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Jan 6, 1915

By Edward J. Felten

Binary Cr-A1 alloys containing from 2.5 to 30 wt pct Al and 0.7 wt pct Y were heated in oxygen, air, and nitrogen between 1000" and 1200°C. The reacLivity of the alloys was found to be dependent both on the alloy composition nnd the nature of t he atmosphere. In oxygen, nllojs containing up to 15 to 20 wt pct A1 reacted to produce an external scale of Crz03 and a subscale consisting Predominently of Al203. Alloys contazning 20 to 30 wt pct A1 react in oxygen to produce an A1203 external scale and little m no subscale. The latter alloys were markedly more oxidation resistant than those of low alurninum content. In air, the alloys on which an external Crz03 scale was formed were found to be permeable to nitrogen ns evidenced by the copious amomts of chromium and aluminum nilrides observed ns part of the subscale. The reactizities in nir (or nitrogen) of these alloys increase <m their aluminurn contents increase. However, alloys on which Al,O, us an external scale is formed were nol culnerable to nccelerated attack in air, and no eltldence of nitvide subscnles were observed. For all alloys, yttrium serwed pYimarily to improve oxide adhrence. THE role of chromium in the oxidation resistance of Fe-Cr alloys &apos;-&apos; and that of aluminum in Fe-Cr-A1 al10s&apos; has received considerable attention in recent years. This is understandable since many of these alloys have excellent oxidation resistance due to the formation of either a Cr203 or a-Ala03 film between the metal and the oxidizing atmosphere. Small additions of yttrium or other rare earth metals are effective in preventing spalling of the protective oxide from the metal substrate."" In contrast, little is known regarding the oxidation resistance of Cr-A1 alloys, although some work has been done by Tumarov et a1.&apos; The poor niechanical properties exhibited by Cr-A1 alloys make them undesirable for use as structural components, but their use as coatings cannot be disregarded. The use of chromium-rich aluminide coatings for refractory metal alloys is an example of the potential use of this type of sytem. The purpose of this work is to examine the oxidation behavior of Cr-A1 alloys containing 2.5 to 30 wt pct A1 and 0.7 wt pct Y. The effects of temperature, atmosphere, and thermal cycling have been determined. EXPERIMENTAL PROCEDURE The alloys used in this investigation can be divided into two groups. Those containing 2.5, 5, 7.5, and 10 wt pct A1 and 0.7 wt pct Y were extensively evaluated in the temperature range from 1000" to 1200°C. Alloys containing 15, 20, 25, and 30 wt pct A1 and 0.7 wt pct Y were tested only at 1200°C. All of the alloys were prepared by standard arc-melting techniques in the form of cylinders approximately 4 in. long and 19 in. in diam. Wafers were cut from the cylinders and subsequently subdivided into rectangular coupons. The alloys were brittle and therefore some cracks were found in almost all specimens. The coupons were prepared for oxidation by mechanically polishing through 600 grit Sic paper, and were thoroughly degreased just prior to testing. Two types of oxidation experiments were conducted, namely; cyclic tests in which the specimens were examined and weighed after each 2 hr exposure, and continuous thermal balance tests run in a controlled atmosphere (oxygen, air, or nitrogen) for 20 hr. In the former test the spalled oxide was not included when the specimens were weighed. The physical condition of a specimen was noted visually after each cycle and testing was continued either to failure or until the performance of the specimen was well characterized. Both Micro and Semi-Micro Thermal Balances (Ains-worth) were used in the continuous tests. The oxidized specimens were sectioned and prepared for metal log raphic examination. The specimens were polished through 600 grit Sic paper. After polishing through 6 and l p diamond, a final mechanical polish with Linde B-Alz03 was used. Specimens containing 2.5 pct A1 were etched electrolytically using a 10 pct oxalic acid solution at 4 v for about 2 sec. Selected specimens were examined in the electron microprobe analyzer. Oxide specimens were examined by standard X-ray diffraction techniques. EXPERIMENTAL RESULTS For convenience, the test results have been broken down according to the exposure temperature, and further subdivided according to the type of test and atmosphere employed. Because of the poor quality of the specimens a larger than normal amount of scatter was observed in the measured rate constants. Also, the evaluation of the weight gain data was done on a somewhat arbitrary basis and may not be truly representative. However, the results obtained do show a significant trend in behavior regarding both alloy composition and the nature of the oxidizing atmosphere. I) Oxidation Behavior at 1000°C. A) Continuous Oxidation estsin Oxygen. This series of experiments was run in the Ainsworth Micro-Thermal Balance using pure oxygen at a pressure of 76 mm Hg. Under these conditions all specimens oxidized in accordance with the parabolic rate law over a major portion of the exposure time; the rate constants appear in Table I. The oxide formed externally on all specimens was predominantly Cr,O,, which was generally adherent. In some cases a slight amount of spalling in the form of a fine powder was noted. a-A1203 was observed as a subscale, along with Yz03 in all alloys. Alloys containing up to 7.5 wt pct A1 oxidize more rapidly than the Cr-0.7Y alloy.

