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By W. T. Swensen

The Anaconda Company, through its wholly owned subsidiary The Anaconda Company (Canada) I,td., has investigated, optioned and partially developed a large tonnage of iron ore amenable to magnetic concentration. The reserves are located in north central Ontario and occur within a twenty-two mile belt of layered and intricately folded metamorphic rocks, close to the north contact of an igneous complex of granite and pegmatite. There are two main ore deposits. Briarcliffe is a steep to vertically dipping body 100 to 500 feet wide and over a mile long. The Two Mile Lake deposit is flat dipping and confined to an open, asymmetrical syncline; it is approximately a mile wide and 250 to 4.00 feet thick. On its flat easterly plunge, it is saucer-like in shape and is amenable to open-pitting for an east-west distance of several thousand feet. Magnetometer surveys, confirmed by drilling, indicate at least a three mile eastward extension of this deposit. Location and Access: The property is located in the Kowkash Mining District of northwestern Ontario, roughly forty-four miles north of the community of Nakina on the main line of the Canadian National Railroad. (Fig. 1) Access during the exploration period was entirely by airplane from Nakina. (Fig. 2) More recently, Nakina itself was connected to the highway network in the Longlac-Geraldton area. The property is roughly 190 miles by existing and proposed railroad from the Great Lakes waterway system. The Trans-Canada pipeline moving natural gas from western to eastern Canada passes through Geraldton roughly 70 miles south of the property. Topography: The surface features in the area are typical of a sizeable portion of the Precambrian Canadian Shield area. Many lakes, low swampy areas, and glacial moraine-type features are common in this recently glaciated area. The average elevation is between 800 and 900 feet above sea level, and the relief is probably less than 100 feet with the greater portion of the area less than 50 feet. The topographic "highs" are formed either by outcrops that were resistant to glacial erosion or by moraines, eskers and drumlins which were deposited upon the recession of the glaciers. The better mineralized zones, composed chiefly of quartz and magnetite, commonly form ridges resistant to erosion and weathering. Previous Work: Because of the obvious outcrop of the magnetite-rich beds and knowledge gained from early developments within the general region, it is conceivable that the presence of the iron formations has been known for a good many years. The area is included in studies made by L. F. Kindle* in 1929 and 1930 for the Ontario Department *Kindle, L.F., Kowkash-Ogoki Gold Area, Ontario Department of Mines Annual Report, Vol. XL, Part IV, 1931; map 40f

Jan 1, 1961

By David M. Gullikson

As part of its program of petroleum production research the Federal Bureau of Mines has long been engaged in the study and development of systems of analysis of oilfield waters (8, 12, 20, 21, 22, 27, 30).21 However, many of the early chemical procedures developed by the Bureau and widely adopted by the petroleum industry are time consuming, and some are unreliable for determining certain constituents found in California oilfield waters. Because of the need for more rapid and more accurate methods having greater sensitivity with low concentrations of some constituents, a study has been made by the Bureau's Petroleum Research Laboratory at San Francisco, in developing new techniques and modifying previously published techniques for analyzing oilfield waters by flame spectrophotometric, potentiometric, and colorimetric methods. Test solutions were synthesized for testing the suitability and accuracy of the procedures, and the effect of interfering ions. These solutions contained known quantities of characteristic constituents of oilfield waters including sodium, magnesium, potassium, calcium, lithium, strontium, barium, sulfate, chloride, bromide, iodide, carbonate, bicarbonate and borates in a wide range of concentrations. The compositions of these synthetic brines are listed in table 22. Many California oilfield waters contain salts of petroleum-derived organic acids and several synthetic oilfield waters also were prepared to which large quantities of naphthenates or salts of petroleum acids were added.

