium oxide and the low dephosphorizing capacity of magnesia-containing slags which already have been reported in the literature2 are confirmed by the results of this investigation. It appears that calcium fluoride has a beneficial effect on the distribution of phosphorus between slag and metal in acid slags only. Although the obtained distribution ratios between the phosphorus contents of slag and copper are not directly applicable to the dephosphorization of steel, they are sufficient for evaluating the effect of slag additions on the dephosphorizing capacity of slags in general. An increase in the ratio of distribution of phosphorus between slag and metal indicates lowering

Jan 1, 1968

By D. C. Buffum, L. D. Jaffee

QUANTITATIVE measurements of the temper brittleness of steel are made by comparing the difference between embrittled and unembrittled specimens in the temperature of transition from ductile to brittle fracture. Since hardness affects the transition temperature, a study of the combined effects of hardness and temper brittleness appeared desirable. In this investigation a commercial SAE 3140 steel, which has been reported on previously in temper brittleness studies,* was used. Blanks from this steel were austenitized for 1 hr at 900°C and water quenched. The blanks were then divided into six groups and further heat treated as follows: Group 1—tempered at 675°C for 4 hr and water quenched; Groups 2, 3, 4, and 5—tempered at 675", 650°, 625', and 600 °C respectively for 1 hr and water quenched; and Group 6—tempered at 500°C for y2 hr and water quenched. Each of these groups was divided into two parts; one part was tested without further heat treatment, and the other was embrittled for 48 hr at 500°C and water quenched. Tempering treatments between 500" and 600°C were avoided because of the rapid embrittlement occurring in that range for this steel. The heat-treated blanks were machined into standard V-notched Charpy bars. Each group was tested over a range of temperatures on a 217 ft-lb Charpy machine. The energies necessary to fracture the bars and the percentage fibrous fracture of each bar were recorded. The transition temperatures were obtained from a plot of the percentage fibrous fracture as a function of testing temperature. They were taken as the lowest point on these curves at which the fracture was 100 pct fibrous. The transition temperatures for both embrittled and unembrittled specimens are presented in Fig. 1 as function of the hardness. It will be noticed in this figure that the point for the unembrittled condition at 21 Rockwell C is out of line. These specimens were tempered for 4 hr at 675 °C and this point indicated that under isothermal conditions at this temperature, as is well known, embrittlement may develop fast enough to more than offset the effects of softening. From this data, it was concluded that the difference between transition temperatures for the embrittled and unembrittled conditions at any given hardness, within the range of Rockwell C 24 % to 32lh, is constant. It is also concluded that, within the hardness range studied, the transition temperatures for embrittled and unembrittled specimens rise in a parallel fashion with an increase in hardness. The authors wish to acknowledge the assistance of Frank Carr in this work.

Jan 1, 1952

By F. E. Bash

IN recent years, there have been a number of experiments conducted to determine the rates of heating and cooling of various sizes and shapes of steel ingots. Up to date, however,-most of the published data has dealt with small sized ingots, the largest being an 18-in. (46 cm.) cube, the data on which was presented before the Iron and Steel Institute in May, 1918, by E. F. Law. It is due to thus lack of information on the rate at which large ingots absorb heat and come to temperature that the heating- practice varies so widely in different plants. One of the questions over which there is much debate is the proper rate of heating of large ingots for forging and the time actually required for the center of a mass of steel to come to forging temperature. As a continuation of experiments described by M. E. Leeds1 and at the request of Mr. G. R. Norton of the Sizer Forge Co. and Mr. R. C. Drinker of the Emergency Fleet Corpn., the test described in this paper was carried out on a 24-in. (61 cm.) round ingot and the rate of heating and cooling determined under regular production conditions. The ingot had been partly forged at one end but, on developing a flaw, had been scrapped so that it was available for test. The size and shape of the ingot and its position in the furnace are shown in Fig. 1.

Jan 9, 1919

By H. E. Stauss, G. Sandoz

THE purpose of this note is to draw attention to the possibility that a melt may be contaminated by a material not in direct contact with it by means of gaseous intermediate agents. In recent years silicon has assumed a position of importance because of its use in rectifiers and transistors and close attention has been required to control of both purification and contamination during all stages of preparation.' This note reports the observation that a graphite heater may have contaminated silicon ingots without direct physical contact through reactions that developed gaseous products. Several ingots made with the equipment of Hino and Stauss,2 using a graphite heater in a dried helium atmosphere, were found to have a small amount of a very hard substance on the free surface. X-ray analysis by F. W. von Batchelder showed the sub- stance to be Sic. Similar contamination was not found when the heater was tantalum, indicating that the carbon had not come from an original impurity in the silicon powder. One source of the carbon could have been volatile matter released from the graphite heater. This heater had been used about ten times at the time of the observations. A second source of carbon could have been a direct reaction between the quartz crucible and the graphite heater to form CO, or an indirect reaction involving a crucible-melt interaction and volatile SiO as an intermediate product. Such reactions should have developed Sic on the heater; and in fact a yellow powder did form on the inside of the graphite heater although its composition could not be determined. References 'H. C. Torrey and C. A. Whitmer: Crystal Rectifiers (1948) Chapter 10. New York. McGraw-Hill Book Co. 2 J. Hino and H. E. Stauss: Trans. AIME (1952) 194, p. 656; Journal of Metals (June 1952).

