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By T. F. Ford, J. F. Fidiam, A. G. Loomis

It is only within the past 10 years that serious attempt appears to have been made to improve rotary drilling fluids by the application of the principles of colloid chemistry, although the use of chemicals to control the rheological properties of clay slips has long been known in the ceramic industry. The main difficulty apparently lay in the lack of a complete analysis of all of the functions of a drilling fluid in the drilling of the well, together with the lack of adequate consideration of how colloid science could be applied to secure these ends, and particularly how apparent antithetical properties of the fluid could be compromised. Thus one analvsisl of the many requirements of a drilling fluid proved conclusively that the viscosity should be low, in order that cuttings and entrained gas might be eliminated effi-ciently in the settling ditch, while the loss in carrying capacity accompanying low viscosity could be regained by increasing either the density of the mud or the upward velocity of the mud stream in the annular space of the well, and the danger of sticking of the drill stem due to rapid settling in case of enforced suspension of drilling operations could be eliminated by enhancing the thixotropic properties of the fluid. The desired properties of the drilling fluid having thus been established, it was a natural step to treat the fluid with vis-cosity-reducing chemicals, such as salts of weak organic acidsl for example, sodium tannate or gallate—and to adjust the pH to the alkaline side to such a degree of thixo-tropy as would give low viscosity and low yield point under the conditions of flow prevailing in the settling ditch, but rapid gelation and high yield point when quiescent in the annular space during shutdowns. In fact, flow in the settling ditch should be just short of turbulent while flow in the well, together with the flow of mud past the cuttings, is practically always turbulent. The use of chemicals other than those mentioned, such as Calgon (sodium hexametaphosphate) and certain other phosphates together with sodium tannate, has now become standard practice and it is the consensus that this method of treatment has proved to be an important step in the development of the art of drilling oil wells. It is safe to assume that the application of colloid chemical principles can also help in solving other outstanding problems of drilling fluids, such as the development of cheaper and more efficient viscosity reducers ; the development of chemicals that do not lose their effectiveness in a short time during drilling operations; the finding of chemicals to preserve the plastering properties of muds when concentrated brines are encountered or in drilling through salt beds; improvement in the plastering properties of poor muds by further defloc-culation, and, conversely, the prevention of excessive deflocculation of certain marine shales sometimes encountered; the preparation of muds suitable for the successful drilling of heaving shale formations; the finding 0f chemicals to treat the mud to prevent or to diminish lost circulation; the development 0f muds that will not impair 6

Jan 1, 1941

By J. L. Wyatt

THE smelting of ilmenite to produce a slag rich in titanium, with pig-iron as a byproduct, introduces new concepts in electric smelting metallurgy. Titanium slags are characterized by low electrical resistance, thereby requiring a different type of electric furnace operation, and power supply sources substantially different from those encountered in normal steel melting and siliceous ore smelting furnaces. This paper describes special apparatus for determining specific electrical resistivity of titanium slags, and reports the values obtained on slags encountered in the process of smelting ilmenite ores. In an induction furnace under conditions approximating normal furnacing operation, 25 general heats and 6 special standardization and comparison heats were run. Results indicate relatively low resistivity. Resistivity depends primarily on slag composition, and, to a lesser degree, on temperature. During the summer of 1947 a cooperative project between the National Lead Co. and the Bureau of Mines was conducted at Boulder City, Nevada, in the Electrometallurgical Laboratories of the Bureau. The project involved smelting of ilmenite ores in electric furnaces, and has been reported in detail.' The author participated as a member of the staff of the National Lead Co. during the entire campaign. One outstanding characteristic of the titaniferous slags, their apparently excellent and variable electrical conductivity, was considered sufficiently important to warrant further study. Although little electric smelting of iron ores has been done in the United States, a certain amount of information is available for comparative purposes. Personal experience in smelting siliceous iron ores in electric furnaces furnished further information for comparison. In general, silicate slags are relatively poor conductors of electricity. Current flow during smelting operations may be maintained through a floating layer of coke on top of the slag bath, or through a bath of molten iron, beneath the slag. Silicate slags are not sufficiently conductive to furnish a path for current passage when normal furnace voltages are used. Experimental smelting of a silicate iron ore was undertaken for comparative purposes. A fluid melt was not obtained until the FeO content was reduced to 15 pct. The resistivity increased as the FeO content decreased, FeO compounds being the most conductive of the various oxides in such a normal slag system. The converse appears to be true in slags containing large percentages of TiO2. It has been found that titanium slags become molten with FeO percentages in excess of 30 pct, and that the conductivity becomes generally better as the FeO con-tent of the slag diminishes. This phenomenon was demonstrated in the furnacing operations at Boulder City. During the initial smelting period furnace electrodes could be held immersed several inches in the slag, with tap selectors set for a no-load voltage of 70 v. As the FeO content decreased, the furnace electrodes would "walk up," until at one point in the process the tips would break the surface and arc on top of the slag. This was undesirable since direct arcing caused losses of important flux additions. The slag compositions under study at that time were such that losses due to surface arcing sometimes caused viscous slags to be formed. Forcing the electrodes into the slag bath by manual control to prevent surface arcing resulted in excessive power input and lack of control. Suitable low voltages were not available. Measurement of the electrical resistivity of titanium slags at various operating temperatures and slag compositions was undertaken. It was believed that this information would be of use in the design of electric furnaces suitable for smelting ilmenite, with voltages, electrode sizes, and electrode spacing adapted specifically to titanium slags.