Jan 1, 1970

Page Laboratory Methods...........................127 Special Analytical Methods.......................127 Improvements in the Accuracy of the Vacuum-fusion Method for the Determination of Oxygen in Steel....................127 Quantitative Spectrochemical Analysis of Mixtures of Gases.......131 Oxygen Samples from Open-hearth Bath...............133 Rapid Analysis of Sample for Alumina.................139 Accurate Carbon Analyses in Low-carbon Steel.............139 Laboratory Technique for Study of Reactions Involving Liquid Metal. . . . 142 Rotating Liquid Crucibles......................143 Stationary Crucibles.........................145 Jones and Laughlin Experimental Furnace...............148 Vacuum Melting..........................149 Measurement of Temperature of Liquid Iron and Steel;..........149 Pouring and Teeming Temperatures..................149 Bath Temperatures.........................151 Plant Methods.............................154 Methods of Studying Slags.......................154 Sampling Slag in the Open Hearth..................155 Viscosity of Open-hearth Slags....................155 Petrographic Examination of Slag...................156 Statistical Methods Applied to Study and Control of Chemical Relations in Bath...............................166 Rapid Method of -Correlation Applicable to Study of Steelmaking Reactions............................166 INTRODUCTION On Thursday morning, Feb. 16, 1939, a round table discussion was held on the subject of Experimental Methods in the Study of Steelmaking. Dr. John Chipman, Professor of Metallurgy at the Massachusetts Institute of Technology, and chairman of the A.I.M.E. Committee on Physical Chemistry of Steelmaking, presided. In opening the meeting, the chairman said: "The purpose of this round table is to discuss methods of study by which more and better information on the fundamentals of steelmaking can be obtained. It was thought that a round table discussion rather than a symposium would furnish the best opportunity for those actually using various methods of study to get together and discuss their common problems. For this reason attention will be focused upon methods of study rather than upon their results. We want new and current and up-to-date discussion.

Jan 1, 1940

Page Laboratory Methods...........................127 Special Analytical Methods.......................127 Improvements in the Accuracy of the Vacuum-fusion Method for the Determination of Oxygen in Steel....................127 Quantitative Spectrochemical Analysis of Mixtures of Gases.......131 Oxygen Samples from Open-hearth Bath...............133 Rapid Analysis of Sample for Alumina.................139 Accurate Carbon Analyses in Low-carbon Steel.............139 Laboratory Technique for Study of Reactions Involving Liquid Metal. . . . 142 Rotating Liquid Crucibles......................143 Stationary Crucibles.........................145 Jones and Laughlin Experimental Furnace...............148 Vacuum Melting..........................149 Measurement of Temperature of Liquid Iron and Steel;..........149 Pouring and Teeming Temperatures..................149 Bath Temperatures.........................151 Plant Methods.............................154 Methods of Studying Slags.......................154 Sampling Slag in the Open Hearth..................155 Viscosity of Open-hearth Slags....................155 Petrographic Examination of Slag...................156 Statistical Methods Applied to Study and Control of Chemical Relations in Bath...............................166 Rapid Method of -Correlation Applicable to Study of Steelmaking Reactions............................166 INTRODUCTION On Thursday morning, Feb. 16, 1939, a round table discussion was held on the subject of Experimental Methods in the Study of Steelmaking. Dr. John Chipman, Professor of Metallurgy at the Massachusetts Institute of Technology, and chairman of the A.I.M.E. Committee on Physical Chemistry of Steelmaking, presided. In opening the meeting, the chairman said: "The purpose of this round table is to discuss methods of study by which more and better information on the fundamentals of steelmaking can be obtained. It was thought that a round table discussion rather than a symposium would furnish the best opportunity for those actually using various methods of study to get together and discuss their common problems. For this reason attention will be focused upon methods of study rather than upon their results. We want new and current and up-to-date discussion.

Jan 1, 1940

By A. E. Wheeler, H. Y. Eagle

The copper industry in the Province of Katanga, in the Belgian Congo, which is now controlled and operated by the Union Minére du Haut Katanga, had its inception many years ago in the vision of a Scotsman, Robert Williams, now Sir Robert Williams, Baronet. He it was who personally negotiated the mineral concession with King Leopold of Belgium, sent in the prospecting parties who located most of the present mines of the company, later arranged for the Belgian participation from which the present company was formed, and has been its active mentor ever since. The idea back of his efforts was the establishment of an industry on the Congo-Zambezi divide, of sufficient importance to draw up to it the head of the Cape to Cairo Railroad, the dream of Sir Cecil Rhodes, and the consummation of which he had left as a legacy to Mr. Williams, his successor. The reports of the prospecting expeditions showed that copper in profitable quantity was there, but many difficulties lay in the way of the establishment of the infant industry. The isolated location of the mines, various tribal wars, the Boer War, and many other factors contributed to making progress very slow. However, in spite of these difficulties the railroad was finally built and a blast-furnace plant erected at Lubumbashi, near Elisabethville, the capital of the Province. Operations of this plant were started in 1911, treating high-grade oxidized ores and producing pig copper by a reducing smelting. Production has been continuous since that time and the company has grown so that at present it ranks as the largest individual copper producer in the industry. It is a fitting monument to the foresight, optimism and driving force of its founder, and the progressive policies of his Belgian colleagues. In January, 1914, the Union Miniere du Haut Katanga engaged as its consulting engineer, Archer E. Wheeler, metallurgical engineer, at that time general superintendent of the Great Falls plant of the Anaconda Copper Mining Co. Mr. Wheeler was commissioned by the Board of Directors to proceed into Katanga, and make all necessary investigations to enable him to report on a comprehensive development program, and to recommend a scheme of treatment particularly for their low grade