Jan 1, 1954

By B. H. Kear, H. G. F. Wilsdorf

After a few percent strain, dislocations in disordered Cu3Au are arranged in groups in ulell-defined slip planes, which contrasts with the more or less random distribution of dislocations in the corresponding ordered alloy. Unusually long and straigkt dislocation segments observed in the ordered alloy are interpreted in terms of cross slip of screw dislocations from their slip planes into cube planes. It is proposed that cross slip, and also dislocation reactions of the Lomer type, play an important role in work hardening of the ordered alloy. ACCORDING to to dislocations in the disordered lattice are only partial dislocations in the corresponding super lattice, so that in the super-lattice dislocations must occur as pairs, with each pair connected by a ribbon of antiphase boundary. Recently, striking confirmation of the theory was obtained by Marcinkowski, Brown, and Fisher3j4 in a study of dislocation configurations in thin foils of the Cu3Au alloy by transmission electron microscopy. In the present investigation, the observations made by these workers have largely been confirmed. Moreover, it has been found that dislocations in the plastically deformed ordered alloys are often unusually long and straight. This paper is mainly concerned with these new observations. A tentative explanation is offered in terms of cross slip of dislocations in the ordered alloys. PREPARATION OF SPECIMENS An alloy close to the stoichiometric composition Cu3Au was prepared by melting together high-purity copper and gold (99.995 pct) under vacuum in a graphite mold. The resulting ingot was rolled down and cut into strips 1 1/2 by 1/8 by 0.005 in. in thickness. All strips were annealed at 900°C for 3 hr and cooled to 500'~. A few of the strips were quenched from ~OO'C, while the remainder were slowly cooled in the temperature range 400" to 150°C at intervals of a few degrees every 24 hr to produce a high degree of order. After this annealing treatment the average grain size of the material was about 0.1 mm. Material in different states of order was obtained by reannealing fully ordered material at temperatures below the critical temperature: followed by quenching. The equilibrium degree of order attained at a particular reannealing temperature was obtained from the paper by Keating and warren.' A simple hand-operated tensile jig was used to give the strips the required amounts of plastic strain. Following straining, a number of specimens were cut from each strip by means of an electrolytic cutting device.= Finally, each specimen was thinned electrolytically using the polishing procedure described by Bakish and Robertson,7 and these thin sections were examined in the Philips EM-100B electron microscope operating at 100 kv. EXPERIMENTAL OBSERVATIONS Antiphase boundaries. The average domain size in the ordered alloys was found by direct observation to be about 0.25 p. Also, it was observed that the grown-in configuration of antiphase boundaries was changed little by plastic deformation, at least up to 6 pct strain. Fig. 1 shows an electron micrograph of a thin foil of partially ordered alloy (S - 0.8) after 3 pct strain. The micrograph shows a few dislocation pairs and a somewhat crystallo-graphic network of antiphase boundaries. The normal to this foil was found by diffraction analysis to be approximately 11121, with principal directions in

Jan 1, 1962

By Niels Hansen

Dispersion-strengthened aluminum products consist of an aluminum matrix containing finely distributed ceramic or intermetallic particles. Examples of the two types of product are SAP, in which the dispersed phase is aluminum oxide, and materials made from atomized aluminum alloy powder, in which the dispersed phase can be FeA1, particles.' A fundamental difference between the two types of product is that the elongation of aluminum/aluminum oxide products decreases with increasing temperature, whereas the elongation of aluminum- FeA13 products, like that of aluminum alloys, increases with increasing temperature. As regards the structural stability, aluminum/aluminum oxide products are stable to temperatures above 600° C as aluminum oxide does not react with aluminum, whereas prolonged heating at above 400°C of aluminum-FeA1, products leads to coarsening of the intermetallic phase and loss of strength.' On the basis of these results it is supposed that a dispersion-strengthened product combining strength, ductility, and stability at elevated temperatures may be obtained if the dispersed phase reacts with the matrix in such a way that the reaction does not proceed at any significant rate at the application temperature. Different ceramic or intermetallic compounds may be selected as the dispersed phase, and, as alloying of the matrix phase may also influence the reaction, many possibilities exist for each metal. In the present study, aluminum products containing different oxides have been examined. For a reaction to take place between the dispersed oxide and the aluminum the free energy of formation of the oxide (MeO) must be greater than that of aluminum oxide; the difference should, however, not be too great in order to limit the reaction rate. Furthermore the aluminum alloy formed when aluminum reacts with the dispersed oxide should have a melting point near

