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By Oren C. Baptist

Umiat field contains the largest accumulation of oil discovered so far in Naval Petroleum Reserve No. 4 in Arctic Alaska. The Umiat anticline was tested with 11 wells; 6 produced oil in varying quantities. Behavior of the wells during testing was unpredictable. For example, one well was abandoned as a dry hole after all tests failed to recover any oil, yet an offset well, only 200 feet from the dry hole, produced 400 barrels of oil a day. The main oil reservoirs are less than 1,000 feet deep and are in the permanently frozen zone (permafrost). Reservoir pressures are low, and most primary production will be by expansion of gas-in-solution in the oil. Because of the unusual reservoir conditions and the difficulties encountered in drilling and completing the wells, the Department of the Navy asked the Federal Bureau of Mines to make laboratory studies of the reservoir sand to determine the cause of well plugging and to provide laboratory information, to be used as an aid in estimating oil recovery from frozen reservoir rocks under solution-gas expansion from low-saturation pressure conditions.

Jan 1, 1960

By Eldon C. Pattee

THE BUREAU OF MINES began an investigation of tungsten resources of Montana in September 1953. This report presents information obtained from July 1955 to September 1957 on tungsten deposits in and near the Mount Torrey batholith. The batholith comprises part of the Pioneer Mountains of Beaverhead County in the southwest corner of Montana. Included in the report are assays and preliminary-examination data on 22 properties. Tungsten minerals are known to occur in 19 of the properties. The major producer is the Brown's Lake mine which has produced more than 625,000 tons of ore. Nearly all of the deposits are in the Lost Creek, Utopia, and Bald Mountain mining districts along the east and south margins of the Pioneer Mountains. The districts are less than 27 miles from Dillon, Mont.

Jan 1, 1960

By Claude E. Wykes

Deep Well turbine pumps receive constantly increasing application to the problem of mining water and other fluids from great depths. Many installations of medium settings are presently operating successfully and it is felt that mach greater depths are immediately within reach. Settings and lifts in excess of 2000 feet: are not at all out of reason with present knowledge experience, and materiels; however, conditions of individual applications will govern in each case and dictate methods and possibilities to the designer. Design and operating problems of deep set -turbine pumps ire discussed together with a description of various types of equipment falling within this category. Although the deep well turbine pump has been produced In the vertical turbine pump industry for many years, the connotation of the word "deep" still remains questionable. Among the manufacturers of this type of machinery, answers to the question implying the practical limitation of setting for a deep well pump will vary to an extreme. Most pump designers are in accord that this type of equipment has not yet been exploited to its fullest degree; however, the subject is admittedly fraught with unsolved problems and un¬tried solutions so that such a discussion must necessarily derive from personal opinion and, belief., even though based on substantial experience and background. For this reason, it will be stipulated that the present writing will deal with what may be termed euphemistically ?a highly controversial subject.? During the nineteenth century, a paper was published under proper authority proving beyond question that the human body could not withstand speeds exceeding 20 miles per hour. As a limitation, this looks ' pretty ridiculous to us today. At the beginning of the twentieth century, there was not a single machine in operation that could be described as mullti-stage deep well centrifugal pump. As a matter of fact, very few centrifugal pumps of any type wire operating against heads in excess of 50 feet, since such applications were considered impractical. In the

Jan 1, 1960

By C. Wert, D. Keefer

The results of this study indicate that sudden increases in aging temperature lead to reversion phenmena in carbon in the a, iron system. These phenomena are thought to be associated with the dissolution of carbide precipitates. Reversion is studied with respect to three variables: 1) Specimen grain size, 2) the initial amount of carbon in solution, and 3) difference between initial and final aging temperature. It is found that of these variables the initial carbon concentration has the greatest effect on reversion. THE solid solution of carbon in n iron has been the subject of numerous investigations throughout the past few years. Despite the great amount of effort which has been put forth toward understanding this system, however, there persist a number of interesting aspects of the system which are open to further research' Studies Of the precipitate which forms as a result of aging a supersaturated solution of carbon in a, iron appear to be particularly interesting. The present work is an attempt to determine certain