Jan 1, 1951

Jan 1, 1947

Jan 1, 1947

By E. T. Turkdogan, L. E. Leake

A number of measurements have been made on the vapor pressure of pure iron at 1600°C. Experiments were carried out by the transportation method in which a sample of iron is exposed in a furnace to a stream of pure argon, metered at a predetermined flow rate for a specified period of time. The vapor pressure was obtained from the weight loss of the sample. A detailed diagram of the apparatus used for the experiments is given in Fig. 1. It consisted of a horizontal molybdenum-wire-wound furnace fitted with a recrystallized alumina tube 1 1/8 in. internal diam. The boats, 1 by 3/16 by 1/8 in., were fired in argon at 1600°C to constant weight before use. After this treatment, subsequent heating of the boats to 1600°C gave little or no further change in weight, e.g. ±0.05 mg in 24 hr. The furnace and reaction tube were separately fed with argon from two independent flowmeters. These were connected to a common supply source via an argon purification furnace containing metallic titanium sponge at 700°C, and an anhydrone drying-tower. A rotary displacement-type meter was included in the gas train to provide a direct means of measuring the total volume of gas passed through the reaction tube. The material used was vacuum melted high-purity iron in the form of wire 2mm in diam. The following impurities were present in the iron: 0.008 pct C, 0.002 pct Si, 0.005 pct Mn, 0.008 pct S, 0.001 pct P, 0.01 pct Ni, 0.001 pct Cr, 0.006 pct Cu, and 0.001 pct Al. Samples consisting of three small pieces of this wire were laid end to end in a recrystallized alumina-combustion boat, and were separated by small fragments of alumina. The wire samples were then melted in argon to form spherical beads 2 to 3 mm in diam. After weighing, the boat with its contents was placed on the boat carrier and introduced into the cool end of the reaction tube. The entire furnace system was then flushed with argon for 30 min. At the end of this period, the flow of argon to both furnace and reaction tubes was adjusted to the desired level; then the boat was slid rapidly into the hot-zone of the reaction tube. After a known volume of gas had passed through the reaction tube, the boat was withdrawn quickly to the cool end of the furnace. When quite cool, the boat was removed from the fur-mace and placed in a desiccator for subsequent re-weighing. The semi-micro balance used in these experiments had a sensitivity of 0.005 mg. The above procedure was repeated at several flow rates within the range of 25 to 300 ml per min. The flow of argon in the annular space between the two tubes was at a rate of 300 ml per min in all experiments. During all the experiments the furnace temperature was maintained at 1600° ± 5°C by means of a temperature controller. The temperature of the reaction zone was measured with a Tinsley high precision disappearing filament pyrometer which was initially calibrated against a Pt-13 pct Rh/Pt thermocouple; the errors due to temperature measurements were within * 5°C. RESULTS Assuming that the iron vapor is in the monatomic state, the vapor pressure can be calculated from the weight loss of the sample and the volume of the carrier gas. The results obtained are plotted in Fig. 2 against the rate of flow of argon through the chamber containing liquid iron beads. At low flow rates, the thermal diffusion of iron gives an apparent high vapor pressure, but at high gas flow rates, the carrier gas is not saturated with the vapor, and therefore, low vapor-pressure values are obtained. This is now a well-known phenomenon. There is a distinct inflexion of the curve at about 120 to 160 ml per min rate of argon flow and the vapor pressure of iron within this

