Search Documents

By T. A. Evans

The Bureau of Mines conducted a Laboratory and pilot-plant investigation of the flotation of iron sulfides from zinc-lead mill tailings near Platteville, in south-western Wisconsin, at the North Central Experiment Station, Minneapolis, Minn. The procedures used and the results obtained in this investigation are described in this report. Samples for laboratory tests were obtained from each mill in the district, namely, Calumet & Hecla, Inc., Eagle-Picher Co., Vinegar Hill Zinc Co., and Tri-State Zinc, Inc. The sample fat pilot-plant work was obtained from the Davis Mining Enterprises mill.

Jan 1, 1957

By Miro Mihelich

The mines and prospects in the vicinity of Landlocked Bay, 25 miles southwest of Valdez, Alaska (fig. 1), were examined, mapped, and sampled in July and August 1955 as part of a comprehensive investigation by the Bureau of Mines of ore deposits adjacent to Prince William Sound. The purpose of the investigation is to establish and record the location, nature, extent, and metallurgical characteristics of copper and associated metallization in the Prince William Sound district and to indicate, if possible, those areas in which additional exploration and development may be justified. Of particular interest are the possibly numerous deposits of massive iron sulfides that were neglected during early mining operations. These deposits may constitute important reserves of sulfur and iron. At Landlocked Bay deposits of copper-bearing iron sulfide minerals have been mined or partly explored through mine workings, which are in a zone about 1 mile wide along the western side of a large overthrust fault known as the Landlock Overthrust. Eight of the principal mines along this zone were examined end sampled. Although only three of the mines have a recorded production of shipping-grade copper ore, all have deposits of copper-bearing iron sulfide minerals that are similar in occurrence. The deposits occur as lenticular masses and disseminations of chalcopyrite, pyrite, and pyrrhotite which replace crushed rock or fill cavities along shear zones in greenstones and in sedimentary rocks that are exposed between sea level and an altitude of 2,500 feet. These lenticular masses of sulfide minerals range in size from small pods to ore bodies that have been stoped to maximum widths of 9 feet, strike lengths up to 70 feet, and dip lengths as much as 350 feet. Where accessible for sampling,, the copper content of the deposits ranged from a few hundredths of a percent to over S percent; zinc, gold, and silver are present in negligible amounts. Flotation tests of a sample composited to represent typical mine-run ore indicate that 81 percent of the copper is recoverable in a product assaying 28 percent copper at a concentration ratio of 17.5 : 1. INTRODUCTION Statistical records indicate that approximately 110,000 tons of metallic copper (about 16 percent of total Alaskan production) was produced from mines adjacent to Prince William Sound during the 40-year period ended in 1938. Although the principal production was from a large-scale mining and milling operation on Latouche Island (Kennecott Copper Corp., Beatson mine), a substantial amount of the total copper was derived from direct-shipping ores selectively mined or hand-sorted from numerous other deposits in the district. No production has been made since 1938; many of the claims have long been abandoned, and mine workings are either caved or deteriorating rapidly.

Jan 1, 1957

By M. R. Geer

The widespread adoption during the past decade of the dense-medium process for cleaning coal increases the need for technologic studies of the process. Such studies provide information that will insure maximum usefulness of this process in its present form and may well lead to substantial improvements in design and opera¬tion. The Bureau of Mines has published the results of cleaning trials on a wide variety of coals in two dense-medium pilot plants5/ and reported the recovery of coal from waste by dense-medium treatment.6./ The present report deals with the viscosity of magnetite dense medium, an important subject about which virtually nothing has been published. Specifically, the report concerns methods for measuring viscosity, the influence of various medium contaminants on viscosity, the effect of viscosity on cleaning results, and the influence of viscosity on consumption of medium. Cleaning trials on four coals of varied density composition in a pilot plant, using mediums of different viscosities, showed a steady reduction in cleaning efficiency with increasing viscosity in every instance. However, the behavior of each coal in a viscous medium was distinctly individual. With one, an increase of only 1 centipoise in viscosity caused a reduction in recovery efficiency of 7.7 percent, whereas the same increase in viscosity with another reduced recovery efficiency only 2.7 percent.