Jan 1, 1961

By J. P. Capp

The Federal Bureau of Mines and the Alabama Power Company conducted an experiment in underground gasification of coal at Gorgas, Ala. involving the use of hydraulic fracturing to increase the air acceptance of a coalbed for the introduction of combustion air and removal of product gases. Air acceptance is defined as the flow rate of air which can be injected into the coalbed at 65 p.s.i.g. This was the second time the hydraulic-fracturing technique was used at Gorgas. Sand suspended in a heavy oil served as the fracturing fluid in the first experiment; in the second the sand was two to six times larger and was suspended in a water-starch gel. In addition to providing further tests of the underground-gasification process, the purpose of the second experiment was to determine the effects of the larger sand and greater volumes of a water-base fluid on (1) the extent of the fractured area, (2) the air acceptance of the coal, and (3) the rate at which a gasification path could be carbonized (linked) through the coal, and to compare these results with those of the first experiment. The coal was fractured by injecting 11,000 lb. of sand and 33,580 gal. of water and water-gel at 200 to 600 g.p.m. and 900 to 1,000 p.s.i. The fluid fractured the coal and the sand served as a propping agent to hold the cracks and crevices open. Pressures during the fracturing operation at test boreholes indicated that the fracturing fluid extended only about 150 ft. from borehole H, the point of application of the fracture. Injection of air revealed that the air acceptance of the coalbed within this e t was materially increased. On the other hand, increased air acceptance also was noted at boreholes up to 280 ft. from borehole H and at the electrolinking area 300 to 400 ft. away, indicating that the fracture effects extended considerably farther than was evident from observation. Similar effects were noted at approximately the same distances after the first hydraulic fracture.

Jan 1, 1961

By J. L. Gillson

Joseph H. Birman (Chairman, Dept. of Geolcgy, Occidental College, Los Angeles, Calif.) Many thanks to J. L. Gillson for so comprehensive a survey of the titanium sand deposits of the world. Over the past two years, the writer studied rather carefully some of the Cretaceous ilmenite deposits in New Mexico and Colorado, including the Sanostee deposit shown in Gillson' s map, Fig. 6. The deposits were geologically mapped and sampled, surveyed by magnetometer, and the Sanostee deposit was drilled. Moat of the genetic interpretations made by Gillson concerning the recent sedimentary ilmenites can be clearly read in the Cre-taceous deposits in New Mexico. The deposits are in marine regressive members of the Mesaverde group. The deposits trend within a few degrees of N 55° W and persistence of this trend through both distance and time (the deposits are in different members of the Mesaverde group) implies that the deposits are offshore bar accumulations. Heavy mineral content ranges from about 10 pct to more than 50 pet. Thicknesses are from 4 ft to as much as 20 ft, widths range from 150 to 600 ft, and lengths range from a few thousand feet to a few miles. All are locally or completely overlain by carbonaceous shale and thin coal. The deposits are strongly altered, and from X-ray diffraction the principal titanium alteration product appears to be anatase. Drilling of the Sanostee deposit shows that the alteration is not related to the present erosion surface but took place at the site of deposition and before burial by the overlying sediments. Iron oxide derived from the alteration cements the grains and is the chief coloring agent in the immediately overlying shales. In the Sanostee deposit, there is virtually no feldspar, the gangue mineral being almost exclusively quartz. Sorting is excellent, but the quartz grains are subangular to angular. Petrographic examination reveals that the angularity is not due to overgrowths. Therefore, short distance transport is implied. The mineralogical composition suggests a low relief granitic terrane as the source area. Feldspar may have been decomposed by weathering at the source, but an alternative preferred by the writer is that each of the deposits represents a long-term concentration site (for example a large sand bar) which was continually being deprived of light minerals by wave action and selective transport. Feldspar may have been mechanically reduced in size more quickly than the quartz, and thus its rate of removal may have exceeded that of quartz. Concentration of heavy minerals would thus occur until the marine regression removed the zone of maximum wave energy from the site. Chemical alteration would then become the most important process until burial by encroaching swamp deposits.