Jan 1, 1969

By Eli T. Conner

WITH Thomas G. Fear, chairman of the Coal Di- vision, presiding, the coal miners opened their program Monday morning with a general session at which three papers were presented. The first, "The Classification of Coal for Stationary Steam Generation," was presented by the author, Thomas W. Harris, Jr. In discussion, H. T. Coates inquired if it would not be possible to pick out a geographical coal section, certain seams or a group of mines, which would rank high in a desired feature or features, perhaps giving different -- - local sections or different mines something to designate a rating ("good," "fair," and "poor"). This might be done relative to anti-clinkering, free-burning, ,anti-slagging, smokelessness, friability and grindability. These might be listed or arranged on a map or diagram so that the prospective customer could find a coal that rated particularly high in desired characteristics. C. A. Reed pointed out, in part, that coal producers and sellers have found a bad but necessarily present condition in the country, especially with the smaller user of coal. This is entirely due to the fact that the employer expects his purchasing representative to be a genius and have expert knowledge of everything he buys, coal included, whereas in the larger plants he has and uses expert knowledge from the active organization when necessary. J. B. Morrow said that size rating was important in classifying coal and he emphasized that it was impossible to come to a definite basis on analysis alone.

Jan 1, 1933

By F. N. Rhines

STUDIES upon the sintering of metal powders, in the solid state, have led to the proposal that the surface energy of the powder particles provides the driving force that causes points of contact between pairs of particles to grow into broad welds which isolate the residual vacant space into pores that tend to spheroidize and gradually to diminish in total volume.' Investigators differ with regard to the mechanism of the movement of the metal, under the influence of surface energy, to accomplish these changes. One school asserts that there is a mass movement of the metal, referred to as a "viscous flow," while the other school prefers to view the movement as a self diffusion process, wherein individual atoms are, transferred without disturbance of the basic pattern of the crystal lattice. Extensive experimental studies upon the sintering of copper, conducted recently by A. J. Shaler,2 have been in- terpreted by their author as support for the viscous flow mechanism of transport, the theory of which was developed originally by J. Frenkel.3 Duplicating a portion of this work with minor changes, G. C. Kuczynski4 is led to the alternate view, namely, that the initial stages of sintering, at least, proceed as a self-diffusion process. Both of these investigations were designed to deal with an isolated unit of sintering, i.e., with the shrinkage of a single pore, or with the growth of a single point weld. It remains to ascertain the behavior of a typical metal powder compact composed of a large number of particles of varying size and sintering to a body with a multiplicity of pores. The observation of density changes alone during sintering is not sufficient in such a case; it is essential to know how the internal geometry of the compact changes. This has been the object of the present investigation, the results of which are used to support the self-diffusion mechanism of sintering. The present studies consist in the measurement of the number of pores as a function of size and time at temperature during the sintering of a copper compact made from a commercial copper powder lightly pressed and sintered in several different atmospheres. A brief survey was made also of the change in shape of the pores, under the influence of the same variables. All of this was done by direct observation with the microscope. Densities were measured on the same sample. It is found that, while the compact is exhibiting an overall shrink-

Jan 1, 1951

By J. Larsen-Badse

The resistance to dry sliding abrasion us been measured for some hardened and tempered carbon steels. The wear resistance, defined as the reciprocal of the volume loss per unit sliding distance, is found to vary linearly with the hardness of the abraded surface. The data fit two lines, one, of high slope, for the pure metals and for the annealed steels and another, of smaller slope, for the hardened and tempered carbon steels. A relationship is developed showing the alwasion resistance to be proportional to the hardness of the material and to en, where n is the exponent of work hardening. The values of n and of the hardness FOR most materials a high resistance to abrasion is generally associated with a high value of indentation hardness. Brine11 even used the abrasion resistance as a measure of hardness in an attempt at expanding the hardness range covered by his indentation-hardness test.' When comparing different types of materials there is, however, only a very general relation between abrasion resistance and hardness. Sample brittleness seems to contribute to the deviation from a direct relationship. In general, increased brittle- are those relating to the heavily deformed abraded surface. However, for materials having n constant or varying m a regular manner over a wide range of strailts, the wear resistance will also be a linear function of the bulk hardness of the material. For tempered steels containing a dispersion of cementite in ferrite the increase in wear resistance due to the dispersion is found to be a linear function of the volume fraction of Fe3C and of the reciprocal of the mean free ferrite path. This indicates indirectly that the yielding of this material, when it is already heavily deformed, follows the Orowan criterion. ness leads to decreased abrasion resistance.' When comparing materials in the same group, e.g., the metals, the spread is less. Kruschov found that the abrasion resistance of pure metals and of annealed steels is directly proportional to the hardness of the metal. For hardened and tempered steels he obtained another linear relationship, one of smaller slope and intersecting the line for the pure metals at the location of the data for the annealed steels. He also found that the abrasion resistance of cold-worked metals is independent of the degree of cold working. This shows, as he concluded, that the process of abrasion work hardens the metal in the surface region to a very high degree.