Jan 1, 1957

By R. F. Dickerson, D. A. Vaughan, A. F. Gerds

ALTHOUGH the metallurgy of uranium has been under intensive study since the early 1940's, no systematic effort has been made to identify the non-metallic inclusions in uranium. Uranium carbide (UC), which is probably the most common inclusion found in graphite-melted metal, has been tentatively identified by previous investigators, but the other nonmetallic inclusions have received little attention. Since metallography is a valuable tool in metallurgical studies, the metallographic identification of the nonmetallic inclusions in uranium is important. Such an investigation has been completed and the identification of slag-type inclusions and of uranium monocarbide, uranium hydride, uranium dioxide, uranium monoxide, and uranium mononitride is described. Metallographic Preporation It is often possible to prepare specimens for metal-lographic examination equally well by several methods. The specimens which were examined in this work were prepared by one of two acceptable methods. For the convenience of the reader, both methods will be discussed in detail and will be referred to simply as Method I or Method II in the subsequent sections. For both Methods I and 11, specimens for microscopic examination usually were mounted either in bakelite or in Paraplex room temperature mounting plastic. Method I—Specimens were ground in a spray of water on a revolving disk covered successively with 120-, 240-, and 600-grit silicon carbide papers. It was necessary to perform the final grinding operation carefully on worn 600-grit paper to keep the scratches as fine as possible. After washing and drying, the specimens were polished for 3 to 4 min on a slow speed wheel (250 rpm) covered with a medium nap cloth. Diamet Hyprez Blue diamond polishing paste, Grade 00, 0 to 2 µ, was used as abrasive with kerosene as lubricant on the wheel. Specimens were washed thoroughly in alcohol and final polished electrolytically in an electrolyte composed of 1 part stock solution (118 g CrO, dissolved in 100 cm3 H2O) with 4 parts of glacial acetic acid. A stainless steel cathode was used. At an open circuit potential of 40 v dc, a polishing time of 2 sec retained inclusions well with the bath at room temperature. If additional etching was required to sharpen the interface between the metal and the inclusions, an electrolyte composed of 1 part stock solution (100 g CrO3 and 100 cm8 H20) and 18 parts glacial acetic acid was used at room temperature. Best results were obtained by etching for from 10 to 15 sec at 20 v dc in the open circuit. Surfaces obtained by this method are suitable for microscopic examination. However, if desired, they may be etched further with other chemicals. Method 11—Rough grinding was done on a wet 180- or 240-grit continuous grinding belt. The specimen was then ground by hand successively on 240-, 400-, and 600-grit silicon carbide papers in a stream of water. Final polishing was accomplished on a 4 in. high speed wheel (3400 rpm) covered with Forstmann's cloth. Linde B levigated alumina, suspended in a 1 volume pet chromic acid solution, was the abrasive. Specimens usually were polished in 5 min or less by this technique. Often the inclusions present in the metal were identified in the mechanically polished condition. When etching was required to outline inclusions more sharply, one of the two following methods was used. In the first method, the specimen is etched lightly while electropolishing in the chromic-acetic acid solution described above (1 part of stock solution to 4 parts of acetic acid). The electrolyte was refrigerated in a dry ice-ethyl alcohol bath and specimens were etched at 60 v dc on the open circuit for 2 or 3 cycles of 3 to 4 sec each. The second technique utilizes electrolytical etching at about 10 v dc (open circuit) in a 10 pet citric acid solution at room temperature. X-Ray Diffraction Technique The major problem in the identification of inclusions in metals by X-ray diffraction techniques is the extraction of a sufficient amount of each type of inclusion to obtain an X-ray diffraction pattern. In the present study, X-ray diffraction patterns were obtained from individual inclusions of the order of 10 µ diam. The polished and etched samples shown in the micrographs were examined at a magnification of X54 or XI00 with a binocular microscope. This allowed sufficient working distance to extract the inclusions with a needle probe for powder X-ray diffraction analysis. Friable inclusions such as MgF2, CaF2, UO2, and UH3 could be freed from the metal by probing the as-polished and etched surface. The fine particles then were picked up on the end of a Vistanex-coated glass rod (0.002 in. diam) which was held in a brass adapter made to fit the powder X-ray diffraction camera. The end of the glass rod was centered in the path of the X-ray beam. In the case of the UC, UO, and UN inclusions which are smaller in size, more metallic in appearance, and less friable than the other inclusions, it was necessary to etch the inclusion in relief before extraction. UN inclusions etched sufficiently in relief in the electrolytic polishing solution described in Methods I and II by increasing the polishing time. UN inclusions were relief etched by extending the