Jan 1, 1960

By William H. Waggaman

The United States not only is the largest producer of phosphate rock but also manufactures and consumes greater quantities of phosphate products than any other country. New and expanding uses will increase even further the demand for this basic raw material. Only a small proportion of the total quantity of phosphate rock mined and marketed is consumed directly in a raw or unprocessed state; the vast bulk is chemically treated and converted into [ertilizer] and a wide variety of finished products that play a vital role in [r] national economy. Three fundamental methods are employed in decomposing phosphate rock. 1. Reduction by carbon at high temperatures. 2. Treatment with one or more acids. 3. Calcination or fusion with silica, sodium salts, magnesium minerals, or small quantities of phosphoric acid.

Jan 1, 1960

"D bed, Ky., coaL, washing characteristics RII 5140coking coal, reserves, estimate RI 5037Pa., coal, washing characteristics RI 4834, 4941D bed mine, Ky., coal, washig characteristics"

Jan 1, 1960

By Robert L. Rough

This report presents the results of an investigation by Federal Bureau of Mines engineers of water-injection projects in the northwestern Pennsylvania and southwestern New York area, where oil-producing wells have been converted from pumping to flowing. Data from 24 leases converted to flowing were collected and examined. Only 10 leases had information of significant scope for inclusion in the final analysis. The projects were classified in one of two categories. Group I consisted of leases operated to permit an evaluation of operational changes in terms of existing pressure differentials between injection and producing wells. Group II included remaining properties, for which enough information was available to justify an economic analysis but which did not have sufficient production data to support an engineering study because of radical changes in operational techniques. Variations in production and costs resulting from conversion to flowing were examined for production methods, well-spacing and completion techniques, and reservoir characteristics. Where water-injection rates were constant, oil production usually decreased rapidly at the time of conversion; production then increased slightly for 6 to 8 months before resuming a normal decline rate considerably below the estimated pumping rate. The abrupt decrease in production after conversion is indicative of lower pressure differentials between injection and producing wells, caused by the increased hydrostatic head in the producing wells.

Jan 1, 1960

By Howard E. Rollman

South Central United States, an area including Arkansas, Kansas, Louisiana, Mississippi, Missouri, Oklahoma, and Texas, is a net exporter of refractories. Nearly $45 million of these materials was shipped in 1954 from plants in the area, compared with area consumption of $18.5 million. About 88 percent of all refractories production is concentrated in Missouri. The prevalent consumption pattern, however, is one of localized shortages. For example, although Texas uses more than half of the refractories consumed in the South Central United States, production of refractories in Texas is relatively small. Also, the apparent self-sufficiency of the area is in terms of value produced rather than in terms of products consumed. Nearly all of the $6,425,000 nonclay refractories consumed in the area were shipped from other States. Local resources possibly could be developed for making refractories to serve markets that currently are being supplied from outside the area. Since other industries are growing rapidly in the area, the market for refractories is expected to continue to grow--more rapidly than the national market. The Missouri refractories industry is economically important nationally. Nearly one-fourth of the clay refractories produced in the United States are made in Missouri. Moreover, Missouri produces most of the higher grade clay refractories, about 62 percent of the high-alumina refractories, and 85 percent of the superduty refractories. The competitive position of the Missouri refractories industry is strong. The national market for clay refractories and the market in the South Central United States are expected to continue to grow. The ratio of net income to the value of refractories shipped in Missouri is larger than the national average.