Jan 1, 1967

By R. D. Reiswig

An increasing amount of high-temperature metall~?~gical research is carried out in resistively heated tube furnaces in which a bare specimen is suspended by a fine wire at the midpoint of the tube. It is shown that the assumption of near-blackbody conditions on the surface of the sample may give rise to errors in optical pyrometry of 50°C or more. A number of papers published in the metallurgical literature in recent years have described the use of high-temperature tube furnaces for heat treatments, melting-point determinations, and other work. Typically, the tube is of a refractory metal with open ends, is heated by the passage of an electric current, and has concentric cylindrical radiation shields outside it. In at least one of these,' the specimen is contained within a crucible having a small hole in its lid through which optical-pyrometer measurements are made under essentially blackbody conditions. In another design,* the specimen is inside a muffle which is concentric with the heater tube and which contains a number of washerlike longitudinal radi- ation shields to reduce axial temperature gradients and to give conditions near the specimen closer to those of a black cavity. Yet another design3 employs a wire specimen coaxial with the heater tube. Blackbody conditions are simulated by passing current from a separate supply through the wire until it "disappears" against the background (the inside of the heater tube) as seen through a radial spy hole in the tube. Good agreement with known melting points is achieved when an optical pyrometer is used under such disappearance conditions as the melting point is approached. That this latter method works so well is due, evidently, to considerations such as those mentioned by Dike4 and others.5-8 A more common method than the above, however, has been the suspension of an uncovered specimen by a fine wire in a resistively heated tube with open ends. A radial spy hole about midway between the ends of the tube permits optical-pyrometer observations on the specimen, the inside of the tube, or both. So observed, the specimen typically appears to differ but little in brightness temperature from the inside of the tube. According to De vos9 the radiation from such a spy hole in an empty tube of reasonable 1ength:diameter ratio (e.g., 10 or greater) should be essentially blackbody radiation. For these reasons, apparently, descriptions of work carried out in such furnaces usually include a statement to the effect that conditions surrounding

Jan 1, 1964

By W. C. Knopf, G. Samsel

For several years International Minerals & Chem-ical Corp. has used a radiation method to assay potassium content of products from potash and feldspar beneficiation. The procedure is rapid, accurate, and inexpensive and is easily handled, if necessary, by nontechnical personnel. Data are presented to show the accuracies that may be expected if the technique is used for control of pilot plants or large-scale plants. Natural potassium is composed of three isotopes —K, K and K. Five other isotopes, artificially produced, have been detected. In natural potassium only the K isotope, with a half life of 1.4x10 years, is radioactive. Its modes of decay are beta and gamma rays, positrons, and x-rays. Only the more abundant beta rays, however, are important in radiation measurements using geiger tubes. Barnes and Salley' measured radiation of potassium salts in solution in 1943. Gaudin and Parnell2 first reported the use of solid salts arranged in a vessel surrounding the ß counter in 1948. Later, Scheel used the method to assay potassium content of various crude and finished potash salts. Experimental: Dip-type Geiger-Muller tubes (TGC-5) supplied by Tracerlab Co. were used in all radiation counting measurements. The tube was encompassed by a glass container about M in. larger in diameter than the tube. This container, which served as a sample holder, was closed at the bottom with a rubber stopper to facilitate removing the samples. Samples were not weighed, but about 40 g of sample were needed for each test. Electrical impulses from the tube were counted on either a Tracerlab scaler or a rate meter. To obviate the need for constant attendance, preset features were incorporated into the scalers, so that at a predetermined time or count the units were automatically deactivated. When rate meters were used, counting rates were read directly from instrument or from a recorder used in conjunction with the rate meter. Each tube was calibrated, according to the manufacturer's instructions, to determine the correct operating voltage to insure reproducible results. A linear calibration plot of percent K2O vs counting rate was also obtained for each tube by recording the counting rate plus background count of several standards of different K2O content chemically analyzed by the chloroplatinate method.' These standards were of approximately the same particle size distribution as samples to be assayed. Specific background count caused by cosmic rays and other surrounding radiation was checked periodically by counting a sample of pure NaCl. Fig. 1 is a representative calibration plot. Assays were determined directly from the standard plot or calculated by subtracting the background count from the counting rate, then multiplying by the slope of the line. Chemical assays of the test samples were made by the Sherril method," a flame photometric technique, or the chloroplatinate method. Data: The radiation assay method has been used for three years by International Minerals & Chemical Corp. in the laboratory and in pilot plants processing ores containing potassium. These dry concentration plants process sylvinite and langbeinite ores at Carlsbad, N. M., and feldspar ores at Top-sham, Maine. Sylvinite ore is predominantly a mixture of syl-vite (impure KCl) and halite (impure NaCl). Contaminants include sulfates, such as langbeinite (2MgSO - K2SO4), kieserite (MgSO H2O), poly-halite (MgSO4.K2SO, 2CaSO, . 2H2O), and slimes. Langbeinite ore is predominantly langbeinite and halite with small amounts of sylvite, sulfates other than langbeinite, and slimes. Several variables, in addition to correct calibration and standardization of tubes, were found to be important in obtaining reproducible results. Particle size distribution of standard samples should be