Jan 1, 1957

By J. R. Kyte, L. A. Rapoport, R. J. Stanclift, S. C. Stephan

Experimental studies covering a wide range of core materials and fluid properties have been conducted to determine the mechanism of oil displacement by water in a partially gas-saturated porous medium. In all instances, the presence of a gas phase was found to have a beneficial effect in reducing residual oil saturations. The practical significance of this benefit is discussed, and a simplified procedure is outlined for evaluating the effects of free gas on water flooding by means of short core tests. INTRODUCTION In addition to oil and water, reservoirs subjected to water flooding frequently contain, also, a gas phase. Common engineering procedures account for the presence of this "free gas" only from the viewpoint of volumetric balance, implying that the only role of the gas consists of providing "fill up" space. It is usually visualized that during the initial stages of the water invasion, the oil, moving ahead of the water, displaces part of the gas and that subsequently the remaining portion of the gas phase is totally compressed and dissolved in the advancing oil bank. Thus, consideration of a two-phase, water-oil flooding mechanism supplies an adequate basis for predictions of oil recovery if the pressure build-up caused by the flood is sufficiently great, so as to reduce the free gas saturation to a negligible value in any portion of the reservoir by the time that portion is reached by the advancing flood water. In many in- stances, however, waterflooding operations are carried out when the reservoir pressure is still relatively high SO that the pressure build-up associated with the water flood may not result in complete dissipation of the gas phase. Under such circumstances it is necessary to ascertain whether or not the presence of free gas has an effect on waterflood behavior and, if so, to account for any such effect in the evaluation of field operations. The difficulties encountered in attempting to arrive at a comprehensive picture of the displacement mechanism of oil by water in the presence of free gas stem from the fact that most of the published data on this subject were obtained under conditions that were either not clearly representative of those existing in a reservoir or not sufficiently controlled to permit evaluation of the effects specifically caused by the gas phase. Some of the most precise data found in the literature were obtained in tests using a "static" gas phase created prior to each water flood by circulating oil through partly gas-saturated cores until a "trapped," residual gas saturation was established throughout the system.' Other investigations were conducted under more representative conditions where the gas phase was free to move during the water flood: but in most cases the results of these tests were obscured by auxiliary phenomena which arise from the compressibility and solubility of the gas and preclude quantitative conclusions.2,3,4 Prior to water flooding, a reservoir usually contains oil and gas, distributed in a manner in which both are free to move. Thus, the principal objective of the present studies was to determine the type of displacement mechanism occurring when water invades a porous medium containing oil and a "mobile" gas phase. Further-

Jan 1, 1957

By Fred A. Webber

STEEL ROPE WIRE is one of the more specialized commodities among the many grades of highcarbon steel wires. In its production there are many metallurgical aspects of interest from the steelmaking on through the final stages of wire drawing. We produce rope wire in an integrated mill com prising all the operations from the blast furnaces to finished wire drawing in the wire mills. Steelmaking is carried out with close control on hot metal, selection of scrap, and fluxing materials. The basic open hearths are of 170 tons capacity. Steel is teemed into 19 1/2 in by 19 1/2 in big-end-down molds and is hot-topped with the use of clay refractory hot-tops. The weight of this ingot is 6,900 pounds. All high -carbon steel ingots are charged hot into the soaking pits and are then rolled through the blooming mill in 16 p asses to a bloom ax~ in. by 41/2 in. and approximately 65 feet long. Necessary bottom and top crops are taken on the bloom as it passes from the blooming? mill to the billet mill. The still hot bloom is continuously rolled through the billet mill in . 5 passes to a 2 3/8 in. square. Billets are cut to 32 feet in length by a flying shear and then allowed to cool on the hot bed.

Jan 1, 1957

By G. R. Webber

CHEMICAL AN AL YSIS by x-ray emission spectrometry has become increasingly important during the past few years. The method is analogous to optical spectrography ?with x-rays being used instead of light and should not be confused with methods of x-ray diffraction used? for identification of minerals and chemical compounds. X-ray emission spectrometry has many advantages for both qualitative and quantitative analysis. Its optimum concentration range is higher than that of the optical spectrograph, and the group of elements which can be detected is not identical to that which can be detected by the optical spectrograph. Elements which can be detected by the x-ray spectrometer are those elements from magnesium (atomic number 12) to uranium (atomic number 92) in the periodic table. The lightest elements in this range have low sensitivities and more specialized equipment is necessary for their detection than for the heavier elements. A large number of applications of x-ray analysis have been directed toward the analysis of ores, metallurgical products, and related materials (see References at end of paper). A more complete bibliography is presented in the Norelco Reporter, Vol. 3, 1956, pp. 37-39. The periodicals Analytical Chemistry and Applied Spectroscopy are a good source of current articles and references.