Jan 1, 1961

By Strathmore R. B. Cooke, Eugene L. Talbot

THE perfluoro acids and derivatives show unusual surface-active properties that qualify them as possible flotation reagents. They lower the surface tension of water from 15 to 20 dynes below that obtainable with the corresponding hydrocarbon compounds.1, 2 Fluorochemicals adsorb very strongly on solid surfaces to give films that exhibit larger contact angles than films of the corresponding hydrocarbons."' * The large contact angles probably result from the terminal —CF3 group. The perfluoro acids are made by electrolysis of the corresponding carboxylic acid in anhydrous hydrogen fluoride.5 From the perfluoro acids many derivatives may be obtained, such as amides, amines, alcohols, xanthates, ethers and esters and others. Since the fluorinated analogues of the conventional hydrocarbon flotation collectors possess enhanced surface properties, a few were selected for testing. Because a survey of all possible minerals and reagent combinations would be out of the question, hematite was chosen to represent a nonsulphide system and pyrite to represent a sulphide system. The fluorinated reagents used in these experiments were prepared in the research laboratories of Minnesota Mining & Mfg. Co. Some were synthesized especially for this research. They are not available cokmercially. Separation of Nonsulphide Ores: The separation of oxides from silica has always been a challenge to the flotation industry because differences in surface properties of the minerals are normally insufficient to produce clean concentrates. Oleic acid," rosin acids,' and amine salts% ave been used to considerable extent to effect separation of metal oxides and silica. The system hematite-silica was chosen to represent the nonsulphides both because of its difficulty of separation and because large tonnages of easily obtainable material are available, such as gravity concentration tailings and nonmagnetic taconites on the Mesabi Range. The wash-ore tailings used here contained approximately 35 pct iron after desliming. Samples of the material used in this work were part of the same lot used by Chang, Cooke, and Huch9 and were prepared in an identical manner. Reagents for Nonsulphide Ores: Since one of the purposes of this investigation was to compare hydrocarbons with fluorocarbons, reagents of known behavior such as oleic acid, and the alkali metal salts of certain resin acids (Dresinates), were established as standards. Hydrocarbons and fluorocarbons of comparable chain length and other experimental fluorocarbons were tried as collectors for hematite. A list of the materials used and the concentrations of their stock solutions are given in Table I. Since silica can be selectively floated from hematite by conventional reagents," a few fluorocarbon reagents were also tried for this purpose. Their composition and concentrations are given in Table 11. Most of these reagents served the dual function of collector and frother. In the case of F-11 flotation did not occur but it served as a frother when F-6 was employed as a collector. Reagent grade sulphuric acid and sodium hydroxide were used to regulate the pH. Deionized water containing less than 0.1 ppm of salts expressed as NaCl was used for all solutions and flotation tests. The pneumatic flotation cell consisted of a 350-ml fritted glass Buechner funnel with a source of filtered air which could be controlled by a needle valve." A 50-g sample of ore and 250 ml of deionized water were added to the flotation cell and stirred slowly. The reagents were added and the pulp was conditioned before air was admitted to the cell. Approximately 15 ml of the pulp were removed for pH determination before flotation was started and were then returned to the system. The pH was again measured after flotation. Air was admitted to the cell until no further flotation occurred or until the character of the float changed markedly. Both the float and the nonfloat products were filtered, dried, weighed. and assayed for iron. The cell was washed in hot water and rinsed with deionized water after each test. Occasionally the cell was cleaned with concentrated hydrochloric acid to remove iron oxide particles from the glass frit. Experimental Results: Above a pH of 8, sodium oleate was an effective collector for hematite. The emulsification of equal parts of heavy fuel oil (20"