Jan 1, 1934

By J. R. Long, R. S. Dean, F. S. Wartman, E. T. Hayes

The production of titanium in I5-lb. lots and with a purity sufficient to be consolidated into ductile metal, as described in a previous paper,&apos; has provided adequate material for a study of the physical properties of titanium and a more thorough examination of its working qualities. Data on the physical properties reported in that paper were obtained on metal fabricated by a fixed procedure, standardized for the purpose of control of the reduction, and are representative only of material fabricated under those conditions. There are many possible variables in the working schedule, which will have significant effects on the properties of the finished material; and since the previous working methods were not necessarily the best, an investigation of the fabrication of titanium by other methods was undertaken. In this work the consolidation of the powder by pressing and sintering was conducted essentially as outlined in the report cited&apos; and all efforts were centered on fabrication methods for those powders and the proper- ties produced by them. Hardness, density, microstructure, and tensile properties were determined at various stages in the working and annealing; and resistivity measurements were made on a few bars and drawn wire. Consolidation of the PowdeR The screen analysis of the available titanium powder is given in Table I. No attempt was made to alter the size distribution from that noted because this powder, although coarse by normal powder-metallurgy standards, produced acceptable compacts suitable for the present work. Because of their large specific surface, finer powders are more contaminated by oxygen and produce harder compacts, which are difficult to work. The powder as produced is soft, compresses in a normal fashion, and exhibits very little tendency to adhere to the die surfaces. Unlike aluminum and magnesium powders, it can be readily pressed without the use of die lubricants. When compacted at 50 tons per

Jan 1, 1946

By J. R. Long, E. T. Hayes, R. S. Dean, F. S. Wartman

The production of titanium in I5-lb. lots and with a purity sufficient to be consolidated into ductile metal, as described in a previous paper,&apos; has provided adequate material for a study of the physical properties of titanium and a more thorough examination of its working qualities. Data on the physical properties reported in that paper were obtained on metal fabricated by a fixed procedure, standardized for the purpose of control of the reduction, and are representative only of material fabricated under those conditions. There are many possible variables in the working schedule, which will have significant effects on the properties of the finished material; and since the previous working methods were not necessarily the best, an investigation of the fabrication of titanium by other methods was undertaken. In this work the consolidation of the powder by pressing and sintering was conducted essentially as outlined in the report cited&apos; and all efforts were centered on fabrication methods for those powders and the proper- ties produced by them. Hardness, density, microstructure, and tensile properties were determined at various stages in the working and annealing; and resistivity measurements were made on a few bars and drawn wire. Consolidation of the PowdeR The screen analysis of the available titanium powder is given in Table I. No attempt was made to alter the size distribution from that noted because this powder, although coarse by normal powder-metallurgy standards, produced acceptable compacts suitable for the present work. Because of their large specific surface, finer powders are more contaminated by oxygen and produce harder compacts, which are difficult to work. The powder as produced is soft, compresses in a normal fashion, and exhibits very little tendency to adhere to the die surfaces. Unlike aluminum and magnesium powders, it can be readily pressed without the use of die lubricants. When compacted at 50 tons per

Jan 1, 1946

By Thomas Read

PERSONNEL work is a term recently introduced to cover the great variety of activities in industrial work that deal with the human factor. Much attention has been focussed upon individual phases of personnel work, such as accident prevention, sanitation, "welfare" work, reducing labor&apos; turnover, and so on. In most cases these activities have been carried on as though they were distinct and separate fields; as a matter of fact, they are only different phases of the single problem of human engineering, and each has important and fundamental relations with the others. Thus, for example, high labor turnover is one of the most .important causes of a high accident rate, and unsatisfactory housing conditions are an important cause of labor turnover. In the early stages of the study of these problems, it was necessary to take them up separately; the time has now arrived at which it is desirable to consider them as a whole in order to bring them into the right relation to each other. When thus considered as phases of an interrelated whole, they may be grouped as personnel work. A discussion of the importance of personnel work as a means of in creasing dividends in industry may be objected to by some as a too materialistic way of looking upon work that is humanitarian. Nothing could he more mistaken than such an opinion. Humanitarianism, per se, has no place in industry, and nothing is gained and much is lost in pre tending that it has. The only reason why a corporation engages in business is to make profits, and any activity of the corporation that does not tend either directly or indirectly toward that end is poor business. It is equally poor business to overlook any activities that do tend indirectly to the making of profits. On this basis, personnel work can be justified as a corporate activity; there is no justification whatever for abstract humanitarianism from the business standpoint. One characteristic of the American workman is a general high level of intelligence, and it is an insult to intelligence to ask a man to believe that anything so impersonal as a corporation is really desirous of benefiting