Jan 1, 1957

By W. A. White

UNDERCLAY squeeze is the plastic flowing of underclay below coal pillars into mined-out entries and rooms. Squeezes may be caused either by wet mine conditions where the moisture is taken up by the clay—making it more plastic—or by the presence of certain clay minerals, such as mont-morillonite, which are plastic when there is enough natural moisture. Under either condition, sufficient stress will cause the underclay to flow. Squeezes may fill an entry or room within several hours, or it may be several months before movement stops. Squeeze areas commonly cover hundreds or thousands of square yards. The Coal Div. of the Illinois State Geological Survey has collected samples of underclays from various mines and from cores drilled by coal companies in the state. From these samples natural moisture content, particle size and particle size distribution, and clay mineralogy are determined. Data from samples collected from the underclay below Herrin (No. 6) coal in the Lumaghi Coal Co. mine near Collinsville, Ill., are used in this report to clarify points in the discussion. Data from samples taken from other mines lead to the same conclusions. A generalized geological section for the area is given in Table I. The underclay below coal No. 6 ranges from a few inches to 3 or 4 ft thick. The upper 6 to 18 in. are noncalcareous; the lower part becomes more calcareous with depth. Limestone nodules become larger with depth, almost grading into the limestone below. In areas where the clay is nearly absent the limestone may thicken to take its place; thus they may complement each other in thickness. There are two types of squeeze areas in a mine. In one type up to 3 or 4 ft of underclay lie in what appears to be a depression in the limestone underneath. This is suggested by a rim surrounding the squeeze area where the underclay is thin and the limestone lies within a few inches of the coal. In the second type the underclay of the squeeze area is surrounded by underclay of similar thicknesses which does not squeeze. Test Methods: Natural moisture content, particle size and particle size distribution, and clay mineralogy were determined by the following methods: Natural moisture is the moisture content a clay contains in its natural environment, expressed in percentage of the weight of ovendried clay (110°C or 230°F). To obtain the natural moisture content, given in Table 11, the clay samples were sealed in containers as soon as the samples were taken in the mines. Particle size and particle size distribution were determined by the pipette method,' and the data were plotted as cumulative curves, Fig. 1, on semi-logarithmic paper. Particle size was plotted on the logarithmic scale and percentage on the arithmetic scale. The quartiles (diameters that correspond to frequencies of 25 and 75 pct) and medians (diameters that correspond to the frequency of 50 pct) of the samples were determined from these curves. The clay minerals were identified from the data obtained by differential thermal' and X-ray powder" techniques. The differential thermal analyses were made on the whole samples, whereas the X-ray analyses were made on fractions of less than 2p. Data and Discussion Moisture Content: After the sealed jars had stood for 24 hr, those that contained squeeze samples had perspired, so that droplets of water had accumulated on the insides of the jars. Table II shows the moisture in the clay after it had perspired for 24 hr. (This perspiring was not noted in samples from nonsqueeze areas.) After perspiration one of the squeeze samples still had a higher moisture content than the samples that did not squeeze. Clay Mineralogy: The thermal analysis, Figs. 2 and 3, indicates that the clay minerals are chiefly micaceous in type; the low-temperature endothermal

Jan 1, 1957

The first metal-mine accident-prevention course was prepared and published in 1942-45 as a series of seven miners' circulars (Nos. 51-57). The scope of the course has been broadened, revised, and brought up to date and is being published as a similar series of seven miners' circulars (Nos. 51-57, revised) on accident prevention in metal and nonmetallic mines. These circulars are: Accident Statistics (Miners' Circular 51), dealing with general statistics on accidents and injuries at metal and nonmetallic mines, including causes, costs, and the use of investigations and reports of all accidents.

Jan 1, 1957

By G. G. Eichholz

SUMMARY RADIOACTIVE dynamite has been prepared by introducing a small amount of antimony-124 into the explosive. Test work is described on the effectiveness of this tracer, on radiation levels in its neighbourhood, and on different methods of .application. Factors determining the choice of isotope, amount of activity, and overall cost of this process are discussed. INTRODUCTION Instances are known in which dynamite remains unexploded in drill holes in mining operations. Usually such 'bootlegs' are easily located by inspection of the face and the powder is removed before subsequent drilling is started. Occasionally, however, serious accidents occur because workmen drill into an undetected piece of dynamite. In order to avoid such accidents it was suggested that a different method of location might be tied, such as that afforded by the use of radioactive tracers. This paper describes some experiments that were carried out under the auspices of the Department of Mines and Technical Surveys, with the active co-operation of Canadian Industries Ltd. and Canadian Refractories Ltd., to test the feasibility of such a scheme.