Jan 1, 1959

By Pol Duwez, Paul Pietrokowsky

The crystal structure of the compound TisGeS has been determined from X-ray powder diffraction data. Related silicon and tin compounds have been found to be isomorphous. Unit cell dimensions, axial ratios, and parameters for equivalent atomic positions are given. THERE is, at present, only meager information pertaining to the solid state reactions of titanium with the elements in group 4B of the periodic table (silicon, germanium, tin, and lead). The only two compounds whose crystal structure has been established are TiSi² and TiGe² (references 1 and 2 respectively). These two compounds are isomor-phous and have an orthorhombic symmetry D242h— Fddd. The titanium-rich regions of the constitution diagrams of titanium-silicon, titanium-tin, and titanium-lead have been investigated by Craighead et al.³ While valuable information concerning the alpha solid solubility of these three elements in titanium was obtained, no light was shed on the existence or nature of the titanium-rich compound in these systems. The present study is concerned with the crystal structure of the intermediate phases Ti5Si ?, Ti³Ge³, and Ti5Sn³, which were found to be isostructural. The alloys were prepared by mixing the pure metal powders in the desired proportions, pressing the mixture into pellets, and melting them in an electric arc furnace in the presence of a helium atmosphere.& After melting, the specimens, weighing approximately 5 g, were sealed in evacuated quartz vials, homogenized at 1038°C for three days, and quenched from that temperature. Powder diffraction patterns were made with a 143.2 mm diam Debye-Scherrer X-ray camera in which the Ievins and Straumanis film arrangement was utilized. Filtered copper radiation was used throughout the entire investigation. A study of the powder patterns of a series of alloys of various compositions indicated the presence of a compound around a composition corresponding approximately to a ratio of 3 titanium to 2 silicon, germanium, or tin. From a visual examination of the diffraction patterns, it was evident that the silicon and germanium alloys were iso- morphous. For small angle reflections, the powder pattern of the tin compound was analogous to that of the silicon and germanium compounds, but after the first ten reflections, the similarity was no longer clear. The powder pattern of the germanium compound was selected for indexing, since it exhibited a weak small angle reflection and clearly resolved doublets in the back-reflection range. Good agreement between observed and calculated values of (1/d)² was found by indexing the pattern on the basis of hexagonal symmetry. For the hexagonal system:

Jan 1, 1952

By J. N. Hobstetter, J. J. Becker

Deformed copper single crystals exhibited, upon annealing, a recrystallized twinned grain with a twin plane parallel to an active deformation plane, rotated approximately 22" about its pole, or else did not recrystallize at all. If extraneous deformation was not carefully removed, no simple orientation relationship was found. RECRYSTALLIZATION textures have been a subject of practical interest for many years, but any real understanding of their formation will have to start with a study of the recrystallization of carefully deformed single crystals. Some efforts have been made in this direction,'-' but much more experimental information is needed before a satisfactory picture of the crystallography of recrystallization can be formed. This paper reports a few results in copper single crystals. The crystals studied in this investigation were grown by the Bridgman method," and their orientations determined by the back-reflection Laue technique." Some specimens were simply deformed in compression, others were sheared, and still others tested in a rotating-grip device, in attempts to remove end constraints. The details of their deformation behavior are described elsewhere.' The deformed specimens were annealed and the orientations of the recrystallized grains were determined optically, as described by Barrett and Levenson.8 Compressed Specimens Specimen 17-A, whose orientation is given in Fig. 1, was compressed to a total of 19 pct. As observed before,' increasing deformation took place by increasing density of slip lines in initially formed clusters, with little if any formation of new slip clusters in unslipped areas. The specimen was then etched in nitric acid until its length had been reduced from 0.766 to 0.735 in. It was annealed at 1000°C, in increments of a few minutes. After 63 min, two small grains had appeared in the center, Fig. 2. They were found to be twinned with respect to each other (AB, Fig. 4). After 30 min more, the specimen was completely recrystallized. A typical view of it is given in Fig. 3. A summary of all orientations found is given in Fig. 4, in which the prominent grain G is in (001) standard projection, and the poles of the active slip planes after deformation are indicated by SP (primary slip plane), CrSP (cross-slip plane), and CnSP (conjugate slip plane). All the orientations found were related through seven orders of twinning. A "family tree" of these twins is given in Fig. 5. Furthermore, the BG twin composition plane lies close to the cross-slip plane