Jan 1, 1961

By Murray Jacobson

Data obtained by the Federal Bureau of Mines on the dust explosion hazard in air are presented for 220 samples of agricultural products. Information is given on ignition temperature of dust clouds and layers, minimum explosive concentration, minimum electrical energy for ignition, explosion pressure and rates of pressure rise, amount of inert dust required to prevent flame propagation, and, in a few instances, the permissible oxygen concentration in an atmosphere to prevent ignition by spark and by heated surface. The effects of particle size and source of sample on explosibility are shown. The relative ignition sensitivity, severity of explosion, and overall explosibility of the materials are characterized by empirical indexes. This report contains Ma obtained by the Bureau in laboratory studies on the explosion hazards of agricultural dusts. Recognition of the dangers will encourage adoption of adequate measures to prevent ignition and explosion during preparation, processing, and utilization of the materials. Agricultural products constitute one of the largest groups of materials used in America. More than 260 million tons of various grains, much of which now exists in dust form, was grown in 1958.6/ Over 600,000 tons of the annual production of 200

Jan 1, 1961

By W. L. Hunter

The research on this report was conducted to obtain information on the feasibility of producing ferro chromium of varying silicon and carbon contents from domestic chromite. Concentrates from the Mouat deposit were chosen because they typify the chromite found in the Stillwater complex, the largest domestic reserve, and are similar in composition to other extensive North American and foreign deposits. Batch-smelting tests designed to produce high-, medium-, and low-carbon ferrochromium were made in single phase and three-phase, electric-arc, steelmaking furnaces. Agglomeration studies were made in a rotary kiln. Continuous smelting tests were made to yield data on the production of high-carbon ferro chromium and low-carbon ferrochromium-silicon. The carbon content of high-carbon ferrochromium was lowered to the medium-carbon range by oxygen injection. Mouat stockpile concentrates were nodulized in a gas-fired rotary kiln using quartz, limestone, and fluorspar additions in the proportion necessary to flux the slag. The nodules were smelted in a continuous test using coal, coal char, and mixtures of the two consecutively as reductants.

Jan 1, 1961

By Eugene T. Sheridan

The Bureau of Mines annually canvasses the fuel-briquet and packaged-fuel producers in the United States and publishes economic data on these industries, based upon reports submitted voluntarily by producers. This publication lists all producers that reported commercial production to the Bureau for 1960 and presents data on individual plants. The companies named herein represent virtually all producers of processed minerals fuels. A few small plants may not have been canvassed or failed to respond to the survey because some of the smaller plants operate intermittently and the survey is voluntary. All plants that reported commercial production were included; regardless of size. Specifically excluded were plants that manufactured briquets from wood charcoal. Fuel briquets and packaged fuel are manufactured solid fuels, produced by mixing fine-sized mineral fuels with binding materials and compressing into small individual shapes, Briquets are produced in pillow-shaped and cylindrical form, are 2 to 4 inches long, and weigh 2 to 4 ounces. Packaged fuel consists of 3- or 4-inch cubes; 6 or 8 of which are wrapped together in heavy kraft paper to form a package weighing 10 to 15 pounds, Briquets are durable and may be stored and handled as bulk fuel; packaged fuel breaks easily and must be stored indoors to prevent it from deteriorating. Whereas briquets are consumed in many areas as a general residential fuel, packaged fuel is more of a specialty item, used at times to supplement other fuels. Packaged fuel is burned without re-moving the paper and is referred to as the "white glove" fuel.

Jan 1, 1961

[James C. Gray, President W. B. Stephenson, President-Elect A. B. Cummins, Past-President E. G. Fox, Eastern Regional Vice-President H. C. Weed, Western Regional Vice-President Donald W. Scott, Central Regional Vice-President John Cameron Fox, Secretary 29 W. 39 Street New York 18, N. Y. After September 7, 1961 345 East 47 Street, New York 17, N. Y. D. R. Tone, Assistant Secretary Nathaniel Arbiter, Treasurer]