Jan 10, 1917

By Roswell H. Johnson

The principle of sliding or graduation in royalties is accomplished either by the block, period, cumulative, or class method. The block method calls for a very low royalty rate on all oil produced up to a certain amount. This amount would normally be that which is believed to suffice to repay the cost of the well. A higher rate would be charged after the well is making a profit. This method, common in many industries, is peculiarly inadaptable to any industry such as this where the productivity per day of the units gradually and inevitably decreases. This, for reasons given later, is because it forces an early abandonment of the well and so offends against conservation. In the period method, the royalty rate is changed by some definite amount when the well produces less than a specified quantity per day or other given unit of time. While simple to explain, it operates badly because a great deal is made to depend upon a small reduction in production, whereas the reduction as a matter of fact declines rather erratically owing to the exigency of lease management, connecting of tankage, and vagaries of the gaugers. These disadvantages are obviated by the cumulative method. In this method, all the production less than a certain amount per week has one rate of royalty, or none at all, and the oil produced in excess of that amount pays an additional rate of royalty. In the long run the calculation is probably no greater than with the period method, for simple tables will be published and printed in the oil papers that can be cut out, enabling quick readings to be made. Even without the table the calculation is easy with the few royalty rates, two or three, which would be used. In this method, the amount paid in royalty declines gradually, rather than suddenly as in the period method. The following reasons might be advanced for the adoption oi cumulative royalties: 1. To distribute the burden in accordance with the capacity to pay. This principle is a unique one in business, although familiar in taxation. This is because it does not distribute reward in proportion to efficiency.

Jan 1, 1916

By P. D. Frost, H. A. Robinson, J. R. Doig, M. W. Mote

The mechanism of hardening in heat-treatable zirconium alloys was foUNd to be analogous to that for titanium alloys. Zirconium containing a relatively large addition of a ß -stabilizing element such as molybdenum or columbium can be hardened by the following transformation: Lean alloys, having insufficient alloy content to retain ß at room temperature are hardened by the following transformation: Application of these findings in Zr-Mo-Sn and Zr-Nb-Sn alloys produced strengths as high as 190,000 psi with reasonable ductility. PRIOR research on zirconium alloys has been concerned with development of greater strengths and creep resistance by solid-solution hardening or by dispersion hardening. Although solution and aging heat treatments had been applied earlier to zirconium alloys, quenching frequently produced low ductility. The possibility that the ß-to-w transformation, discovered earlier in titanium alloys,&apos; might also occur in zirconium alloys and cause low ductility was considered, and, indeed, was found as predicted2 to be the case. In the earliest experiments, the heat-treatment response of titanium, too, was disappointing. However, by avoiding the formation of the embrittling w phase, it became practical to obtain room-temperature strengths higher than 180,000 psi, with elongation values of 10 pct.3 Based on the present concept of titanium heat treatment, the principal requirement for a heat-treatable zirconium alloy is that it contains a certain minimum amount of one or more ß -stabilizing elements. Only molybdenum, columbium, and tantalum, when present in sufficient amounts, are known to stabilize ß zirconium to room temperature during rapid cooling from the ß field. Tantalum was undesirable because of its high thermal-neutron cross section. Aluminum and tin are effective a stabilizers, but aluminum has been shown to seriously decrease the corrosion resistance of simple zirconium alloys in hot water. Therefore, for the present study, tin was used as the stabilizer addition. The alloys selected for this evaluation are presented in Table 1 along with their analyses and ß-transus temperatures. The analyses indicated that intended compositions were usually realized. EXPERIMENTAL PROCEDURES All of the alloys were melted from sponge zirconium and fabricated to sheet for heat treatment

