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By R. B. Adair, J. S. Browning

The laboratory batch and continuous flotation pilot plant tests demonstrated the technical feasibility of recovering high grade mica concentrates from weathered mica pegmatite ores of Alabama and Georgia. The research indicated that combinations of anionic and cationic collectors may be used effectively for flotation of fine size mica from weathered pegmatite ores. In continuous tests, concentrates containing 98.5% mica were obtained from the Georgia pegmatite ore; the Alabama pegmatite ore concentrates contained 98.4% mica. The recoveries were 91 and 89% respectively. INTRODUCTION The principal uses of fine ground mica are as a filler in wallboard joint cement, as a filler and surface coating for roofing, as an ingredient in paints, and in oil well drilling mud. The mineral has other uses in the manufacture of rubber, wallpaper, plastics, welding rods, electric insulation, house insulation, and textiles, and as an annealing agent in metal treatment. In recent years, more than 99% of the domestic mica produced has been scrap and flake mica (mica which does not meet specifications for sheet mica and is used for producing fine ground mica). There has been a continued increase in mica production for several years, the 1963 production of scrap and flake mica totaling 117,251 tons.1 Ground mica is obtained primarily by crushing and milling pegmatites and schists. To a lesser extent, mica is produced as a byproduct of kaolin washing and feldspar and spodumene flotation operations. The processes used in recovering mica by crushing and milling pegmatites are generally simple, consisting of various combinations of alternate roll crushers and trommel screens that separate the mica and gangue at screen sizes coarser than 6-mesh. As these processes are designed to recover only coarse mica, high losses in the plant rejects are common. Large tonnages of tailings from the crushing and screening plants have been accumulated in a number of areas. Methods for treating such products were developed by the Bureau of Mines in 1941,2 but have not been generally applied. More recently, mica flotation research has been completed and published by the Bureau of Mines.3 These methods required complete removal of 150- to 200-mesh materials from the flotation feed with consequent fine mica losses. Later, the Bureau of. Mines investigated methods for-recovering fine size mica from pegmatite ores after desliming sufficiently to remove clay materials, but not so drastically as to remove the fine sands. This report summarizes the results of these studies. The process developed was effective on pegmatite ores from two locations and should be applicable to the commercial treatment of other mica-bearing pegmatite ores and fine rejects that have been accumulated at various mica-milling operations. DESCRIPTION OF ORES The ores used in the investigation were obtained from the Dixie Mines, Inc., Heflin, Alabama, and the Ruberoid Corporation, Hartwell, Georgia. The sample from Alabama contained muscovite and quartz, with a high percentage of clay, and minor amounts of biotite, kaolin, limonite and tourmaline. The mica in the ore was essentially all minus 4-mesh in size and was free of attached mineral grains. The Georgia sample contained muscovite and quartz, with minor amounts of biotite, kaolin, and limonite. The mica in the ore, which was essentially all minus 4-mesh, was liberated. Petrographic analyses of the two samples are given in Table I. THE ANIONIC-CATIONIC MICA FLOTATION METHOD Previous investigators2,3 have reported that complete desliming of mica ores at 150- to 200-mesh was required prior to flotation with cationic collectors to obtain satisfactory selective separation of the mica from the other mineral components. Numerous tests were made at the Tuscaloosa Metallurgy Research Center to determine if some reagent combination could be used to selectively float finer size mica without complete desliming. The investigation led to development of a process using a simple reagent com-