Jan 1, 1961

By F. W. Wessel

Manganiferous carbonate slates of the Cuyuna range, which are part of the unoxidized thin-budded iron formation, represent a large potential source of manganese. This report details recent bench-scale research by the Federal Bureau of Mines in applying mineral-dressing techniques to these materials in order to investigate their potential uses. Work outlined in the report was directed toward the production of concentrates usable as iron-blast furnace feed, but an equally important objective might have been to furnish an enriched feed for extractive processes for recovering manganese. Flotation concentrates were prepared that contained 11.1 percent manganese, 27.8 percent iron, and 12.2 percent silica, with recoveries of 73 percent of the manganese and 48 percent of the iron. Calculated analysis for a simulated sinter suggests a product containing 16.0 percent manganese, 40.2 percent iron, and 17.6 percent silica, with 31 percent recovery of the dry weight of the ore. The silica in the flotation concentrates was due to quartz and iron silicates. Substantial quantities of the iron silicates (stilpnomelane and smaller amounts of minnesotaite) were present in the slate, and the need to reject these minerals limited the recovery of iron. The sintered flotation concentrate would be usable as ferruginous manganese ore for iron blast-furnace feed because of its favorable manganese silica ratio. The unsintered flotation concentrates, representing 45 percent of the feed weight and containing manganese enriched in the ratio of 1.6 : 1, also could be used as feed to processes for extracting manganese.

Jan 1, 1961

By W. L. Phillips

The plastic properties of lithium fluoride and magnesium oxide under compression were investigated in the temperature range 25° to 1000°C. At the higher test temperatures, the critical resolved shear stress and the rate of work-hardening of both materials decreased. At the same time, the number of stress lines decreased and the individual stress lines became wider. The density of dislocations decreased for a given strain the higher the test temperature for lithium fluoride. The decrease in the critical resolved shear stress as a function of temperature could be fitted by the equation 7 = Toe-KT. THE influence of temperature on the stress-strain curves of a variety of metal single crystals has been studied for a wide range of temperature.1"5 In general, it has been found that both the critical resolved shear stress and the rate of work-hardening decrease rapidly with increasing temperature and fall to a value of essentially zero well before the melting point is reached. AS the test temperature is increased, the density of slip lines has been found to decrease, while the width of the individual lines increases. Recently, Gallagher,' Graf et al.,7 and Pate1 and Alexander8 have found that single crystals of germanium and silicon, which have a covalent bond, can be plastically deformed at elevated temperatures. In compressing germanium it has been found that the strain-hardening coefficient decreased very rapidly as the temperature was increased. The coefficient did not tend to zero, however, as the melting point was approached. The plastic properties of ionic crystals at elevated temperatures have not been extensively investigated. In the only work previously reported Tamman and salge9 and Theile10 have shown that the yield point of sodium chloride single crystals tested in tension and compression decreased slowly with increasing temperature, falling to zero at the melting point. As the temperature was increased, they found a substantial increase in the amount of plastic deformation that could be sustained before fracture; and at temperatures above 400°C in tension tests there was an obvious necking which produced local extensions of up to 3000 pct. The purpose of the present work is to extend the knowledge of high-temperature deformation to the ionic crystals, lithium fluoride and magnesium oxide. The following were investigated: 1) The gross shape of the stress-strain curve at several temperatures. 2) The change in the critical resolved shear stress as a function of temperature. 3) The appearance of slip bands and the density of dislocations as a function of strain and temperature. EXPERIMENTAL TECHNIQUES The lithium fluoride and magnesium oxide used in this investigation were purchased from the Harshaw

Jan 1, 1961

By W. E. Dunn

CHLORINATION of titanium ores and slags is the source of TiCl,4 intermediate between ore and metal. A number of chlorinators are operating in the United States using a wide diversity of ores. These chlorinators vary in design to accommodate the ore source, but all use chlorine and carbon.

Jan 1, 1961

By R J. Tremblay, R. R. Hoffman

This paper deals with materials of construction and problems encountered and overcome in leaching and filtration of oxidized sulphuric acid slurry in the Port Radium mill after eight years of operation. The slurry is characterized by a high calcium sulphate content as well as a high chloride level under oxidized conditions, both of which affected initial design and subsequent changes. Leach agitation tanks are of wood with a mild steel superstructure and stainless steel agitator and moving parts below solution level. Electro-polished 316 stainless steel cooling coils are used for temperature control of the slurry. The string filters are of the Oliver type with wood decking. Extensive use is made of wood, Linatex lined mild steel and stainless steel for the slurry handling. A typical analysis of the slurry solution follows:(pH-1.30) ClOa Fe+++ Free Acid UaOs c1-so.--0.10 gms/litre 10.2 gms/litre 6. 7 gms/litre 3.5 gms/litre 2.0 gms/litre 155 gms/litre