Jan 1, 1960

By Allan T. Gwathmey, J. Bruce Wagner, Kenneth R. Lawless

Between 250°and 550°C in oxygen pressures of 10 to 760 mm Hg, the relative oxide thicknesses formed per unit time on the (100), (111), (110), and (320), decreased in this order. The predominant oxide orientation was (001)Fe3O4 and [110] Fe304 A small amount of a-Fe2O3 which exhibited a fiber pattern was observed in all oxides except those formed at 250°c in low oxygen pressures. IN order to understand the properties and behavior of thin films, particularly their role in oxidation reactions, there is needed more experimental information on their structure, composition, and kinetics of formation on clean surfaces of known geometry. The present study was undertaken to obtain such information for thin oxide films formed on single crystals of a body centered cubic metal, iron. Crystals in the form of spheres were used in order to expose all possible crystal planes to the reactant gases simultaneously. Using this procedure the relative rates of oxidation of all planes could be estimated, and those exhibiting, maximum or minimum oxidation rates could be selected for a more intensive study of composition and expitaxy. Since the three types of information were obtained from the same experiment using a single crystal substrate, any differences between rate, composition, and expitaxy on the several planes may be attributed to the influence of the substrate structure. EXPERIMENTAL The starting material for this study was Armco iron rods, 6 in. long and 3/8 or 1/2 in. in diam. The analysis was reported to be 99.8 pct Fe, with major impurities listed as carbon 0.018 pct, manganese 0.027 pct, phosphorous 0.005 pct, sulfur 0.029 pct, silicon 0.005 pct, and copper 0.11 pct. These rods were cleaned with ether and heated in an atmosphere of moist hydrogen at 950°C for three days. The purpose of this treatment was to decarburize the iron and to provide a consistent, uniform grain size for the growth of single crystals. Crystals in the form of rods, up to 1/2 in. in diam and 2 in. long, were prepared by a method similar to that reported by Leidheiser and Buck.2 Spherical crystals, 3/8 and 1/2 in. in diam and having a handle about 1/4 in. in diam by 112 in. long, were machined from the single-crystal rods. After machining, each crystal was etched in aqueous nitric acid to remove the cold-worked metal at the surface. Before each experiment, the crystal was polished mechanically with metallographic papers through number 4/0, and electropolished in a perchloric acid-acetic anhydride mixture by the method of Jacquet and Rocquet.3 The crystal was washed in running distilled water for at least 5 min. The excess water was blotted with a soft paper tissue, and the crystal was placed in an all-glass reaction vessel (See Fig. 1). The crystal was heated at 550°C in hydrogen for at least 8 hr prior to the oxidation in order to reduce any surface oxides and to help relieve any stresses in the metal. For the structure and composition studies, flat faces were cut parallel to (loo), (111), and (110) planes on the iron crystal spheres. The orientation of these faces was checked by a back-reflection X-ray diffraction technique. The faces were within 2 deg of the desired orientation. The flat faces were treated as described above except that prior to electropolishing they were given an additional polish on metallographic felt saturated with twenty-minute levigated alumina. After the crystal was heated in hydrogen for at least 8 hr, the temperature was adjusted to the desired value, and the hydrogen was evacuated. Commercial oxygen which had been purified by successively passing through tubes containing magnesium perchlorate, Ascarite and magnesium perchlorate was admitted to the desired pressure as measured by a mercury manometer. A resistance-wound furnace surrounded the oxidation chamber, and a temperature controller maintained the temperature within ±3°C. The furnace was provided with a small window for observing the crystal. The changes in thickness of the oxide films were followed by observing the interference colors. The oxidation was allowed to proceed until the desired oxide thickness was attained on a given crystal plane. The experiment was terminated by evacuating the oxidation

Jan 1, 1962

By Bradley Stoughton

[Secretary&apos;s Note.—TO avoid repetition of foot-notes, references to authorities are made in this paper by means of figures, referring to a numbered list in the appendix.—J. S. 1 Introduction. This paper gives the results: first,, of a research into the somewhat extensive literature of titanium; and second, of a series of original tests upon the effect of titanium on iron castr ings. New investigations have also been made upon the effect of titanium on steel, but I hope to treat this subject in an independent paper at some later date, and, therefore, will not discuss the experiments in detail here. The combined results of this study, which extended over a period of more than two years, can be briefly summarized as follows : 1. Steel or cast-iron, in which the titanium is properly proportioned, and which has been properly treated, is improved in strength, toughness, and durability against wear, such &apos;as, for example, the wear of railroad-rails, of steel and chilled-iron rolls, car-wheels, etc. 2. These improvemerits seem to be caused, not so much by the direct effect of titanium on the metal, as by its cleansing influence in removing harmful impurities, such as oxygen and oxides, nitrogen, occluded slags, and perhaps also sulphur. It appears also to reduce segregation, which would contribute to the same end. 3. In order that its effects may be fully realized, the treatment of steel or iron with titanium must be correctly performed. There are a few simple, but essential, details to be observed; if they are neglected, the best results cannot be expected. To illustrate by an example: A series of tests on cast-iron

Jan 1, 1913

By W. B. Jamison

Man&apos;s material advance from one level of civilization to the next has involved the development of new, more useful tools and the utilization of energy greater than he alone could produce. These two essentials for material progress have developed at an ever increasing rate in the last century. While the first really successful use of mechanical energy derived from burning fuel was in James Watt&apos;s steam engine which pumped water from coal mines in Cornwall about 1770, there was still very little use of mechanical energy in mining by 1900 except for pumping and hoisting. Compressed air, having some of the characteristics of steam and which operated engines not unlike steam engines or steam hammers, powered the first attempts to mine coal with energy greater than human muscle could provide. When direct current-powered traction cars replaced horse-drawn transportation cars on city streets, it was natural that direct current locomotives should begin to replace animal and human power in mine haulage. Slowly, trolley and battery locomotives were developed and introduced. With d-c systems being established for haulage, it was natural that improved cutting machines should be developed and powered by d-c motors. Thus began the years of