Jan 1, 1967

By E. R. Helderman, C. Y. Ang, C. C. Nealey

Beryllium-base alloys have been successfully p7.-epared by the liquid-phase sintering technique. Depending orz the composition and amount of the intended liquid please, microstructures either single -phase or duplex in feature with randomly oriented grains have been obtained. Qualitative and semi-qualitative determination of distribution of alloying elements md microsegregations in some experi)uzental alloys haue been made by electron-micro-probe analysis in conjunction with microliardness testing and standard metallography. Tensile tests reoealed that some conzpositions possess attractive elastic properties with Young's mot1uli greater than 40 X 10' psi. In powder metallurgy, liquid-phase sintering is a process or phenomenon that has proven to be of practical value. For example, the heavy metals such as tungsten-copper-nickel, high-strength heavy gyro alloys,' heavy-duty electrical contacts,' and tungsten carbide tool materials are all products of liquid-phase sintering. Mechanisms involved in liquid-phase sintering, however, are not completely understood. Questions regarding the exact roles played by rearrangement of particles, liquid/vapor surface energy, solution and precipitation, and so forth, have not been completely answered. Evidence has been cited3 that at least volume shrinkage in the densification process is diffusion-controlled. It is possible that the predominant mechanisms for the complete densification and grain growth in a liquid-phase sintered system depend primarily on the alloy systems involved, in addition to processing conditions. Despite the lack of sound understanding of the mechanisms of the process, liquid-phase sintering has been and is being used to advantage either to synthesize microstructures for their special properties or to prepare alloys which are difficult to form by fusion process. Liquid-phase sintering of beryllium alloys was first attempted by Jones and Williams.4 They first tried infiltrating beryllium with magnesium, and then succeeded in preparing the alloy by sintering Be-Mg powder compact in molten magnesium bath. This investigation resulted in the identification of some Mg-Be intermediate phases. Crossley et a1.5 also used liquid-phase sintering technique in an attempt to produce ductile beryllium alloys for structural applications. The major liquid-phase components investigated by Crossley et al. were aluminum and silver with minor additives of germanium, calcium, lanthanum, cerium, and yttrium. The lack of wetting and the bleeding out of liquid phase were the difficulties encountered during experimentation. According to Hodge,6 the two compositions investigated by Crossley, which showed some promise based on compression tests, involved large amounts (over 35 wt pct) of silver, thus making them too heavy to be of practical interest to the aerospace industry and military users. The present investigation was prompted by the search for light-weight (density less than aluminum) beryllium alloys exhibiting small anisotropy in physical properties for precision inertial navigation instrument applications. In addition to isotropy, good structural properties such as high elastic modulus or desirable combination of mechanical and physical properties are also objectives of this investigation. The technique of liquid-phase sintering was chosen for its versatility in producing either duplex or homogeneous microstructures. This report is concerned with the use of copper and aluminum, with or without silicon addition, as the intended liquid phase, and the resultant micro-structures and some physical properties of the beryllium alloys. Qualitative and semiquantitative electron-microprobe analyses of some of the alloys are presented to illustrate the usefulness of this microanalytical technique for the identification of microconstituents and their distribution. EXPERIMENTAL PROCEDURES The beryllium powder used was -200 mesh Brush Beryllium Co. QMV NP-50 grade. Typical chemical analysis of the powder is shown in Table I. Commercial high-purity copper, aluminum, and silicon powders all screened to —100 mesh were used as additions. Mixed powder compositions were ball-milled in ceramic jars for 1/2 hr to ensure thorough blending. Milled powder was loaded either in 3/4-in.-diam button die or in Metal Powder Association flat tensile specimen die and compacted under top and bottom pressure. No lubricant or organic binder was used. Sintering was carried out in a quartz tube under a vacuum of 50 to 100 µ pressure. Surface hardness and some microhardness readings were taken on sintered specimens. Sintered density was