Jan 1, 1954

By J. Laskowski

J. Laskowski (Associate Professor, Dept, of Mineral Processing and Coal Preparation, Silesian University of Technology, Gliwice, Poland) -Referring to the papers by J. A. L. Campbell and S. C. Sun, I must say that I am very pleased to see that type of work, because it is the only way to progress towards an understanding of flotation mechanisms. All those interested in the science of the surface chemistry of coals would find these papers a valuable contribution to the literature. In their extensive research, the authors attempt to synthesize their findings into a theory of coal flotation. To do this, the zeta potential of bituminous coals and their lithotypes, as well as that of an anthracite coal, was measured and H+ and OH- ions were found to be potential determining ions. The measured ZPC of bituminous coals was at a pH range from 3.5 to 4.6 and for the anthracites between 2.0 and 4.5. The authors have pointed out that since the hydrophobicity is pH-controlled, the flotation mechanism should also be. The Campbell and Sun papers confirm a good many of the conclusions on surface properties of coals reported in recent years. It is noteworthy to point out that the ZPC found in the paper on bituminous coals was approximately pH 4, similar to the ZPC for the anthracite coal. In fact, we have been investigating different coals from low to high ranks. Thus, the plot of the pH for ZPC against rank could be derived and this curve-an electrocapillary one-indicates a pH near which the hydrophobicity of the coal surface should be at maximum. This can be proved by so-called salt flotation, which, in a sense, can be treated as method of surface charge measurement. It is obvious that the salt flotation experiment is possible when the native hydrophobicity of the mineral surface is high, e.g., when the solid surface does not have an orienting influence on an adjacent water layer and the hydration layers are controlled by the electrical double-layer potential. The addition of electrolyte or a change of pH which decreases the thickness of the stabilizing double-layer "opens up" the hydrophobic surface micro-area mosaic. Thereby the surface becomes hydrophobic and particles become floatable. The orienting influence of surface on hydration layer increases even after very slight oxidation and flotation is affected by it. It seems that such an explanation agrees reasonably well with those of Campbell and Sun.

Jan 1, 1972

By C. L. HUSTON

MY ANCESTRAL connection with the manufacture of boiler plate runs back through four generations, and my personal acquaintance with the practice reaches back to the time, in my ,boy- .hood days, when iron plates' were made in a mill operated entirely by water power. -The mill originally was driven by an old-fashioned "'breast" water wheel 20 ft. in diameter and with a20-ft. face, geared direct to the roll train. When the mill slowed up and there was danger of its stalling, the men would jump upon the rim and help the wheel around with their weight, to prevent a "sticker." Later, as large plates were called for, a flywheel was set out of line so that it could' be speeded up by gears from the water wheel and connected back again,. by reducing- gears, to the roll train. The flywheel, with its cast-iron rim and wooden spokes, made 90 r.p.m. and the roll train 45 r.p.m. In 1870, our company installed our first steam-driven plate mill two-high rolls, 84 in. long. In these early mills the hot metal was manipulated by hand.

Jan 1, 1920

By V. F. Swanson

At the AIME meeting in Tampa in Oct. 1966, an empirically developed equation was presented which allowed the calculation of free settling velocity for any sized particle: 1 [ ] This equation requires the use of two parameters a and p which are coefficients derived from boundary layer theory.2 It was possible to develop values of a and p for several minerals by back calculation of published data. The original equation had one major flaw. When the fluid density exceeds the density of the solids, the solution to the equation becomes imaginary. A flaw was indicated also by the fact that galena and sylvite both having cubic cleavage, did not have similar values for a and b. Galena gave calculated values of a = 1.082 and g = 3.11, while sylvite gave values of a = 1.870 and p = 2.56. These flaws prompted further study of the equation, resulting in the following empirical modification: [ ] It is obvious a real solution of the equation is possible for all values of ps and p. When PL > PS, V is negative, indicating that the particles will rise against the attraction of gravity. The validity of the modification is borne out by the fact that when values of a and p were back calculated for galena and sylvite using the modified equation, both minerals gave values of a = 1.038 and p = 3.01. With the modification shown in Eq. 2, Newton's friction factor becomes [ ]