Jan 1, 1956

By G. E. Keller, G. D. Coe

Several methods have been devised for rapid determination of sulfur in coal using a high-temperature combustion furnace. The fundamental principles of the various methods are similar but the techniques vary widely. The method described herein is no different in principle from some of its predecessors but varies considerably in technique. Originally devised to overcome the low-accuracy criticism leveled against the others, the tube-furnace method has proved successful for limited applications. Work is being done to widen the applicability of the technique. Subsequent to the work of A. Vita1 in 1920, a number of investigators have published data dealing with the rapid determination of sulfur in coal using a high-temperature combustion furnace.2-5 These, together with several unpublished methods, involve wide differences in technique although they are all similar in principle. Investigation of typical details of procedure showed that poor precision or accuracy could be attributed to one or more of the following: 1) inadequate quantity of sample to be representative, 2) a delivery tube temperature too low to confine condensation to a washable area of the tube, 3) no provision for back washing the delivery tube, 4) incomplete absorption of the sulfur compounds due to inadequate bubbler, and 5) the false assumption that all of the sulfur is evolved as sulfur dixoide. The method herein discussed is no different in principle from some of its predecessors; the differences are in technique. Although the method is rapid—a determination can be completed in 5 min— accuracy has riot been sacrificed in order to achieve speed. MATERIALS AND EXPERIMENTAL WORK Fig. 1 shows the arrangement of the equipment. A metered volume of oxygen is passed through calcium chloride for removal of moisture, then through Ascarite for removal of carbon dioxide, and thence through a glass tee to the feed end of the combustion tube. Connected to the side arm of the glass tee is a rubber tube that is closed with a pinch clamp during combustion of a sample. The products of combustion are expelled through a Vycor bubbler, the end of which is submerged 3 cm below the surface of a 1 pct hydrogen peroxide solution contained in a 300 ml high-form beaker. At the completion of the 4-min combustion period the contents of the beaker are titrated to a yellow end point, using a methyl red indicator, with 0.05 N sodium hydroxide (or sodium tetraborate). The pinch clamp on the tube leading from the tee in the oxygen line is then opened and mouth suction applied to draw the hydrogen peroxide up into the bubbler past the ell, almost to the rubber tube connecting the bubbler to the combustion tube. This washing of the bubbler is repeated until no further acid reaction with the indicator is obtained. The hydrogen peroxide-sul-furic acid solution is then titrated to the final yellow end point. Test work conducted at the Robena Laboratory disclosed the following critical conditions that had important bearing on the precision of the method: Weight of Sample: Several series of tests wherein the sample weight ranged from 0.1 to 0.5 g of -60 mesh coal showed that the lowest variance (standard deviation squared) resulted from the use of 0.5-g samples; the variance was slightly greater when 0.3-g samples were used, and with less than a 0.3-g sample weight the variance increased rapidly with decrease in weight. Although the use of a 0.5-g sample invariably resulted in a very slight explosion as soon as the sample entered the hot zone of the combustion tube, this did not detract from the precision of the method. Temperatures: Mott and Wilkinson5 found that a combination of low temperature (1250°C) and low oxygen flow rate (less than 700 ml per min) tended to give high results due to formation of oxides of nitrogen. Although the method herein employs a much higher oxygen rate than 700 ml per min, as an additional precaution to assure accurate results, 1315°C (2400° F) is recommended as the most desirable furnace temperature. The temperature of the elbow of the bubbler should be at least 75°C to minimize condensation

Jan 1, 1961

By John Freeman

THE tensile properties of steels at elevated temperatures have been studied by numerous investigators,1 primarily for the purpose of determining their suitability for structural uses. Tests with this objective have been confined largely to the temperature range of approximately 20° to 500° C., because of the rapidly decreasing tensile strength at the latter temperature. Tests have also been extended to higher temperatures for the purpose of determining the most suitable forging range. This temperature range is also of theoretical interest. The phenomenon of increased tensile strength and decreased ductility in the so-called "blue-heat" range, approximately 200° to 300° C., is well known. It was suggested to the Bureau early in 1926 that a study of the properties of rail steels in this temperature range might prove of interest in relation to the studies of transverse-fissure failures in rails. There were available from another investigation3 several new rails from several different heats made to approximately the same specification requirements, the complete manufacturing histories of which were known. It was decided to determine, at least in the preliminary series of tests, only the ultimate tensile strength, elongation and reduction of area, because of the difficulty, time and cost involved in determining the proportional limit and yield point at elevated temperatures.

Jan 1, 1930

Prof. Mathesius analyzes the running of Howland's furnace No. 19, according to the method described by him in Stahl and Eisen, 1916, Nos. 30 and, 31, and in his work "Die physikalischen und chemischen Grundlagen den Eisenhüttenwesens" (Spamer, Leipzig). By assuming 500 Cal. lost from the hearth by radiation and cooling water per kilogram of pig iron made, a throat-gas temperature of 600° C., and taking the ratio of C02/CO as 0.64, he finds that his diagram would show 0.68 kg. of carbon oxidized per kilogram of pig iron, while Howland gives 0.66 kg. He expresses himself as well satisfied with this test of the accuracy of his theory. Making the further assumption that the heat losses from the shaft are 1,000 Cal. per kilogram of pig iron (twice as