Jan 1, 1961

By K. C. Li

The scope of this subject is a broad one. The demand for a metal with high refractory properties, great strength at elevated temperatures and high nuclear cross section, has put tungsten in the foreground as: the most promising metal to fill some of these requirements. Recently developed techniques have made it possible to roll large tungsten sheet and-the availability of fabricated tungsten is already upon us. More and more, the demand is for purer and still purer metals. Tungsten is no exception. As technology improves, we are learning more about the effect of foreign elements in minor amounts upon the chemical and physical properties of metals. As equipment and technology improve, specifications become more rigid, and reasonably so. Pure metals have revealed properties hitherto unknown in metals produced by former technology.

Jan 1, 1961

By W. M. Deaton

The Keyes Helium Plant of the Federal Bureau of Mines was constructed under an expedited schedule, to supply the urgent and growing demand for helium in atomic energy, missiles, aerology, space exploration, shielded-arc welding, and low-temperature research. Construction began in December 1958 and ended in August 1959. The plant, near Keyes, Okla., processes 2 percent helium-bearing natural gas from the Keyes gasfield. In 1960 the plant produced and shipped 263 million cubic feet of helium (equivalent to an annual rate of 290 million cubic feet). Production cost was $9.11 a thousand cubic feet of helium. A low-temperature process involving two steps is used; the first separates a crude-helium product from the natural gas at about -250° F. and 225 pounds per square inch gage (p.s.i.g.); and the second purifies the crude helium to a high-purity product (Grade-A helium, 99.995 percent helium) at about -320° F. and 2,750 p.s.i.g.

Jan 1, 1961

By D. P. Seraphim

Single crystals of bee Li-Mg solid solution were grown and their internal friction was measured as a function of temperature, A peak of the Zener type was found in the damping spectrum. The activation energy for the relaxation process is 21.5 ± 1 kcal per mole and the frequency factor is 1015.7 ± 0.7 sec-1. ZENER internal-friction peaks which are observed for a wide range of solid solutions are attributed to stress-induced changes in local order.' In the present work a Zener internal-friction peak, the first reported for a solid solution of an alkali metal, is