Jan 1, 1965

By P. Somasundaran, D. W. Fuerstenau

The length of the collector is found to influence the flotation of the mineral even at incipient conditions, which are below the concentration at which interaction at the solid-liquid interface begins to take place to form hemi-micelles. To study this dependence, concentration for incipient flotation of quartz was determined as a function of pH with collectors of various chain lengths. The observed effect of chain length on flotation is ascribed to that of collector adsorbed on the bubble surface. In previous studies, it was shown that at low concentrations the alkyl collector ions adsorb at the solid-liquid interface as individuals.''2 At higher concentrations, the collector ions adsorbed at the solid-liquid interface associate with each other to form two-dimensional aggregates called hemi-micelles. Above the hemi-micelle concentration, the length of the hydrocarbon chain is extremely important since the hydrocarbons are in effect removed from water during the association, making the energetic conditions more favorable for adsorption at the interface. Because of this enhanced adsorption, one observes a very rapid increase in flotation associated with the hemi-micelle formation at the solid-liquid interface. However, a dependence of flotation on the chain length at concentrations below that required for hemi-micelle association was also observed,' and this cannot be explained by the above mechanism which postulated hydrocarbon chain interactions only at the solid-liquid interface. This prompted an investigation into other possible reactions of the hydrocarbon chains and an examination of the conditions at the bubble surface involved in the flotation system and how these observations might explain the reactions at the solid-gas interface which cause the particle-bubble attachment required for flotation. To obtain more information on chain length effects, flotation, under incipient conditions, was tested by vacuum flotation techniques. The collector-concen-tration-pH relationships for flotation of quartz with alkyl ammonium acetate collectors was delineated by observing the pH at which quartz particles begin to float to the liquid surface. By investigating flotation as a function of pH, it was also possible to study the effect of neutral molecules on incipient flotation conditions, since the aminium ions hydrolyze to amine molecules at higher pH values. EXPERIMENTAL WORK Brazilian quartz specimens were crushed and sized, and the 270 x 400 mesh fraction was used for flotation studies. The samples were leached with concentrated hydrochloric acid until no coloration of the acid occurred. The leached material was washed free of chloride ions and stored in distilled water. The vacuum flotation technique developed by Schuhmann and prakash3 was used to determine the critical pH-concentration curves. This method, which can be used to delineate conditions for incipient flotation, is fairly simple and rapid. About 0.5 gm of 270 x 400 mesh quartz was placed in a 100 ml graduated cylinder which was then filled to the 100 ml mark with the collector solution made from high-purity alkyl ammonium acetate salts. The water used for the test was conductivity water saturated with air that had been passed through a cleansing train consisting of Drierite, Ascarite, a water wash bottle, and a trap. After the pH was adjusted, the cylinder was then conditioned for thirty minutes. In the tests where an acid pH was desired, sufficient acid was added before the collector solution to avoid any effect due to slow desorption of collector from the quartz surface. After conditioning, vacuum was applied to the system and the flotation or nonflotation of the quartz was noted. The pH at which the quartz particles began to float to the liquid-gas interface was taken as the critical PH. Critical pH curves were thus determined for different concentrations of the various collectors. Hallimond tube flotation data were taken from the authors' previous publication1 for correlation with that from the vacuum flotation. RESULTS AND DISCUSSION The results of vacuum flotation studies for determining critical pH-concentration curves, i.e., curves which delineate conditions for incipient flotation, are shown in Fig. I. In generaI, all the curves exhibit an upper and lower pH limit between which flotation will

Jan 1, 1969

By David White

Jan 1, 1925

By John McDonald

THIS report is a continuation of an earlier one with a similar title,1 to which the reader is referred for such details of procedure as do not appear here. A brief summary will be given of the objects and methods of the research at this time. It was pointed out in the previous paper that properties of magnesium alloys, as re-ported by different workers, often differ. This was thought to be due to differences in the preparation of the specimens tested. The ideal way to compare alloys would be to prepare each of them in so many ways that reasonable assurance would exist that the best properties of each alloy had been developed. The alloys would then be com-pared on the basis of these properties. The treatment actually given the alloys of these studies is necessarily a compromise with completeness. Nevertheless, enough treatments have been given so that a con-siderable degree of assurance exists that the properties obtained are representative of the alloy as such, and not merely of the manner in which it was worked and heat-treated.