Jan 5, 1917

By Eugene N. Cameron

Pegmatites of these areas have become important sources of beryl and lepidolite and have yielded cassiterite, columbite-tantalite, and other minerals. Examination of about 60 of these pegmatites leads the author to question the opinion of earlier investigators that the concentrations of beryl, lepidolite, and columbite-tantalite found have mostly formed by hydrothermal or pneumatolytic replacement of previously formed quartz-feldspar pegmatites. The author concludes, on the contrary, that present knowledge of the occurrence of minerals in zoned pegmatites can be applied to prospecting and mining of pegmatite deposits in these two areas of South West Africa. PEGMATITES occur in abundance in certain areas of South West Africa and in adjacent parts of northern Cape Province in the Union of South Africa. Some of the pegmatite deposits were prospected before World War I, and intermittent mining was done during the period between the two World Wars. The deposits of the Jooste lithium mines became an important source of lepidolite, and beryl, columbite-tantalite, wolframite, and other minerals were produced. Since World War II prospecting and mining have been carried on vigorously, with the result that South West Africa produced nearly 3000 tons of beryl during 1949 through 1953, together with more than 40,000 tons of lithium minerals, chiefly lepidolite and petalite. Small amounts of tantalite, columbite, and other minerals have also been produced during the postwar period. Most of this mineral production has come from two pegmatite areas roughly outlined in Fig. 1. One is the Karibib-Omaruru area of north central South West Africa. The second is the northeastern part of the Orange River pegmatite area, which extends into adjacent parts of Namaqualand, in northern Cape Province of the Union of South Africa. The writer visited the two pegmatite areas in July 1951. The visit was brief. but it gave an opportunity to compare some of the' pegmatites of these areas with those studied and described in detail by many investigators in the U. S., Brazil, and Canada during and since World War 11.'-l' The writer has attempted to determine, in a preliminary way, whether the concepts of internal structure and distribution of minerals in pegmatite bodies developed out of these studies are applicable to prospecting and exploration of pegmatites in South West Africa. Previous Work In an important series of papers (1929 to 1942) T. W. Gevers, H. I?. Frommurze, S. H. Haughton, G. K. Joubert, and other geologists of the Geological Survey of South Africa described and discussed the pegmatites of the two areas.*-" These works are the principal sources of information on the pegmatite mineral deposits of South West Africa. The investigations showed that in the two areas pegmatites are profusely distributed in pre-Cambrian rocks. These rocks are meta-igneous and metasedimentary units that have been folded and subsequently invaded by younger pre-Cambrian granites and by other igneous rocks. The pegmatites are considered to be genetically related to the pre-Cambrian granites. Pegmatites occur in the granite bodies themselves but are most abundant in the surrounding metamor-phic rocks, a pattern repeated in many pegmatite districts of the world. The origin of the pegmatites and the factors controlling the occurrence of mineral deposits in them were discussed at length by Gevers and Frommurze (1929)" and later by Gevers 14, 15 pp. 41-51, Ref.

Jan 1, 1956

By I. N. Zavarine

AUSTENITE is often defined as a solid solution of carbon or carbide in a nonmagnetic form of iron. Conversely, magnetic measurements are often used by investigators for the purpose of detecting the degree of austenite decomposition after an iron alloy has been subjected to certain thermal or mechanical treatments. Association of the magnetic state with the gamma-phase decomposition is often extended to the alloys of iron with elements other than carbon. Definition of austenite as a nonmagnetic solid solution cannot be accepted in the light of available information without certain reservations. The relation of magnetic transformations with the gamma-phase decomposition in the complex alloys of iron has never been rigorously proved. The present investigation deals primarily with the magnetic trans-formation that occurs in carbon steels during the quenching process. The work was further limited to a study of magnetic transformation in carbon steels quenched at such rates as are necessary to retain the product of austenite decomposition in a martensitic state.

Jan 1, 1934

By Harrison Everett Ashley

Slimes are usually defined as all material passing a certain sized sieve, which is invariably the finest sieve employed by each metallurgist in his tests; 100-mesh and 200-mesh have been taken as the limits by different writers in recent volumes of the Transactions; 150-mesh is common practice. The reader of the first two volumes of Richards' is impressed by the inflexibility with which all grinding-arrangements are praised or condemned according as they make little or much slime. Until recently, one of the principal aims of the mill-man was to keep down the slimes. He was obliged to have separate apparatus for sand- and slime-treatment. The latter was sometimes puzzling and erratic. Often it was found most economical to omit treatment of the slimes entirely, or to store them in immense basins or heaps, waiting for possible future improvements in methods of treatment. Recently, improved processes of agitation and filtration have made possible the successful extraction of values from many slimes. The tendency, when the metal is exceedingly finely disseminated, is to cut out all sand-treatment and to slime everything. These processes have been almost entirely mechanical in their conception, and it is the object of the present paper to show that certain chemical considerations may greatly hinder or assist their successful operation. It has long been a source of dissatisfaction to chemists that their analyses fail to be of much help to the clay-worker; that it is a matter of common occurrence for clays of closely identical ultimate chemjcal constitution to show the widest possible divergence in physical properties.