Jan 1, 1960

By Alfred Siegel

Mineral pigments give color, opacity, or body to paint, stucco, plaster, mortar, cement, linoleum, rubber, and similar materials. They must be finely divided, substantially insoluble, and generally inert for such uses. Inorganic pigments may be grouped somewhat arbitrarily as follows: A. Natural mineral pigments dug from the earth. 1. Those consisting mostly of iron oxides, such as hematite and limonite. 2. Those containing large amounts of clay or noncoloring matter, such as ocher, sienna, umber, and colored shales. 3. Those whose color is not due to iron oxide, such as Vandyke brown (including sap brown, an alkali extract of Vandyke brown), graphite, and terre verte. B. Synthetic pigments. 1. Those containing iron oxide as the essential coloring matter, such as "pure" reds, yellows, and blacks, and Venetian reds. 2. Those not containing iron oxide, but rather such compounds as lithopone, zinc white, titanium white, ultramarine, Prussian blue, and the like. Only groups A and B-1 are discussed here. All the pigments in those two categories, except Vandyke brown, sap brown, and some of the carbonaceous slates, contain, as their essential color constituents, one or more compounds of iron; namely, an oxide-limonite (2Fe2O3.H2O to Fe2O3.4H20), hematite (Fe2O3), or magnetite (Fe2O3.FeO). Man's first permanent coloring materials were earth pigments-the ochers, iron oxides, and various iron-stained clays. The caves occupied by prehistoric man and the arts of the ancient Chaldean, Egyptian, and Cretan civilizations bear mute witness to this and also testify to the beauty and permanence of earth colors. As the Roman era developed, earth pigments were pushed from their pre-eminent position by white lead and red lead and in the Middle Ages by zinc oxide. Today, of course, the number of acceptable pigments is very large and on a value basis the group of natural and synthetic earth pigments stands forth with $16,000,000 per year; it is surpassed by titanium, lead and zinc pigments. Of this sum,21 natural pigments supplied 31 pct of the tonnage and 16 pct of the value of the total finished pigment in 1957, the remainder representing the tonnage and value of sales of the synthetic iron oxide colors. The average value of finished natural pigments in 1958 was $80.62 per ton. The average value of manufactured pigments in the same year was $202 per ton. Of the 60,000 tons of manufactured colored pigments sold in 1958, the reds comprised 76 pct of the market and the yellows 20 pct. The reds furnished 68 pct of the value and the yellows 24 pct. Of the finished iron oxide pigments (natural and manufactured) sold in 1958, the reds dominated the market with 66 pct of the quantity and 63 pct of the value; yellows supplied 17 pct of the quantity and 20 pct of the value, and browns furnished 11 pct of the quantity and 10 pct of the value. The average value of the reds was approximately $152, and the average value of the yellows $190 per ton. The highest valued pigment in 1958, with almost 12 pct of the total tonnage and 21 pct of the value of the iron oxide pigment market, was manufactured red from calcined copperas valued at $286 per ton.

Jan 1, 1960

By G. Bitsianes

An experimental procedure was developed for studying magnetic roasting on a accurately-controlled laboratory scale. The loss-in-weight method was used and the course of reduction could be followed under a reducing gas atmosphere containing as many as five different components. Some important variables of the operation were checked on a marginal Mesabi iron ore containing porous and dense varieties of hematite as well as pure goethite. The conditions simulated were those for the grate roasting of a coarsely-sized ore burden. Temperature was maintained at 600°C; gas composition at 4.25% CO, 4.25% H2, 17.0% CO2, 15.0% H20, and 59.5% N2,, and gas flow rate at about 1,5 lineal feet per minute. The ore charge was composed of quarter-inch cubes. Under these conditions, the ore porosity was found to be one of the governing variables of the operation. Results showed that an ore size limitation existed as a function of this ore porosity. For efficient magnetic conversion, the size limit was 3/8 inch for very porous ores and about 65 mesh for very dense ores. An anomaly was noted in the weight losses incurred during actual magnetic conversion. For goethitic ores, these were generally about 13 per cent higher than could be accounted for theoretically. The effect was attributed to possible non-stoichiometric structures forming during the reduction process.