Jan 1, 1976

By P. A. Laxen, H. R. Spedden

WHEN a mineral particle is fractured, bonds between the atoms are broken. The unsatisfied forces that appear at the newly formed surface are considered to be responsible for the adsorption of ions at the mineral surface. A knowledge of the mechanism and extent of ion sorption from solution onto a mineral surface is of interest in the development of the theory of flotation.'*' Study of the adsorption of sodium from an aqueous solution oftheon quartz offers a simple approach to this complicated problem. The availability of a radioisotope as a tracer element meant that accurate data could be obtained."." Three main factors which appeared likely to affect the adsorption of sodium are: l—concentration of sodium in the solution, 2—concentration of onotherof cations in the solution, and 3—anions present in the solution. Hydrogen and hydroxyl ions are always present in an aqueous solution. By controlling the pH, the concentration of these two ions was kept constant. The variation in thesethe amount of sodium adsorbed with variation in sodium concentration was then determined under conditions standardized in regard to hydrogen ion. The effect of concentration of hydrogen ions and of other cations was also measured. A few experiments were made to get a preliminary idea on the effect of anions. The active isotope of sodium was available as sodium nitrate. Standard sodium nitrate solutions were used throughout these experiments except when the effects of other anions were studied. It was found that sodium adsorption increased with sodium-ion concentration, but less rapidly than in proportion to it. Increasing hydrogen-ion concentration, or conversely decreasing hydroxyl-ion, brings about a comparatively slight decrease in sodium-ion adsorption. Increasing the concentration of cations other than hydrogen or sodium decreases somewhat the adsorption of sodium ion. It would appear as if the kind of anion is a secondary factor in guiding the amount of sodium ion that is adsorbed. Materials and Methods Quartz The quartz was prepared as in previous work in the Robert H. Richards Mineral Engineering Laboratory' except for the refinement of using de-ionized distilled water for the final washing of the sized quartz, prior to drying." To minimize the laborious preparation of quartz, experiments were made to determine .whether the sodium-covered quartz could be washed free of sodium and re-used. The experiments were successful as indicated by lack of Na" activity on the repurified material and by its characteristic sodium adsorption. Table I gives the spectrographic analyses of the quartz used. The quartz ranged from 16 to 40 microns in size, averaging about 23 microns (microscope measurement), and had a surface of 1850 sq cm per g (lot I), 2210 (lot 11) and 2000 (lot 111) as determined by the Bloecher method." Radioactive Sodium Method of Beta Counting for Adsorbed Sodium: Na22, the radioisotope of sodium, possesses convenient properties.' It has a half-life of 3 years, thus requiring no allowance for decay during an experiment. On decay it emits a 0.575 mev ß+ radiation and a 1.30 mev r radiation. The decay scheme is illustrated in the following equation: ß+ NaR-------'8'77NeZ2 3 years The /3 radiation is sufficiently strong to penetrate an end-window type of Geiger-Mueller counting tube. This, in turn, makes it possible to use external counting, a great advantage in technique. Furthermore, it permits the assaying of solids arranged in infinite thickness, while assaying evaporated liquors on standardized planchets. The equipment used was standard and similar to that employed by Chang.R The original active material was 1 ml of solution containing 1 millicurie of Na" as nitrate. This active solution was diluted to 1000 ml. Five milliliters of this diluted active solution was found to give a quartz sample a sufficiently high activity for accurate evaluation of the sodium partition in the adsorption measurements. Also, 1 ml of final solution gave a sufficiently high count for precision on the liquor analyses. The sodium concentration of the diluted active solution was 1.2 mg per liter, so that 6 mg of sodium for 60 ml of test solution and 12 g of quartz was the minimum amount used. The active solution was stored in a Saftepak bottle. Procedure for Adsorption Tests: The method consisted of agitating 12 g of quartz with 60 ml of solution of known sodium concentration for enough time to establish equilibrium between the solution and the quartz surface. The quartz was separated as completely as possible from the solution by filtering and centrifuging. The activity on the quartz and in the equilibrium solution was measured and the partition of the sodium was calculated from the resulting data. The detailed procedure for the adsorption test is set forth in a thesis by Laxen." In brief, it included the following steps: 1—Ascertainment of linearity between concentration of Na" and activity measured. 2—Evaluation of factor to translate activity on solid of infinite thickness in terms of activity on an evaporated active film of minute thickness, on the various shelves of the counter shield. 3—Taking precautions to avoid evaporation of water during centrifuging