Jan 1, 1961

By J. S. Kirkaldy, D. G. Fedak

The extra degree of freedonz introduced by a second independetzt concentration in a tenzary system gives rise to the possibility of unstable planar phase interfaces in semi-infinite diffision layer couples. Diffusion paths which pass continuously in and out of too-phase regions of the phase diagram but which are not coincident with tie-lines give rise to super saturated zones which may be either adjacent to or isolated from planar phase interfaces, with corresponding nonisolated or isolated precipitates. Nonisolated precipitates are equivalent to morphological development of the interface. Selected couples in the ternary systems Fe-Ni-Cr and Cu-Zn-Sn have been examined nzetallographically and ifz the latter case both isolated and uo~zisolated precipitates have been observed. The diffusion path in one of the couples showing interface morphological developtnent has been examitled using electron probe microanalysis. IGNORING the spurious effects of preferential grain boundary diffusion and anisotropic crystal growth7 it can be unequivocally stated that it is impossible for a binary isothermal diffusion couple constructed of two unsaturated phases to sustain a nonplanar phase interface. Consider for demonstrative purposes the schematic phase diagram of Fig. l(a). Given an initial flat phase interface, semi-infinite boundary conditions and the internal boundary condition fixed by the constitution diagram, xB = xB(T), the unique solution of the diffusion equation requires a persistent flat interface. No other solution is possible. If, however, we anticipate the involvement of surface tension, then the internal boundary condition must be written xB = xB (T,Y) where r is the radius of curvature of a hypothetical nonplanar interface. The introduction of a new parameter such as r can be equivalent to the release of an internal constraint, so that a stable nonplanar interface may be possible after all. Consider a perturbation to the interface as indicated in Fig. 1(b). According to the Ostwald-Freundlich equation: which is applicable to a system of this constitution, the solubility of A in the matrix ß ,xB (Y), at a point of curvature r is given by where Va is the molar volume of the a-phase, R is the gas constant, and a is the interfacial tension. Since the right hand side is positive, xB(r) >xB cm, as indicated in Figs. 1(a) and 1(c). Accordingly, the perturbation will carry the interface concentration in a direction which is opposite to that which would sustain local equilibrium. Such a perturbation is necessarily moderated and the system is returned to its initial condition. This result is general for all binary couples since we can regard an interfacial perturbation as an attempt to precipitate within un-

Jan 1, 1962

By A. C. Watts

FOR several years, a mine in Colorado experienced considerable trouble from small fires caused by the blasting of coal. Although a well-known make of permissible powder was used, it was first thought that the powder ignited gas that might be present and that this, in turn, set fire to line brattices or to the coal. Experiments were, therefore, conducted with another make of powder, but the results convinced the superintendent of the mine, Robt. Williams, Jr., that the fires were not caused by the powder but by the high-voltage electric current used for detonating the shots. The mine "makes" gas very freely, giving off from three-fourths to a million cubic feet of methane per 24 hours. The coal is a good grade bituminous of a very free burning quality. Electric shot-firing from the outside after all men and animals were outside had been practiced for a number of years. The shooting circuit was connected with the main power circuit at the mouth of each entry. Shooting circuit switches were mounted in boxes, which were kept locked with the handle of the switch, in open position, showing through the bottom of the box. The door of the box could not be shut and locked when the shooting switch was closed. At the entrance to each room, or working place, a small switch, called the miner&apos;s switch, was placed on the shooting line. It was the duty of the miner, when entering his place at the beginning of the shift, to see that this switch was open and that it was kept open until he left the place at the end of the shift to go out of the mine. Grounded return was used for main power lines. The current was 500 volts, direct current, with 100 to 300 amp. The nearest working face was 9600 ft. from the shot-firers&apos; switch outside the mine and the most remote working face was 2 ½ miles. The various working faces were scattered over a wide area between these two points.

Jan 9, 1925

By J. L. Rodda, R. L. Wilcox, E. C. Truesdale

In recent years various problems in connection with research work on the preparation and properties of zinc-base alloys have required reliable information concerning the constitution of the zinc-rich portion of the iron-zinc equilibrium diagram. On numerous occasions rather positive indications were obtained that, for example, the solubility of iron in zinc was incorrectly represented on the current equilibrium diagrams. A careful study of all the available literature relating to the iron-zinc system led to the conclusion that much of the early work was unsatisfactory as measured by present standards of experimental accuracy, and as a result it was decided to redetermine the location of the liquidus curve and of adjacent portions of the diagram. Part I of this paper comprises a description of the experimental methods and a summary of the results by means of which the zinc-rich end of- the iron-zinc diagram has been revised in the following ways: 1. Measurements of the solubility of iron in liquid zinc by several different sampling methods, leading to a relocation of the liquidus curve. 2. Microscopic, conductivity, and X-ray studies of the solid solubility of iron in zinc, which, together with thermal analyses, have resulted in new values for the solid solubility and the eutectic temperature and composition. 3. Heating and cooling curves, obtained by a refined differential method, leading to new locations for the two peritectic horizontals. In Part I1 of the paper the attempt is made to review all of the published work having a bearing on the constitution of the iron-zinc system, and to correlate the present results, and some recently published data involving the use of X-ray technique, with the earlier work, much of which was done from 25 to 30 years ago.