Jan 1, 1960

By D. L. Wood

This investigation was concerned with the aluminum-oxide particle dispersions, the mechanical properties, and the re-c,uystallization characteristics of some internally oxidized copper-aluminum alloys. Obserued hardness vaviations are in agreement with variations in oxide particle size revealed by electron metallographic studies. The increase in yield strength caused by internal oxidation is quite sensitive to matrix grain size and is accompanied by a loss of ductility, particularly at higher temperatures. Elevated temperature ductility is con-side,vably improved if major grain reorientation is accomplished by ve recrystallization prior to testing. The oxide particles offer a considerable restraint to softening during annealing after cold deformation. THE diffusion of oxygen under appropriate conditions into a suitable alloy causes solute oxide particles to be precipitated at an inward moving interface.1,2 Previous work has shown that the hardness

Jan 1, 1960

By Kenneth A. Gutschick, Robert S. Boynton

Lime has become a very general loosely used term that includes virtually all finely divided types of limestone as well as burned forms of lime. However, actually (and according to Webster) lime is only calcined limestone (known as quicklime, calcium oxide, or calcia). It also embraces the secondary product of quicklime-namely hydrated lime or slaked lime (calcium hydroxide). Fundamentally there are two basic types of limestone-high calcium and high magnesium (dolomitic). The dolomitic quicklimes and hydrated limes correspond to their "high calcium" counterparts in terminology. The only difference is that the dolomitic types are a combination of the elements, calcium and magnesium, whereas high calcium limes contain only 0.5 to 2 pct of magnesium. Both types, which are made through calcination at high temperatures, are shown chemically as follows: [ ] In the above reactions either type of limestone is burned (calcined) in furnaces known as lime kilns so that the carbon dioxide content of the stone is expelled as a gas. With high calcium limestone 44 pct of the weight of the stone is lost; with dolomitic limestone the loss is 48 pct. Also, both reactions are chemically reversible since quicklime absorbs carbon dioxide readily and in so doing transforms itself back to the original carbonate form. Most quicklimes correspond in size to the original rock, which varies from one to eight inches, depending upon the type of kiln employed. Slight shrinkage occurs during calcination. A few limestones when calcined will decrepitate (break down) into a fine powdery form; however, chemically it is the same as the pebble or lump-sized material. For some uses the lumps of quicklime are pulverized and packaged. Since quicklime has great affinity for moisture and carbon dioxide, it is perishable. When it absorbs moisture and CO2 slowly from the atmosphere, the resulting product is "airslaked." Consequently, it must be stored in dry, moisture-proof areas that are free from CO2. Because of its fugitive nature, it is usually consumed within a few weeks after manufacture. A more stable form of lime is hydrated lime-commercially made by adding water to the quicklime until the lumps break down into a fine, white powder. This product, which is usually packaged, can be stored more safely; and many of its uses are interchangeable with quicklime. The irreversible chemical reactions of hydrated lime for both high calcium and dolomitic types are: [ ]

Jan 1, 1960

By Kenneth M. Ritchie

Mineral wool is a term applied to man-made fibers of silicate glass with useful properties resulting from their fibrous nature. In contrast with crystalline fibrous minerals such as asbestos, mineral wool fibers are amorphous, solid filaments produced by drawing from molten liquid and subsequent cooling. Chemically they are silicate glass with varying percentages of metallic oxides, especially those of aluminum, calcium, magnesium, iron, and in glass wool, sodium, potassium and boron. Other elements such as manganese, titanium, sulfur, etc., result from their presence in the raw materials used and are not purposely added. In the United States, mineral wool is a generic term and may be applied to rock, slag or glass wool. In Europe, glass silk and silicate cotton are products in the same category, but the term mineral wool is less commonly used. Current usage is to ignore the actual source and to differentiate products on a composition basis; thus rock and slag wools have about 35-45 pct of silica, while glass wool has 54 to 60 pct. Much mineral wool of slag origin is called "rock wool," and this practice is increasing, although wool made of slag from lead or copper refining is often referred to as "lead slag wool." Its greenish-gray to greenish-black dark color, due to 5-25 pct Fe (reported as FeO), distinguishes it from "white" wools made from iron, blast furnace slag containing only 1-2 pct FeO or Fe203. Most mineral wool is used for thermal insulation against heat and cold; sound absorption and isolation are probably the next most important uses. Both its thermal and acoustic values result primarily from the physical structure of the heterogeneous mixture of fibers and air which is the form in which the fibers are first obtained and handled. For this reason, within fairly wide limits, differences in chemical composition are relatively unimportant, and for most conventional applications all types are competitive in properties and value. Mineral wool intended for extreme conditions of high temperature, acid resistance and special purposes must have a chemical composition which will insure the desired properties. This may differ greatly from that of ordinary wools; for example one product approximately 98 pct Si02 and another consisting of 50 pct A1203 and 50 pct Si02 are produced and sold for high temperature service up to 2000°F or more. These are considerably more expensive to manufacture and their cost limits their use. Historical The manufacture of mineral wool consists fundamentally of a process which subjects molten material to shear and/or tensile forces that draw them into fibers. The liquids are cooled at a rate which solidifies them quickly. As a solid glass they are technically super-cooled liquids since they have no true melting point. The drawing out of glass into thin rods, filaments and tubes was known from very early times, and present day continuous production of glass filament for textiles was evolved gradually by adapting hand methods to automatic machinery. Rock and slag wool manufacture had a somewhat different development. Early explorers reported finding filamentous material