Jan 1, 1961

By H. H. Klepfer, M. E. Snyder

UNTIL very recently, the commercial availability of the rare earths as metals has been very limited. Fabrication of mill products from these metals has not been studied in most cases. This note reports the results of the development of fabrication techniques for thulium. Thulium has a melting point of about 1550°C and a hexagonal close-packed crystal structure. It oxidizes in air to give a black oxide (TmzO,). The procedures for producing thin thulium foil were developed on one ingot weighing about 220 g and were subsequently applied in processing about a pound of metal to foil. Several alternates for the various fabrication steps were investigated and will be discussed. The metal fabricated was in the form of commercial chill-cast ingots 1 in. in diam and 2 in. long weighing approximately 220 g. Impurities in the ingots were reported by the vendor to be 4000 ppni tantalum, 2000 ppm calcium, 200 ppm nickel, 100 to 200 ppm iron, 100 ppm europium, and less than 100 ppm copper, lutetium, and ytterbium. In addition to these impurities, several salt-like inclusions as large as l/8 in. in diam were revealed along the center line of the one ingot sectioned. Preliminary tests indicated that small wafers cut from the as-cast ingot would not fabricate readily by rolling. Forging of copper-jacketed wafers was therefore attempted. At 1550"F forging was satisfactory but an apparent reaction of copper with thulium demanded investigation of lower temperatures. Therefore, the remainder of the test ingot was forged at 1450°F—with only minor cracking. All ingots forged were inserted into copper tubes of 1 in. 1D and 0.125-in. wall thickness. The jackets were sealed by flattening the ends of the tubes and welding under helium. Heating time at 1450°F was 30 min. Press forgings of 1/8 in. per pass were used, followed by 10 min reheats. When the ingots had been squared and reduced to 0.250 in. in thickness, the original copper jacket was stripped off and replaced by a new jacket in preparation for hot rolling. Hot rolling at 1450" F without edge cracking was readily accomplished after forging. Excellent results were obtained with 10 pct reductions of thickness followed by 5 to 10 min reheats. After reduction of thickness from 0.250 to 0.100 in. the copper jacket was removed. It was found, in fact, that hot rolling in air was possible. A tenacious black oxide similar to that seen on zirconium was formed during 3 min reheats at 1450°F. Reduction in air to 0.010 in. foil was possible taking 10 pct reductions per pass. The oxide coat formed during hot rolling in air could best be removed by sand blasting and pickling. Common pickling solutions containing polar solvents were found to attack the metal too rapidly and a concentrated nitric-hydrofluoric acid mixture attacked neither the oxide nor the metal. The most satisfactory pickling solution was 52 vol pct concentrated nitric acid-48 vol pct glacial acetic acid. After forging to 0.250 in., vacuum annealing and cold rolling was found to be another satisfactory alternate to hot rolling in copper jackets. After forging. a hardness of Rockwell B76 was found. Annealing in vacuum (2 X l0-5 mm of Hg) for 1 hr at 1200"F did not alter this value. Annealing at 1470"F for 1 hr brought the hardness down to R;]63. With cold rolling (5 pct per pass) the hardness returned to about R,1:76 after 20 pct reduction and edge cracking became noticeable. However, cold rolling to a total of 40 pct reduction in thickness (RI,,83) was possible before edge crack propagation became serious. Good surface finish was obtained, and the metal loss due to oxidation was minimized by cold rolling and vacuum annealing. Using this procedure the yield of 1.25 in. wide by 0.010 in. thick foil from a 1-in. diam ingot was about 40 pct.

Jan 1, 1961

By William J. Orlandi

The intent and scope of this paper is to present to you, as concisely as possible, the problems and requirements -- and what we consider advantages -- of all-belt haulage in a modern underground coal mine. Mine No, 10, at Pawnee, Illinois, was opened in 1951; consequently, all the planning and consideration given to haulage selection was based on information then available and on Peabody Coal Company? s experience to that date,

Jan 1, 1961

By James S. Browning

The purpose of this investigation was to develop a dependable and economic method for recovering spodumene and mica from pegmatites of the type found in Gaston County, N. C. Laboratory batch tests and continuous flotation tests were made by the Federal Bureau of Mines to determine the feasibility of treating the ore by flotation to recover high-grade spodumene and mica concentrates. The spodumene flotation circuit yielded concentrates containing 6.50 percent lithia (Li20), with an overall recovery of 81.8 percent of the lithia in the ore, The mica circuit yielded concentrates containing 97.5 percent mica, with a recovery of 82.5 percent of the mica in the spodumene tailing.

Jan 1, 1961

By O. K. Riegger, L. H. Van Vlack

The median angle of relatively few two-dimensional observations provides a satisfactory value for dihedral angle determinations. Those data that contain bimodal or non-equilibriated dihedral angle distributions are readily detected. THIS paper is concerned with a statistical simplification for determining dihedral angles in solids. Microstructures are partially controlled by relative energies of interphase boundaries and grain boundaries. smith1 has shown rather conclusively that such boundaries may be equilibrated to give a vectorial balance at grain and phase edges. Thus if an accurate measurement is made of the dihedral angle associated with grain and phase edges, an accurate calculation of the relative energies may also be made. The accurate measurement is difficult because the dihedral angle involves two planes in three dimensions, and only a two-dimensional cut through the dihedral angle is usually observed. Such a two-dimensional cut is statistically random provided there is no preselection or orientation. Harker and parker2 have shown that the mode of the frequency distribution of observed angles is within 5 deg of the true angle if the true dihedral angle is 120 deg. smith1 had calculations made to show that the same generalization could apply to dihedral angles of 30, 60, 90, and 150 deg. This procedure of requiring the determination of the statistical mode is time consuming because experience has shown that more than 200 angle observations are necessary before the mode is clearly indicated. It is possible to determine the dihedral angle with equal accuracy with only 25 angle observations if the median angle is used in place of the mode angle. Use is made of Harker and parker's2 basic equation tan =2 sin x cos