Jan 1, 1957

By F. R. Cattoir

Analytical methods are presented in this paper for determining soluble titanium, total titanium, indicated titanium, and average effective valence in titanium chloride - sodium chloride mixtures. In addition, data are given showing the effects of coarse and fine grinding on the degree of oxidation and average effective valence of such samples. INTRODUCTION The Electrometallurgical Experiment Station at Boulder City, Nev., as part of the Bureau of Mines program to obtain more efficient utilization of our natural resources, has been developing and improving titanium extractive metallurgical methods and techniques since 1945. Numerous reports have been published describing development of the Kroll process,4/ the electrorefining technique,5/ and methods of analyzing titanium sponge.6/

Jan 1, 1957

By K. O. J. Sidwell

STRATMAT LIMITED, through its subsidiary, the Strategic Manganese Corporation, controls two adjoining iron-manganese properties five miles west of Woodstock, New Brunswick. One is a staked property of 77 claims traversed by one trunk highway, several secondary roads, and a branch line of the Canadian National railway. The other property, a 20-square-mile Concession immediately to the north-east, is also traversed by an excellent network of roads. Both proper-ties are situated in gently rolling farmland. The deposits were discovered in 1836 by Dr. C. T. Jackson. The first attempt to exploit them was made in 1848 when a blast furnace was erected with a capacity of 7 tons per day. The ore was mined by a series of deep trenches that followed the folds of the enclosing slates. In the late years of operation, bog iron ore from Burton and Maugerville, in Sunbury county, was used in conjunction with the Wood-stock ore. An additional 5-ton furnace was erected in 1863 and mining was carried on intermittently until 1884. No further extensive work was done until 1953. During the period of activity, approximately 70,-000 tons of ore are said to have been smelted ( 1). During these earl y operations the Iron Ore Hill and Moody Hill deposits were partially opened, with the ?bulk of the furnace feed being mined from the Iron Ore Hill workings. The low tenor and apparently limited extent of the deposits, the high. ?content of phosphorus, and the increasing scarcity of fuel, were the chief factors that brought the enterprise to an end.

Jan 1, 1957

By J. Gordon Parr, D. H. Polonis

The formation and subsequent decomposition of metastable phases in Ti-Ni alloys containing up to 11 pet (atomic) Ni have been studied. The decomposition of a completely retained ß phase and of a completely transformed 8 phase in a 6 pet alloy has been followed by X-ray diffraction and metallographic methods and by hardness determinations made during the process. The possible mechanisms of the reactions are discussed. PREVIOUS investigations of the Ti-Ni system have usually been limited to phase diagram studies; but little attention has been given to metastable phases and tempering processes. These are important, however, since equilibrium conditions are rarely achieved—nor, perhaps, are they desired—in practice. Up to the present time the available transformation data for titanium alloys appear to be restricted to isothermal transformation curves for selected binary and ternary systems. No quantitative studies have been made of the mechanism by which equilibrium is approached. Several independent investigations have been carried out to determine the Ti-Ni phase diagram. Early work by Wallbaum' and later by Long et al.' produced tentative phase diagrams which were not representative of true binary conditions, since the alloys were contaminated with oxygen and nitrogen. The most recent diagram (Fig. 1) is due to Margolin et al.," and a slight modification of the a + ß/ß boundary (shown dotted) has been proposed by McQuillan.' The structure of the phase Ti,Ni was shown by Duwez and Taylor" to be face-centered-cubic, with 96 atoms per structure cell. The formation of a martensitic ß phase (close-packed-hexagonal) in Ti-Ni alloys has generally been observed when specimens of low nickel content are rapidly cooled from the 0 (body-centered-cubic) range. Margolin et al. reported an increasing tendency for P to be retained in lump specimens as the nickel content increases. McQuillan' has studied the effect on the microstructure of delay time in quenching, and has reported the formation of pro- eutectoid a precipitate in a quenched hypoeutectoid alloy. In a previous study of Ti-Fe alloys," experiments were made on powder specimens produced by filing alloy ingots. Techniques were devised for the preparation and heat treatment of alloys, and X-ray diffraction methods were used both for structure determinations and phase ratio estimations. A similar approach has been made in this study of Ti-Ni alloys. Experimental Methods Ten alloys ranging from 0.25 pet to 18 pet Ni* * All compositions are in atomic percentages unless otherwise stated. were prepared from iodide titanium bar stock (hardness Rf 72) and Johnson-Matthey spectrographic standard nickel by levitation melting.' As a check