Jan 1, 1960

By H. S. Caldwell

This report describes work by the Bureau of Mines on the vacuum distilla¬tion of some of the more volatile metals such as cadmium, zinc, and magnesium from lead and tin. Evacuation within a distillation apparatus allows rapid diffusion of vapor away from the evaporation surface and prevents reaction of the vapor with residual gases. A reduction of pressure to several tenths of a millimeter makes possible practicable distillation rates, at temperatures for which the partial pressure of the metal vapor exceeds 10-3 atmosphere. The rate and selectivity of distillation depend primarily on the volatility and molal ratios of the alloy metals, and their chemical activity to each other. For very rapid evaporation or low concentration of the more volatile constituent, the rate is determined by the rate of diffusion of the evaporating metal, to the surface of the melt. Cadmium, zinc, magnesium, and tellurium were found to volatilize readily from both lead and tin. Tellurium appears to volatilize as an intermetallic compound rather than the pure metal. Antimony could not be removed from lead at 1,000° C.; the condensate was nearly all lead. Antimony, bismuth, and lead were removed from tin.

Jan 1, 1960

By J. Intrater, E. S. Machlin

In a study of grain boundary sliding in superpure Copper (99.999 pct),&apos; bicrystals of a specific shape were used, Fig. 1. That shape was adopted in order to minimize the deformation of grains on both sides of the boundary due to clamping. Another requirement was to obtain bicrystals with a rnicroscopically straight boundary, Fig. 2. Single crystals of predetermined orientation (growth axis parallel to <310>) were grown in a graphite mold from seed crystals. The apparatus for growing single crystals consisted of a vacuum system, argon purification train, vycor tube (in which a graphite mold was placed), a carriage for the induction coi1,and a Lepel (7-1/2 KW) high-frequency converter. The graphite mold was heated by induction and the charge in turn was heated by conduction. The induction coil was moved by means of a motor at a speed of 1 1/2 in. per hr. Single crystals of two different orientations were grown from the melt in one-half of a split graphite mold, Fig. 3(a). Two such crystals were then placed in contact with each other in another split mold, Fig. 3(b) using tapered inserts. The pair of crystals was then remelted starting 2 in. from the top to insure that the whole top portion of the crystals was maintained molten. By moving the induction coil

Jan 1, 1960

By Douglas Castleberry

The degree of fragmentation obtained in primary quarry blasting has always been a factor in the speed of digging&apos; the muckpile This paper will discuss a case history of increased production and associated lowered costs from increased fragmentation. The quarry under discussion is fairly new, located in Georgia, and is in the large operation .category. Loading is done by three yard shovels, and, primary crushing by a 48" x 60" haw crusher preceded by a 5&apos; wide feeder. The stone is a hard granite gneiss, of Los Angeles rating 22, and apparent specific gravity is 2.68. The product is shipped to points in that state for railroad ballast, concrete aggregate, and road building stone. Inasmuch as fairly large shovels and a large Jaw were to be utilized, initial drilling and blasting were pointed toward producing fairly large sized muck for this large equipment. This was following a concept somewhat in vogue for some years in the Southeast wherein many large equipment plants would tend towards larger fragmentation, and smaller equipped plants would conversely tend toward attempts at smaller sized rock piles for smaller shovels and crushers.