Jan 1, 1961

By C. G. Dunn, J. L. Walter

Secondary recrystallization to the (110) [001] texture in high-purity silicon iron occurs if low-oxygen material is annealed in a nonoxidizing atmosphere. Any departure from these conditions results in a growth of (100) oriented grains. The nature of the matrix and secondary recrystallization structures and textures and the nature of grain boundary interactions during growth show that the low gas-metal interfacial energy of the (110) surfaces provides the driving force for growth of these grains. A type of grain growth, characterized by a driving force which derives from energy differences of {hkl} surfaces at the gas-metal interface, has been treated in recent papers.&apos;-7 Secondary recrystallization to the cube text!:: in high-purity silicon iron provides one example. The present paper also deals with a surface energy driving force but the texture that results by secondary recrystallization is not the cube texture; it is a texture in which the (110) plane is in the plane of rolling and the [001] direction is in the direction of rolling. The phenomenon described in this paper is different from the impurity (dispersed phase)-controlled secondary recrystallization process in which the (110) [001] oriented grains grow under the action of grain boundary driving forces.8-12 It is also different from tertiary recrystallization,2 which also produces the (110) [001] texture in high-purity silicon iron, since the matrix textures and grain sizes are different. Finally, it is unlike any other form of secondary recrystallization reported in the literature. The possibility of obtaining the (110) [001] texture in high-purity silicon iron became clear in a study of the effect of impurity atoms on the energy relationships of (100) and (110) surfaces. In this study Walter and Dunn6 observed the migration of (100)/(110) boundaries, i.e., boundaries between two grains, one of which has a (100) plane and the other a (110) plane, respectively, parallel to the plane of the sheet specimen. At 1200°C the (100)/(110) boundaries advanced into (100) grains in a vacuum anneal, then reversed their direction and migrated into (110) grains in a subsequent anneal in impure argon. Finally, the direction of migration reversed once again with (110) grains growing into (100) grains in a second vacuum anneal. These results were explained in terms of a change in concentration of oxygen atoms at the gas-metal interface during the anneals. Thus, oxygen atoms were added to the surface during the anneals in impure argon to the point where ?100, the specific surface energy of the (100) oriented grains, was lower than ?110, the surface energy of (110) oriented grains. In vacuum, however, the oxygen concentration at the surface was lowered to the point where ?110 < ?100. Concerning the possibility of secondary recrystallization in high-purity silicon iron with a low initial oxygen concentration, the observed effect of adsorbed oxygen atoms has indicated6 that a good vacuum anneal would favor the rapid growth of matrix grains with the (110) plane in the plane of the sheet much more than grains in the (100) orientation. The growth of only (110) oriented grains of course would depend upon y110 being less than ?hkl, where hkl refers to any plane different from (110). The present paper is concerned with the application of the above ideas to secondary recrystallization to the (110) [001] texture in high-purity silicon iron. The matrix and secondary recrystallization textures and structures are defined and discussed. Observations of growth of nuclei for secondary recrystallization and of boundary interactions are included to provide direct information on the surface energy relationships between (110) and other (hkl) surfaces. EXPERIMENTAL PROCEDURE As before, 2,4-6 high-purity iron and silicon were melted and cast in vacuum to provide an alloy containing 3 pct Si with less than 0.005 wt pct impurities. The oxygen content of the ingot was lower than in previous ingots, being approximately 3 ppm (by weight). The carbon content of this ingot may have been slightly higher than was found for previous ingots. The same rolling and annealing schedule used previously2 was followed in this study to obtain samples 0.012 in. (0.3 mm) thick. These samples were electropolished prior to annealing. After rolling and polishing, the oxygen content of the material was approximately 6 ppm; material used in the previous studies contained about twice this amount of oxygen.

Jan 1, 1961