Jan 1, 1957

By I. Fatt

Networks of resistors are used as analog computers to obtain relative permeability and resistivity index curves for networks of tubes. These curves have all of the characteristics of those obtained on porous media and, therefore demonstrate the validity of the network of tubes model. INTRODUCTION In paper I' of this series the network model was shown to give information on the structure of porous media that could not be obtained from the bundle of tubes model. The agreement between the capillary pressure characteristics of a network of tubes and those of typical porous media does not prove the validity of the network made. The bundle of tubes model, although it gives less information, also shows this agreement. In this paper the flow properties of a network of tubes are shown to be in agreement with flow properties of porous media. The flow properties of the bundle of tubes model are not in adequate agreement with those of porous media. The dynamic properties of porous media, such as fluid permeability and electrical conductivity, have been found experimentally to be more sensitive functions of structure and pore size distribution than are the static properties such as porosity and capillary pressure characteristics. The network model can, therefore, be best tested by comparing the dynamic properties of a network of tubes with the observed properties of porous media. All static and dynamic properties of a completely valid model must agree with the observed properties. The most commonly measured sensitive dynamic properties are the relative fluid permeability and the relative electrical resistivity. Experimental measurements of these dynamic properties on sandstone, sintered glass, sintered alumina, and soil are reported in the petroleum and soil science literature. These properties were chosen, therefore, for the test of the network model. In the network model, relative permeability is the permeability of the network when some of the tubes are not conducting fluid, relative to the permeability when all tubes are conducting fluid. Similarly, the relative resistivity is the electrical resistivity of the network of tubes when some of the tubes are filled with a nonconductor. relative to the resistivity when all tubes are filled with the electrical conducting fluid. Single Size Tube Network The simplest porous medium is one in which all pores are of the same size. Such media can be approached by packing beds or columns of uniform size particles of sand, glass, or metal. The model of such medium in this study is a network of single size tubes. The network form, the ß factor, is usually not known for real porous media. If the validity of the network model can be established, then the study of the flow properties

Jan 1, 1957

By Grant S. Diamond

THE BIBLIOGRAPHY on the use of static electricity in mineral beneficiation consists largely of patents. Some references are found in mineral textbooks, but very little data on flow-sheets of commercial installations are known to the writer. As a matter of fact there have been relatively few successful commercial applications of importance. Johnson prepared and published a Table showing the polarity and static field intensity requirements of many minerals. There have been reports of successful beneficiation of rutile, zir-con, coal, potassium chloride, and phosphate rock. Otherwise, the field of success has been very limited. This may be due to three reasons: first, the mining industry has been averse to dry processes, be-cause of dust nuisances in dry crushing; second, the electrostatic processes used in the past apparently developed no substantial economic advantages; and third, because flotation or other . methods have proven successful on many minerals, the industry has not felt the need for a radically different process. In the feldspar industry there was ?an attempt at electrostatic beneficiation about twenty years ago which was based on the use of fluoride fuming of the pegmatite head feed, in order to make the mineral reactive in a static field. This process was originally said to be successful, but was discontinued because of corrosion damage to machinery. Another effort by use of a chemical additive such as an or-ganic hydroxyl compound has also been attempted. Neither of these processes is known to be in use today.

Jan 1, 1957

By R. A. Hatch

This report summarizes the results of nearly 8 years research on and production of synthetic mica at the Electrotechnical Experiment Station of the Federal Bureau of Mines, Norris, Tenn. This program was undertaken at the request of the United States Department of the Navy and was financed mostly by the Army Signal Corps and the Navy Bureau of Ships through a contract with the Office of Naval Research, The original objectives included fundamental studies of fluor-phlogupite and other fluorine-micas and production of synthetic mica sheets on a pilot-plant scale. The first 3 years of this project were devoted mainly to a search for practical solutions of the many problems involved in designing and constructing a pilot plant for crystallizing fluor-phlogopite mica. The first and most urgent need was a suitable container for the corrosive mica melt. After extensive study, it was concluded that platinum, graphite, high-silica fire clay, and silicon carbide were the most promising refractories for crucibles; but none was perfect. Silicon car¬bide seemed to have the better combination of qualities, combining good corrosion resistance with oxidation resistance.

Jan 1, 1957

By F. N. Bender

Percolation leaching of wad-type manganese ores was investigated, using a novel system of alternate upward passage of sulfur dioxide gas through moistened ore and downward percolation of wash solutions to extract solubilized manganese. Bench and large-scale tests designed to simulate vat and heap leaching were made on four wad ores from Arizona and Nevada and on a pailomelane ore from Arizona. Three of the wad ores required prebaking at 500° to 600° C. to produce a permeable agglomerate that would not slake during percolation washing. The hard-type ore and one of the wad ores that contained a large amount of granular gangue did not require prior roasting. The deportment of the different ores toward leaching and percolation was studied with particular reference to the influence of the sulfur dioxide - oxygen ratio and the effect of gas dilution on the rate of manganese dissolution, dithionate formation, and acid production. Crushed charges of the ores, as coarse as 1 inch and as fine as 1/4 inch, were treated for periods of 5 to 11 days. Percolation of the gas and leach solutions through the charges was achieved without difficulty. The manganese extractions varied between 78 and 97 percent and depended upon the size and type of ore leached. The average quantity of sulfur dioxide required in the larger scale tests was about 2.6 pounds per pound of manganese recovered. The dithionate formation varied from 0.35 to 0.9 pound per pound of manganese extracted depending upon the strength of leaching gas.