Jan 1, 1953

By P. A. Laxen, H. R. Spedden

WHEN a mineral particle is fractured, bonds between the atoms are broken. The unsatisfied forces that appear at the newly formed surface are considered to be responsible for the adsorption of ions at the mineral surface. A knowledge of the mechanism and extent of ion sorption from solution onto a mineral surface is of interest in the development of the theory of flotation.'*' Study of the adsorption of sodium from an aqueous solution oftheon quartz offers a simple approach to this complicated problem. The availability of a radioisotope as a tracer element meant that accurate data could be obtained."." Three main factors which appeared likely to affect the adsorption of sodium are: l—concentration of sodium in the solution, 2—concentration of onotherof cations in the solution, and 3—anions present in the solution. Hydrogen and hydroxyl ions are always present in an aqueous solution. By controlling the pH, the concentration of these two ions was kept constant. The variation in thesethe amount of sodium adsorbed with variation in sodium concentration was then determined under conditions standardized in regard to hydrogen ion. The effect of concentration of hydrogen ions and of other cations was also measured. A few experiments were made to get a preliminary idea on the effect of anions. The active isotope of sodium was available as sodium nitrate. Standard sodium nitrate solutions were used throughout these experiments except when the effects of other anions were studied. It was found that sodium adsorption increased with sodium-ion concentration, but less rapidly than in proportion to it. Increasing hydrogen-ion concentration, or conversely decreasing hydroxyl-ion, brings about a comparatively slight decrease in sodium-ion adsorption. Increasing the concentration of cations other than hydrogen or sodium decreases somewhat the adsorption of sodium ion. It would appear as if the kind of anion is a secondary factor in guiding the amount of sodium ion that is adsorbed. Materials and Methods Quartz The quartz was prepared as in previous work in the Robert H. Richards Mineral Engineering Laboratory' except for the refinement of using de-ionized distilled water for the final washing of the sized quartz, prior to drying." To minimize the laborious preparation of quartz, experiments were made to determine .whether the sodium-covered quartz could be washed free of sodium and re-used. The experiments were successful as indicated by lack of Na" activity on the repurified material and by its characteristic sodium adsorption. Table I gives the spectrographic analyses of the quartz used. The quartz ranged from 16 to 40 microns in size, averaging about 23 microns (microscope measurement), and had a surface of 1850 sq cm per g (lot I), 2210 (lot 11) and 2000 (lot 111) as determined by the Bloecher method." Radioactive Sodium Method of Beta Counting for Adsorbed Sodium: Na22, the radioisotope of sodium, possesses convenient properties.' It has a half-life of 3 years, thus requiring no allowance for decay during an experiment. On decay it emits a 0.575 mev ß+ radiation and a 1.30 mev r radiation. The decay scheme is illustrated in the following equation: ß+ NaR-------'8'77NeZ2 3 years The /3 radiation is sufficiently strong to penetrate an end-window type of Geiger-Mueller counting tube. This, in turn, makes it possible to use external counting, a great advantage in technique. Furthermore, it permits the assaying of solids arranged in infinite thickness, while assaying evaporated liquors on standardized planchets. The equipment used was standard and similar to that employed by Chang.R The original active material was 1 ml of solution containing 1 millicurie of Na" as nitrate. This active solution was diluted to 1000 ml. Five milliliters of this diluted active solution was found to give a quartz sample a sufficiently high activity for accurate evaluation of the sodium partition in the adsorption measurements. Also, 1 ml of final solution gave a sufficiently high count for precision on the liquor analyses. The sodium concentration of the diluted active solution was 1.2 mg per liter, so that 6 mg of sodium for 60 ml of test solution and 12 g of quartz was the minimum amount used. The active solution was stored in a Saftepak bottle. Procedure for Adsorption Tests: The method consisted of agitating 12 g of quartz with 60 ml of solution of known sodium concentration for enough time to establish equilibrium between the solution and the quartz surface. The quartz was separated as completely as possible from the solution by filtering and centrifuging. The activity on the quartz and in the equilibrium solution was measured and the partition of the sodium was calculated from the resulting data. The detailed procedure for the adsorption test is set forth in a thesis by Laxen." In brief, it included the following steps: 1—Ascertainment of linearity between concentration of Na" and activity measured. 2—Evaluation of factor to translate activity on solid of infinite thickness in terms of activity on an evaporated active film of minute thickness, on the various shelves of the counter shield. 3—Taking precautions to avoid evaporation of water during centrifuging

Jan 1, 1953

COMMITTEE IN CHARGE SPENCER PENROSE, Chairman A. E. CARLTON, Chairman Finance Committee GEORGE M. TAYLOR, Vice-Chairman J. DAWSON HAWKINS, Secretary DENVER Arrangement DAVE G. MILLER FRANK BULKLEY GEO. E. COLLINS Entertainment F. H. BOSTWICK F. E. SHEPARD HOWLAND BANCROFT B. P. MORSE J. G. PERRY Finance T. B. STEARNS RICHARD A. PARKER T. B. BURBRIDGE

Jan 7, 1918