Jan 1, 1960

By A. S. Yue

It was deemed desirable to obtain an understanding of the vacuum desulfurization process. McKechnie1 has reported that the sulfur content of nickel- and cobalt-base alloys is reduced in vacuo. Keverian and Taylor2 have observed that vacuum melting causes desulfurization of iron-carbon-silicon alloys. Garnyk and samarin3 have desulfurized transformer steel by vacuum treatment. Experiments were conducted in order to investigate the desulfurization of liquid iron under reduced pressures, and to establish the effect of some alloying elements, and various crucible materials. A vacuum-induction furnace of 50-lb capacity was used. The charge was Armco iron. Silicon was added as 90 pct ferrosilicon, carbon as electrode graphite, and aluminum as high-purity aluminum metal. Magnesia and silica crucibles were used, their inside diameters were 5 1/2 and 5 3/8 in., respectively. The temperature was measured with an optical pyrometer and it was held at 1600 1 15°C. Samples were withdrawn with quartz tubes of 6 mm ID, without disturbing the furnace atmosphere. Pressures were measured with an alphatron gage. The experimental results are shown in Fig. 1. They indicate that: 1) Sulfur can be removed from liquid iron alloys by vacuum treatment; 2) The desulfurization is enhanced by the presence of silicon, carbon, and aluminum, all these elements increase the activity of sulfur dissolved in liquid iron;4 3) The pronounced effect of silicon indicates that probably a volatile silicon sulfide is formed, Alcock and Richardson5 have observed a similar phenomenon; 4) The same rate of desulfurization was obtained when the metal was contained in either magnesia or silica crucibles. Dr. J. Keverian has contributed many discussions and recommendations. M. S. Sutliff has helped in conducting the heats. The permission of General Electric Co. for this publication is gratefully acknowledged.

Jan 1, 1960

By James A. Barr

Phosphate rock is a natural rock containing one or more phosphate minerals usually calcium phosphate, of sufficient purity and quantity to permit its use, either directly or after beneficiation in the manufacture of commercial products.1 The principal minerals in phosphate rock have the apatite structure which may be represented by the type formula: Ca10(X2) (PO4)6 where X represents the hydroxyl group (OH), chlorine or fluorine, either singly or collectively. The calcium may be partly replaced by sodium, magnesium, and other positive ions such as manganese, strontium, lead, uranium, cerium, yttrium and other rare earths. The PO4 radical may be partly replaced by small quantities of UO4, AsO4, SiO4, CO3, SO4, or Vo4. A typical commercial rock is usually a calcium phosphate containing 3 to 4 pct fluorine, the major impurities being limonite or other iron oxides, clay, aluminum phosphates and silica as quartz sand. A little vanadium is present in most of the domestic rock deposits (except the Tennessee Brown Rock), according to Jacob, Hill, Marshall and Reynolds! A little uranium occurs in the Florida leached zone, as will be brought out later. The chemical analyses are reported as P205, or tricalcium phosphate Ca3(PO4)2, the latter often designated by the trade name BPL (bone phosphate of lime). Commercial analyses usually report iron and alumina as oxides, lime as CaO and silica or insoluble. Colony3 examined many samples of apatite, staffelite, dahlite and American phosphorites and concluded that all have identical X-ray diffraction patterns. The phosphates in the phosphate rock have very minute crystalline structures. The mineral apatite Ca3(F.Cl) (PO4) 3 is the principal primary source of the element phosphorus, and occurs widely distributed in igneous rocks but rarely in a minable mass. Only about 12 pct of the world production of phosphate rock comes from primary apatites; the remainder is derived from secondary phosphorites. These phosphorites have been formed by the alteration of sediments by solutions containing phosphoric acid. Such solutions have come from the weathering or leaching of igneous rock containing apatite, bone deposits of prehistoric animals, marine life or guano deposits. These phosphorites are mostly alterations of phosphatic limestones. The sedimentary phosphate deposits are of marine origin and may have been enriched by subsequent solution of the more soluble calcium carbonate by waters containing carbon dioxide, by physical concentration by wave action, and by redeposition of the dissolved phosphate ions. Uses of Phosphate Phosphorus is the spark of life and is the structure builder and one of the main elements of plant food (fertilizer). Without phosphorus, life cannot exist. A "complete" plant food[t] in addition to phosphorus compounds contains potash, which acts as a catalyst to convert nutrients to useful forms, nitrogen to supply the growth element and many minor elements. The cycle of supply of phosphorus is from the apatite to solution and soil, absorption of plant life, decay and return to the soil or by animal life feeding on the plants. With insufficient supply of phosphorus in vegetation, life is not prolific. If crops are removed from