Jan 1, 1957

By R. W. Cahn, C. D. Graham

Two predictions of the oriented growth theory of recrystallization textures have been tested by measuring the orientation dependence of the rate of growth of a single grain into a strained single crystal of aluminum, and determining the orientations of artificially and spontaneously nucleated grains growing preferentially into strained aluminum single crystals. Growth rates are found to be insensitive to orientation, except that new grains with orientations similar to the matrix or to a twin of the matrix have very low mobilities. Similarly, new grains growing preferentially into a strained crystal have random orientations, except that orientations near that of the matrix or its twins are avoided. The predictions of oriented growth theory are thus not confirmed. BASICALLY, the oriented growth theory of re-crystallization textures1 rests on the assumption that the rate of growth of a recrystallizing grain depends strongly on the orientation of the growing grain relative to the strained matrix into which it grows. In particular, the theory holds that in face-centered-cubic metals the orientation which corresponds to maximum growth rate is one in which the growing grain and the matrix are related by a rotation about a common <111> direction. The amount of rotation, as derived from several kinds of experiments,2-1 has been assigned various values, generally in the range between 20" and 40". (A <111> rotation of 60" is a twin relationship.) The conclusion that boundary migration rates depend strongly on orientation is based almost entirely on indirect evidence; there have been very few direct measurements of boundary migration rates as a function of orientation.* " The present investigation was undertaken to provide such measurements, to help make possible a decision between the oriented growth and oriented nilcleation theories of recrystal-lization textures. The basic experimental program consisted of measuring the rate of growth of a single recrystal-lizing grain consuming a strained single crystal, with the orientations of both grains preselected so that the effect of orientation on growth rate could be determined. A prerequisite for such an experiment is a strained single crystal which will support the growth of a new grain but which will not spontaneously nucleate new grains on heating. That is, the crystal must support the growth of a grain nucleated artificially, but contain no recrystalliza-tion nuclei which will become active at the testing temperature. Beck was apparently the first to note that such a condition could exist," and to make use of the condition for am experiment of the type described here.&apos; The present work was actually suggested, however, by a report of Tiedema". " that an aluminum single crystal strip, oriented with a (111) plane in the plane of the strip and a < 112> direction parallel to the tensile axis, would not recrystallize after 20 pet extension even when heated almost to the melting point, provided that the strip was heavily etched before being heated. This result could not be duplicated in the present work. In fact, it was found that any crystal which deformed in multiple slip (<100>, <112> and <111> orientations) underwent spontaneous nucleation after 15 pet extension, even if etched. However, crystals which deformed in single slip, and which did not develop heavy deformation bands, could be extended 15 pet without showing spontaneous nucleation at temperatures up to 600°C. Crystals oriented within about 10o of <110> which developed heavy deformation bands could be extended 10 pet without showing spontaneous nucleation. In all cases a heavy etch was required to prevent nucleation. Etching was necessary because of the presence of an oxide layer on the crystal surface at the time of straining, which leads to preferential nucleation at the surface.&apos;&apos; Grain Growth Rates Experimental Procedure and Results—Aluminum strips of 99.6 pet purity (principal impurities 0.19 pet Fe and 0.12 pet Si), 1 mm by 1 cm in cross section, were grown into single crystals of controlled orientation by the strain-anneal method of Fuji-wara.&apos;"&apos; " A sharp temperature gradient was maintained in the strips during growth by lowering them into a salt bath controlled at 650°C. Crystal orientations were determined by the etch-pit method of Barrett and Levenson" to an accuracy of ±2O. The crystals were extended by 10 or 15 pet in a simple hand operated tensile machine. Crystal orientations were rechecked after extension, and were found to be in agreement with the orientations predicted by the formula of Schmid and Boas." After extension, the grip ends of the single crystal specimen were cut off with a jeweller&apos;s saw, and the crystal heavily etched (at least 20 pet wt loss) in hot 10 pet Na or KOH solution. A region of severe local deformation was then introduced at one corner of the strip, usually by cutting off the corner with shears. Heating this end of the strip caused a large number of new grains to nucleate at the sheared edge. One of these grains grew to occupy the full width of the strip. The appearance of the strip at