Jan 1, 1911

By J. W. Hickman

Most of the electron diffraction studies of oxide films which form on metals and alloys have been carried out by oxidizing the specimens in an auxiliary furnace, cooling down to room temperature and then inserting the sample in the camera and taking a diffraction photograph. Prior to the investigations at the Westinghouse Research Laboratories, no systematic study of the oxidation of any metal or alloy had been made over a wide temperature range with photographs taken at elevated temperatures except the investigation of iron by Jackson and Quarrell.' In order to interpret the electron diffraction patterns of the oxides which may form on alloys, it seemed advisable to make a comprehensive study of the oxidation of the purest metals available in the bulk form. Thus far studies have been completed on iron,2 cobalt,~ nickel,= chromium,= copper,z tungsten,s molybdenum,3 beryllium,' uranium,' thorium,' titanium6 and zirconium6 while investigations are in progress on tantalum and columbium. The next step in the study is concerned with the investigation of the oxides which form on binary alloys. Some of the alloys consist of a single phase while others contain more than one phase. The identification of the oxides on the surface of a binary alloy may be more difficult than on the metals since oxides containing both metals as well as those of each metal separately may form. Furthermore, it is possible that solid solutions of the various oxides may occur. In these cases the electron diffraction method may not be able to identify the oxidation products unequivocally. Examples of solid solutions which may present difficulties are MOO* and WOp, Fe304 and FeO.CrnOa since the diffraction patterns are so similar. Since electron diffraction can determine only the structure of the oxide, the chemical composition must be inferred from the diffraction data based upon X ray diffraction investigations of specimens of known composition. It is possible in some cases to decide whether a given solid phase reaction can occur on the surface of an alloy by a study of available thermodynamic data. Table I lists the equations for the formation of most of the oxides from the elements together with values of loglo Kg for the several temperatures. AF"B = -RT In KR AF°R and KR are the free energy and equilibrium constant of the reaction. Calculations may be made using the the given in I 1 to determine whether a given solid phase reaction is possible thermodynamically. For example, a solid phase reaction should occur between aluminum and chromium oxide to form

Jan 1, 1949

By Frederick C. Hull, Robert F. Mehl, Robert A. Colton

IT is known that pearlite forms from austenite by a process of nucleation and growth, and that the rate of formation of pearlite may be described by a rate of nucleation and a rate of growth.1,2 The manner in which these two quantities operate to produce the observed isothermal reaction curve has been analyzed in a paper published in 1939.3 Two types of process were described: (1) that in which nucleation occurs at the grain boundaries of the parent phase, with the nodules growing toward the centers of the grains, initially as hemi¬spheres and then after impingement as roughly radial-columnar structures; and (2) that in which nucleation occurs generally, with the nodules growing to full spheres until impingement with other growing nodules restricts growth. Both cases are met in the formation of pearlite from austenite (Fig. 1);2.4 the former, occurring near the knee of the S-curve has been named "grain-boundary transformation," and the latter, occurring at temperatures near Ae1, has been named "group-nodule transformation." In developing our knowledge of the factors that determine the rate of formation of pearlite from austenite, it is important 1,2 to obtain data on the rate of nucleation and the rate of growth of pearlite. Such data, when obtained near the knee of the S-curve, will furnish information of use in understanding the factors that affect hardenability; when obtained at higher temperatures, such data will be useful in understanding the behavior of steels that during heat-treatment react to pearlite.2 It is the purpose of this paper to present data on the rate of nucleation and the rate of growth of pearlite in dependence upon composition, grain size, temperature, and the degree of homogeneity of the parent austenite. The studies are restricted chiefly to plain carbon commercial steels.* PREVIOUS DATA ON RATE OF NUCLEATION AND RATE OF GROWTH Data on the rate of nucleation and the rate of growth of pearlite have been published by Scheil and Lange-Weise,5 by Mirkin and Blanter,6,7 by Mehl,1 and by Dorn, De Garmo and Flanigan.2 It is difficult to interpret the data, for in most cases too little information is given on austenitizing temperatures and times, the state of homogeneity of the austenite (presence or absence of carbide, etc.), austenite grain size, and mode of formation of pearlite at the temperatures given.