Jan 1, 1936

By P. L. Russell

The use of nuclear explosives for excavation has been demonstrated to be feasible and practical. Application of nuclear explosives for overburden removal from large ore deposits appears to offer economic advantages over present methods, but under the present pricing schedule, high-yield devices must be used to obtain an economic advantage. The use of nuclear explosives presents problems not inherent in the use of conventional explosives, and thus they can be used only in areas where large explosions and associated phenomena can be tolerated. Stripping of coal with nuclear explosives does not appear practical at this time, but stripping overburden from copper or iron ore deposits may be a potential use. Even here, however, the use of nuclear explosives would require isolation, favorable topography, favorable ground-water conditions, and a low population density. If these basic requirements can be met, the use of nuclear explosives for overburden removal would offer both economic and time advantages. The possibility of using nuclear explosives for peaceful purposes was a subject for speculation as early as 1945. The PLOWSHARE Program was formally established by the AEC in June 1957 for the purpose of developing and demonstrating peaceful applications for nuclear explosives. The technical direction of the program is the responsibility of the Lawrence Radiation Laboratory, Livermore, Calif. Mining and excavation were two fields that received early consideration as areas in which nuclear explosives might be used. Knowledge gained from underground weapons testing increased this possibility, and the development of the thermonuclear device which has a small fission-to-fission ratio, reduced the hazard of radiation, and spurred interest. Nuclear explosives appear to have the greatest potential in the following mining operations: 1.— Surface Mining a) Stripping of waste for open-pit excavation b) Breaking of ore in open-pit mining c) Quarrying d) Blasting for production of aggregate, riprap, etc. 2. — Underground Mining a) Block caving application b) Crushing of ore for in-situ leaching, etc. c) Preparation of underground waste disposal areas Of the potential applications, excavation is perhaps the most obvious and the best understood, and probably the most practical for use in the near future. Large quantities of rock and earth can be moved by proper emplacement of nuclear explosives, but economic and practical relationship must be determined between the known capabilities of nuclear explosives and the required excavating to remove overburden. REMOVING OVERBURDEN IN OPEN-PIT MINING Removing the overburden is one of the largest jobs in open-pit mining. In 1960 open-pit mines produced approximately 130 million tons of coal, 108 million tons of copper ore, and 135 million tons of iron ore. To obtain this much production, an estimated 3-billion tons of overburden were removed from the coal, 216 million tons from the copper ore, and 135 million tons from the iron ore. These figures do not include the initial stripping required before ore production. For example, the ASARCO Mission mine started stripping operations in August 1959 and by mid-November 1961 had removed 46.3 million tons of material including 1.2 million tons of ore.* Initial excavation of this type offers the most favorable conditions for utilizing the earth-moving ability of nuclear explosives. EXPLOSIVE CASTING FOR REMOVING OVERBURDEN The use of explosives to remove overburden is not a new idea. Conventional explosives have been used for this purpose for many years with varying degrees of success. Several small coal strip operators have used this idea to increase production. At these mines about one-third or more of the overburden is thrown by explosives across the pit and onto spoil piles. The additional costs of drilling more blast holes and more explosives are more than compensated for by a reduction in the time required to uncover the coal, and by an increase in coal production.

Jan 1, 1964

By C. G. Dunn

Many investigations have been made concerning the nature of plastic deformation and recrystallization of metals either in the form of polycrystalline materials or in the form of single crystals. However, similar work on strip materials composed of large grains as thick as the strip and having a high degree of preferred crystal oricntation has not been carried out extensively. Such materials are ideal not only for studying changes in single crystals under conditions where neighboring grains exert their influences but also for obtaining the complete change in orientation of a grain or group of grains during the course of plastic deformation and subsequent recrystallization. It is well known that first-order twins in the form of Neumann bands may be produced during the plastic deformation of ferrite crystals, particularly silicon ferrite crystals.l--3 Furthermore, it is believed that high-stress regions exist in the vicinity of these bands4. and it has been said that these banded regions would be active in recrystallization processes.5 Evidence to that effect in silicon ferrite had already been presented with photomicrographs showing recrystallization among Neumann bands during the early stages of recrystallizati~n.5,6 Similar evidence has been published for nonferrous metals5 Merging of fine parallel deformation bands during annealing to form twin bands of ordinary appearance in alpha brass has been offered not only as evidence of an active role being played by mechanical twins but also as evidence that such twins cxisted prior to recrystalli~ation.5 Proof that such new structures are actually first-order twins, or even twins at all, must be considered inadequate except for those cases where X-ray or optical data have been obtained to confirm the necessary oricntation relationship.7,8 A. B. Greninger has obtained excellent iliustrations of annealing twins in alpha iron.9 Since his material was previously deformed by sharp hammering, a process that generally induces Neumann bands, the existence of twins following annealing might suggest that they grew from mechanical twins. In connection with transformation twins in alpha iron, Greninger reported that grains containing three twin orientations occurred rarely and none occurred with three sets of well-developed bands.9 The work at the Pittsfield Works Laboratory on silicon ferrite in the form of large-grained strip steel deformed a small amount and annealed to partially recrystallize the grains indicates that the deformation and recrystallization processes that lead to annealing twins involvc more complex processes than the formation of Neumann bands and the growth of such bands. Some groups of annealing twins are obtained which contain not only three well-developed twin structures, but also contain more than one order of twins. It is also shown, in one case, that an interrelated group of twins did not arise within one single parent grain and, furthermore, orientations of grains in the group