Jan 1, 1960

By Robert W. Smith

Computation of the thermodynamic properties of the reaction products in the deflagration of explosive gas mixtures has been a most valuable guide regarding the possible kinetic mechanisms of homogeneous combustion processes. Knowledge of the physically possible end states is indispensable for understanding observed deviations from equilibrium in heterogeneous combustion. However such information on dust flames is entirely lacking. To complement a Federal Bureau of Mines study of stationary graphite dust flames burning in pure oxygen,6/ this report gives examples, at atmospheric pressure and room temperature, of composition profiles in an idealized oxygen-dust flame, with both mass and enthalpy being preserved. Similar profiles can be obtained from the data of the paper for elevated temperature and pressure.

Jan 1, 1960

By S. Weinig, J. Winter

The grain boundary adsorption of solutes as a function of bulk concentration and solution temperature was studied using internal-frictimz techniques. From the variation of the cor-responding energy of activation for the Phenomenon, the inter-actior2 energy between a solute atom and a high-angle boundary was calculated. Interaction energies in the range of 0.3 ev were obtained, and were used to obtain the actual concentration of solute at the grain boundary. In corroboralory creel, studies the direct grain boundary contribution to the total creep strain was measured. It was found that the interface creep varied with the type and magnitude of the solute adsorbed. Subscribing to the theory of their being energetically favorable sites at the grain boundary for solutes of both Positive and negative size deviations, ternaries were investigated in Which solutes of both types were present. A marked increase in the resistance to grain boundary creep was manifested. THE major difficulty which has been encountered in investigations of the grain boundary segregation of solutes has been the lack of a sufficiently sensitive method of measuring the amount of adsorbed solute at the boundary. For the general case of a high-angle boundary, no direct method of measuring the adsorption at the boundary has been found to date. Internal friction has been used in several studies of grain boundary adsorption1-3 and although it is somewhat indirect, it was demonstrated to have the necessary sensitivity. In this investigation the authors have used internal-friction techniques in conjunction with a study of the grain boundary contribution to the total creep strain. As both parts of the investigation were performed on the same specimens it was possible to combine a highly sensitive technique with a somewhat more direct method in order to obtain information about the adsorption phenomenon. From internal-friction studies the rate of increase of the activation energy was observed to be a function of the difference in size between the solute and solvent atoms. It was proposed that if Gibbs&apos; adsorption isotherm is considered, i.e., where r is the excess solute at the boundary, c is the bulk concentration, and ay/ac is the change in grain boundary energy with bulk concentration, then AH b/ac must vary in the same way as ay/ac and therefore In this way a relative measure of the grain boundary adsorption of solutes is directly obtainable from in-ternal-friction studies. If the previous work in the field of grain boundary adsorption of solutes is examined, certain apparent information is desirable if the phenomenon is to be understood. The most important questions that must be asked are as follows: 1) Is the adsorption of solutes at the grain boundary an equilibrium process? 2) Can the Mott model of the grain boundary be used as a basis of setting up an elastic interaction between the grain boundary and solute atoms? 3) Is it possible to obtain an exact measure of the excess solute at the grain boundary as a function of temperature and bulk concentration rather than merely a relative measure of the adsorption 4) Are the conclusions obtained from an indirect method such as internal-friction studies meaningful in considering gross grain boundary effects such as creep? EXPERIMENTAL PROCEDURE The material used in this investigation was Bureau of Mines "superpurity" titanium (79 Bhn—1500 kg

Jan 1, 1960