Jan 1, 1942

By T. Carl Shelton

The coal industry of the United States in 1967 had reasons to be both exuberant and concerned about its present and future role in the economy of the country. Continuing a momentum that began in the early 1960's, the industry has moved ahead in providing competitive customized products to strengthen its long-term domestic and foreign commitments, and has maintained with steady progress its position as a major supplier of energy. On the other hand, the industry must overcome air- water pollution and conservation-reclamation problems that have been identified by 1967 legislation. Throughout the year, the industry was characterized as "progressive," "healthy" and "dynamic." To have been termed a "growth industry" in 1967, is an accolade the coal industry can accept with pride. Culminating its efforts throughout the decade, the industry has emerged with a competitive image that is representative of its future strength.

Jan 2, 1968

By Jerome Strauss

IN his review of developments in 1943, Gilbert Seil, Chairman of this Committee on Reduction of the Ferroalloy Ores, tabulated the consumption of the alloying metals in relation to the steel production of that year. In the year just closed the approximate tonnage was of the same order, differing only to a minor degree or suffering some correction with more precise figuses available, as indicated in the following estimates: Consumption Metals in Tons Steel 92,000,000* Manganese 700,000 Silicon 200,000 Chromium 200,000 Nickel 75,000 Molybdenum 20,000 Tungsten 8,000 Vanadium 1,700 Titanium 1.600 Boron 10 `Production figure. The technologic studies instituted during 1942 and carried forward with such great vigor during 1943 continued into 1944 although in some instances were brought to a close either by completion of the specific development

Jan 1, 1945

By K. A. SPENCER

THE production of soft coal from strip mines in the United States has shown a remarkable growth in the last sixteen years, increasing from one and one-quarter million tons in 1914 to approximately twenty-two million tons in 1929. This is a growth of approximately 1660 p& cent, as compared with a growth of approximately 20 per cent in the underground mines for the same period. But even with this marked in- crease the total tonnage produced by open-face mining represents only 4 per cent of the nation's soft coal tonnage.

Jan 1, 1931

By Arthur F. Taggart

Some years ago, A. M. Gaudin and one of the authors published a paper showing removal of tar acids from solution by sulfides preferentially as compared to gangues (specifically by galena as compared to quartz).' The underlying phenomenon was classed as adsorption, and the paper went on to develop the general thesis that so far as water-soluble frothing and collecting agents in flotation are concerned, the phenomenon of adsorption is one of controlling importance. Adsorption was defined in that paper as "a process of rearrangement of a system, which results in establishing a difference in concentration, as between the interfacial layers and the bulk of the phases, of a substance or substances initially uniformly dispersed in one or several of the phases." The paper went on to develop the relation between adsorption and surface cnergy according to Gibbs' equation (which may be thrown into the form U/c = KdT/dc, where U = excess concentration in surface layer, c = concentration, T = surface tension, and K is a constant), and pointed out that, according to this equation, degree of adsorption and change in surface tension vary directly. The present paper offers a somewhat different definition for the term adsorption; and sets up, in sweeping terms, the generalization that simple chemical reaction underlies the functioning of the flotation reagents which control mineral collection, when these reagents are soluble in and act from solution in the water of the pulp. Adsorption According to the modified definition, adsorption means concentration at an interface between different phases in a heterogeneous system (thus far the definition runs as before), by the action of some mechanism, of which nothing is properly implied in the word, and concerning which the user of the word is probably in entire ignorance. Thus defined,

Jan 1, 1930

By Norman Goss

IT is generally agreed that cold-working mechanically refines the grains into smaller fragments and with continued working these are oriented with certain crystallographic directions bearing a relation to the direction in which the metal is worked. Some of the energy expended on the metal during plastic deformation appears in the form of heat, but a very small portion remains in the metal as stored energy. The entropy, specific heat capacity, temperature at which recrystallization will just begin, density, ductility, elasticity, tensile strength, and resistance to corrosion are affected. These properties have been studied extensively and some of the changes in the physical properties due to cold-working were attributed to lattice distortion.1-8 The broadening of the K. lines on the X-ray diffraction diagrams of plastically deformed metals is believed to indicate lattice distortion, and consequently the existence of internal stresses. The evidence supporting this theory rests solely upon the observed experimental fact that the dif-fraction lines are broadened and the K a doublets are completely diffused. Elam9 has reviewed the matter of lattice distortion in relationship to the hardening of metals by plastic deformation. The X-ray diagrams of plastically deformed metals differ in general from annealed metals. The hardening of a metal was believed due to lattice distortion.9 The resolu-tion of the doublet is lost when a metal is cold-worked and the Lane spots are elongated. At one time this elongation was thought to indicate the elastic bending of the crystal planes. However, more careful work showed that the asterism was due to new orientations developed within the fragmented grains during plastic deformation. Some theories attrib-uted the hardening to fragmentation of the grains into smaller units.