Jan 1, 1944

By C. G. Dunn

Many investigations have been made concerning the nature of plastic deformation and recrystallization of metals either in the form of polycrystalline materials or in the form of single crystals. However, similar work on strip materials composed of large grains as thick as the strip and having a high degree of preferred crystal oricntation has not been carried out extensively. Such materials are ideal not only for studying changes in single crystals under conditions where neighboring grains exert their influences but also for obtaining the complete change in orientation of a grain or group of grains during the course of plastic deformation and subsequent recrystallization. It is well known that first-order twins in the form of Neumann bands may be produced during the plastic deformation of ferrite crystals, particularly silicon ferrite crystals.l--3 Furthermore, it is believed that high-stress regions exist in the vicinity of these bands4. and it has been said that these banded regions would be active in recrystallization processes.5 Evidence to that effect in silicon ferrite had already been presented with photomicrographs showing recrystallization among Neumann bands during the early stages of recrystallizati~n.5,6 Similar evidence has been published for nonferrous metals5 Merging of fine parallel deformation bands during annealing to form twin bands of ordinary appearance in alpha brass has been offered not only as evidence of an active role being played by mechanical twins but also as evidence that such twins cxisted prior to recrystalli~ation.5 Proof that such new structures are actually first-order twins, or even twins at all, must be considered inadequate except for those cases where X-ray or optical data have been obtained to confirm the necessary oricntation relationship.7,8 A. B. Greninger has obtained excellent iliustrations of annealing twins in alpha iron.9 Since his material was previously deformed by sharp hammering, a process that generally induces Neumann bands, the existence of twins following annealing might suggest that they grew from mechanical twins. In connection with transformation twins in alpha iron, Greninger reported that grains containing three twin orientations occurred rarely and none occurred with three sets of well-developed bands.9 The work at the Pittsfield Works Laboratory on silicon ferrite in the form of large-grained strip steel deformed a small amount and annealed to partially recrystallize the grains indicates that the deformation and recrystallization processes that lead to annealing twins involvc more complex processes than the formation of Neumann bands and the growth of such bands. Some groups of annealing twins are obtained which contain not only three well-developed twin structures, but also contain more than one order of twins. It is also shown, in one case, that an interrelated group of twins did not arise within one single parent grain and, furthermore, orientations of grains in the group

Jan 1, 1944

By S. A. Mersol, C. T. Lynch, F. W. Vahldiek

The room-temperature Knoop hardness of single -crystal titanium diboride has been determined. Variations in microhardness have been correlated with orientation and structural imperfections in the crystals. Maximum differences in hardness values of 750 kg per sq mm with respect to orientation and 450 kg per sq mm with respect to substructure were found. The effects of etchants, load on indenter, and degvee of cracking of indentation were studied. The average hardness was determined as 2800 kg per sq mm on the as-grown crystals. Annealing increased the average hardness to 3375 kg per sq mm. ThE microhardness of polycrystalline titanium diboride approximating the stoichiometric composition TiB, has been studied by several investigators. The values for the Knoop hardness number range from 2710 kg per sq mm (Khn = 2710 kg per sq mm) to 3400 kg per sq mm.&apos;-4 Samsonov et al.&apos; reported a Vickers hardness number of 3400 kg per sq mm (Vhn = 3400 kg per sq mm) at 120-g loads for a 98 pct Ti + B material of 96 pct theoretical density. Recently Dunegan measured the Vickers hardness and obtained 2060 kg per sq mm with a 10-g load (Vhnlo = 2060 kg per sq mm), 1425 kg per sq mm for Vhnloo, and 1320 kg per sq mm for Vhnlooo. We have obtained a Khnloo = 3000 * 350 kg per sq mm for hot-pressed polycrystalline TiB2 that was 99.1 pct Ti + B and 96.6 pct of theoretical density. The present investigation has been made on single-crystal titanium diboride boules, and is believed to be the first such study on TiB, crystals of known orientation. EXPERIMENTAL The single crystals were prepared by a Verneuil-type process using an electric arc by the Linde Division of Union Carbide Corp. The largest specimens were 6 mm in diameter by 12 mm long. The crystals were of theoretical density (4.50 g per cm3) with a Ti + B content of 99.8 pct. The major impurities present were: 0.03 pct (by weight) 0, 0.06 pct C, 0.01 pct Si, 0.05 pct Fe, 0.01 pct Cr, and 0.01 pct Ni. The crystals were boron-rich, the average boron content being 31.S7 wt pct (stoichiometric value is 31.12 wt pct), and titanium-poor, the average titanium content being 68.2 wt pct (stoichiometric value is 68.88 wt pct). Titanium was determined gravimetrically by cupferron precipitation and boron by titration of H3B03 from a NaOH-fused specimen after removal of titanium with BaC03. The outer edge of the boule accounted for some of the excess boron. An electron-microprobe analysis showed that the titanium content increased from 60.0 wt pct at the edge to 68.5 wt pct at D, ~ 1000 p, where D, = distance from outer edge (see Fig. 5). X-ray measurements indicate that the boules are single crystals with considerable substructure. Upon etching this structure is seen in the form of a Widmanstatten-type rhombohedral line pattern in the basal (c) plane and a parallel "lines" pattern in the prism (a) planes. A typical WidmanstHtten-type pattern is seen in in Fig. 1. Electron microscopy reveals that the lines are less than 1 p across, which does not allow direct electron probe or microfocus X-ray determination of their composition. The identity of the second phase has not been established. It might be a higher boride or a nonstoichiometric TiB2. On annealing above 2200°C the precipitate is dispersed and dissolves in the matrix. The best etchants found were HF/HNO/HO, KF(CN)$NOH/HO (Murakami&apos;s Etch), and A large number of other etchants were previously Studied. The acidic etchant produced an acicular or "needles" pattern in the (a) planes which is an etchant effect on the "lines" pattern.

Jan 1, 1965