Jan 1, 1957

In common with general experience in the iron-making industry overseas, Australia has in recent years suffered a deterioration in the physical quality of her iron ores in their suitability as a direct blast furnace feed. The increasing amounts of fines and the more friable nature of lump ore, especially in the ore from the Cockatoo Island deposits in Yampi Sound, Western Australia, have focused attention on problems of ore preparation and agglomeration, particularly sintering.Although very small pilot scale Dwight-Lloyd type sinter machines were operated at the steel-making centres at Newcastle and Port Kembla during World War II, no sizeable capacity was installed, so that ore was charged to the blast furnaces almost entirely unscreened, and the resultant flue dust was stockpiled.Towards the close of the war, the pilot plant at Newcastle was replaced by a small machine, adjacent to the flue dust stockpile, with a rated capacity of some 20 tons per hour. After approximately five months of part-time operation, this plant was closed down in January, 1945. Production was not resumed until December, 1950, when, due to a temporary ore shortage, it was decided to supplement available ore with sinter produced from the large flue dust stocks of about 300,000 tons. In spite of mechanical and process difficulties, inherent to the design of the plant, operation was continued on a two-shift basis, with several shutdowns for extensive overhaul and plant alterations, until September, 1954, when production was put on a three-shift basis. Addition of Yampi ore fines to the sinter machine burden was not commenced...

Jan 1, 1957

By Howard Martens, Pol Duwez

XPERIMENTS were performed on a Cr-Fc alloy Econtaining 44.7 pet Cr in order to determine the heat evolved during the transformation of the a solid solution into the s phase, and the change in volume accompanying the transformation. Since previous measurements on the rate of formation of a from s indicated that the reaction was quite fast as soon as the equilibrium temperature of 820°C was exceeded by some 50°, standard thermal analysis experiments were performed on heating specimens of s at the rate of approximately 40°C per sec. A definite thermal arrest was observed at 870"C, Fig. 1. This result indicates that the reverse seaction of into a is exothermic. From the heating curve of Fig. 1, taking 15°C per sec as the heating rate in the neighborhood of the transformation, 2.4 sec as the time for transformation, and assuming that the specific heat of the alloy at 850°C is an average between iron and chromium, namely 9.5 cal per mol per "C, the latent heat of transformation is approximately 342 cal per mol. The order of magnitude of this latent heat was also obtained by comparing the heating curve of Fig. 1 with a similar curve obtained with pure iron under identical experimental conditions. It was found that the length of the thermal arrest for s was about 1.8 times as long as that for iron. Since the latent heat of the a to 7 iron transformation is 203 cal per mol1, 2 the latent heat of it to a would be 365 cal per mol, which is in relatively good agreement with the value determined from the heating curve. For the determination of volume change, thermal expansion curves were recorded using a specimen containing 44.7 pet Cr and completely transformed to cr by previous treatment. The curves were recorded at a rate of heating of about 4°C per min and at approximately 840°C a sharr, increase in length of about 0.08 pet took place. Fig. 2. It is therefore established that the specific volume of a near the transformation temperature is about 0.24 pet smaller than that of a, and consequently, when the s phase forms in an a matrix, it would tend to shrink away from the matrix. Since the s phase is known to be extremely brittle, these results offer an explanation for the microscopic cracks often observed in the a phase under the microscope. The results of this study are in qualitative agreement with previously published data on stainless steel 19-9DLa and on a Cr-Fe alloy containing 45 pet Cr.&apos; The increase in density due to the transformation from n to s given in ref. 4 is 0.90 pet. These measurements, however, were made at room temperature. whereas the presently reported 0.24 pet is the change at the temperature at which the transformation takes place during heating. In the graph of Fig. 2, the percentage change in length that would be observed at room temperature is given by the length X, which is about 0.27 pet. This would correspond to 0.81 pet in volume change. Acknowledgment This work was done at the Jet Propulsion Laboratory, California Institute of Technology, under Contract No. DA-04-495-ORD-18 with the Army Ordnance Corps, Washington, D. C. The authors wish to thank this agency for permission to publish the results of this investigation. References I H. Klinkhardt: Measurements of True Specific Heats at High Temperatures. Annalen der Physik (1927) 84, pp. 167-200. - H. Esser and W. Runghardt: Influence of the Method, of Dctcrmination on the Measured Heat Content of Iron. Archtvo ffur Dct Eisenhiittenwesen 11934) 8, pp. 37-38. J. J. Gilman, P. K. Koh, and 0. Zmeskal. Delta Ferrite Formation and its influence on the Formation of Sigma in a Wrought Heat Resisting Steel. Trans. ASM 1 1949) 11, pp. 1371-1388. 1 J. M. Thomas: Discussion of ref. 3. Trans. ASM (1949) 41, pp. 3 390-1392.

Jan 1, 1957