Jan 1, 1940

By A. E. Bibb, F. W. Kunz

A platelet form of zirconium hydride was found in zirconium and ZY-1 wt pct U single crystals containing hydvogen in the range of 50 to 100 ppm. The habit planes for the hydride plateletg in the zirconium crystals were found to be {1012}, {1121}, and (1122) while the habit planes in the ZY-1 wt pct U crystals were {1121), {1123}, and (1.231). With the exception of the {1231} plane, these have been identified as the twin planes in zirconium. The different effect of hydridc on the mechanical puoperlies of zirconium at high and low strain rates has been explained in terms of the defornzation mechanism and the habit planes of the hydride. ZIRCONIUM and zirconium-base alloys are considered for many nuclear reactor applications, where the pick-up of hydrogen is a distinct possibility, if not an unavoidable occurrence. An excellent example of this is the absorption of hydrogen by zirconium and its alloys during aqueous corrosion, where as much as 30 pct of the hydrogen produced by the corrosion reaction is picked up by the metal. Under the proper conditions, the absorbed hydrogen would precipitate as zirconium hydride and consequently alter the mechanical and physical properties of the zirconium-base alloys. The knowledge obtained from a study of the crystallographic aspects of the hydride precipitation is necessary for the interpretation of the observed changes in the mechanical and physical properties. The deleterious effect of hydrogen on zirconium-base materials is not always observed in normal slow tensile loadings at or above room temperature, but becomes immediately obvious under impact loading, where the energy absorbed decreases with increasing hydrogen content,' and in notched specimens where triaxial loadings are attained.2 This effect is of serious consequence in the applications of Zr where shock loads or high strain rates are experienced. The purpose of this investigation was to determine the crystallographic planes of the Zr and Zr-1 wt pct U matrices upon which zirconium hydride will precipitate and to correlate these with the observed mechanical property data. PROCEDURE Crystal Growth—Single crystals of Zr and Zr-1 wt pct U alloy were used in this investigation. The Zr crystals were made from sponge that had a typical analysis as shown in Table I. Large grains were grown in this material by rapid cooling an arc-melted charge in a button furnace. This operation undoubtedly lowered the volatile impurity concentration below those listed in Table I. Back-reflection Laue patterns of these large grains showed the presence of considerable substructure and lattice distortion within each grain. It was found that an 18-day anneal in an argon atmosphere at 840°C (a high a heat-treatment) followed by furnace cooling, resulted in the further growth of the large grains and removed the detectable substructure ana lattice distortion. Equiaxed crystals with a cube edge of approximately 1/4 in. were produced in this manner. Large crystals of Zircaloy-2 (1.5 wt pct Sn, 0.15 wt pct Fe, 0.1 wt pct Cr, 0.05 wt pct Ni) also were produced by this technique but the large amount of substructure formed could not be removed by annealing. The Zr-1 wt pct U solid solution crystals were produced from an alloy rod consisting of Westing-house-Foote hafnium-free crystal bar zirconium and depleted uranium. The chemical analysis of the alloy is also given in Table I. Three-inch sections were cut from an 0.120-in.-diameter alloy rod and tapered to a fine point on each end. The samples were sealed in evacuated Vycor tubes, homogenized for 5 hr at 1000°C in the ß-phase field, and slowly lowered in a gradient furnace into the a phase (800°C), annealed for 60 hr at this temperature to produce grain growth and furnace cooled. This technique produced large grains approximately 1/2 to 3/4 in. long over the entire cross section of the rod, which were free of observable substructure. Metallographic examination up to X1000 did not show the existence of any second phase in these grains. Crystal Orientation—All crystals were abraded on fine emery paper to produce two flat surfaces 90 deg to each other. The crystals were analyzed by the standard Back-Reflection Laue technique to obtain the crystal orientation with respect to the abraded surfaces. The Back-Reflection Laue Photograms of all crystals used were clear and sharp indicating that the crystals were free from any substructure that could be detected by these means. Hydriding—Only samples containing four to five grains were used for hydriding. Samples that exhibited fine grained patches were discarded. The samples were hydrided using the following technique. After etching in 48 vol. pct HNO3, 48 vol. pct H2O, and 4 vol. pct HF (48 pct) solution, the specimens

Jan 1, 1961