Jan 1, 1940

By Maurice Ewing, L. Don Leet

The most important quantitative method in seismic prospecting by refraction shooting is the method of profiles. A profile is established by firing a series of charges at various points along a straight line which terminates at the seismograph. The same data are obtained by repeatedly firing charges at one place and recording at a series of stations along the line of the profile. The quantities which are measured are the distance x from each firing position to the seismograph and the time t required for the first disturbance from each explosion to travel to the seismograph. These data are used in plotting the familiar time-distance graph. The only time-distance graphs that will be considered here are those obtained in localities where the velocity of propagation depends solely on the depth beneath the surface; that is, where there is no slope in the subsurface. The essential calculation to be made from such a time-distance graph is the determination of P(x), the maximum depth of penetration of a disturbance coming to the seismograph from a firing point at the distance x from the instrument. If the time-distance graph consists of a series of straight lines, as is often the case, the penetration P(x) can be calculated by means of formulas which appear in almost every description of seismic prospecting.' Until the present, however, the only formula that has been available for calculating P(x) for time-distance graphs which are smooth curves is one which requires an arbitrary assumption regarding the law of velocity increase with depth.2 The practice in these cases has been to approximate the curve by means of a number of straight lines and then to apply the ordinary straight-line formulas. This method clearly can yield accurate results only when a sufficiently large number of straight lines is used. The labor of computation increases rapidly when the number of lines is increased, so too few lines often are used. Further than that, there is a strong tendency to overlook the approximate nature

Jan 1, 1932

By H. Biloni, R. Morando

The surface structure and substructure of Al-Cu alloys solidified as conventional ingots and under particular conditions such as those used by Bower and Flemings are studied. The influence of lampblack coating on the mold walls is especially considered and the results compared with those obtained in copper and graphite molds where no coatings exist. When high heat extraction conditions exist the observations show that mechanism of copious nucleation is responsible for most of the chill zone. When the heat extraction through the mold walls is low, a coarse grain structure with dendritic morphology arises, with a size that depends on the degree of convection present, analogous to that analyzed by Bower and Flemings. In both cases the effect of the convection on the macroscopic and microscopic appearance is discussed. The ingot macrostructure consists of one or more of three zones: "chill zone", "columnar zone", and central "equiaxed zone". The mechanism of the columnar-equiaxed transition has been subject of considerable interest and at present at least three theories exist about the formation of the equiaxed region: 1) the constitutional supercooling theory1 maintains that the equiaxed crystals nucleate after the columnar zone has formed, as a result of the constitutional supercooling of the remaining liquid; 2) chalmers2 pointed out, however, that there were several objections to this proposal, and that consideration should be given to the possibility that all the crystals, equiaxed as well as columnar, originated during the initial chilling of the liquid layer in contact with the mold; 3) Jackson et aL3 and O'Hara and ~iller~ suggested that a remelting mechanism of the dendrite arms is responsible for the formation of the equiaxed region. After the work of Cole and Bolling and other authors6 it became evident that convection (natural, reduced, or forced) plays a very important role in the transition from columnar to equiaxed and on the size of the resultant equiaxed structure. Until recently the accepted explanation of the chill zone was that it occurs as a result of copious nucleation in the liquid layer in contact with the mold walls.798 The columnar region is a subsequent result of the growth of favorably oriented grains and, as a result of a selection mechanism studied by Walton and Chalmers,9 elongated grains with marked texture are formed. Recently, however, Bower and Flemings" using an ingenious laboratory experiment introduced the idea that the "copious nucleation" mechanism is not responsible for the formation of the chill zone and that the presence of convection, introducing some form of "crystal multiplication", plays a decisive role in the formation of the chill zone. Unfortunately, it is important to consider that for their conclusions Bower and Flemings extrapolated the results obtained in their special experiments to the case of conventional ingots, and that these authors only analyzed the macrostructures of the specimens. Let us consider the work by Biloni and chalmers" concerning predendritic solidification. These authors were able to show that a study of the segregation substructure of A1-Cu gives information about the nucleation and growth of crystals formed in contact with a cold surface. A spherical predendritic region characterizes the first part of every grain nucleated in contact with the surface as a result of the chill effect. The aim of this paper is to elucidate through the observation of the segregation substructure the conditions under which (in the Bower and Flemings type of experiments and in conventional ingots) either the nucleation or the multiplication mechanism gives rise to the structure in contact with the mold walls. I) EXPERIMENTAL TECHNIQUES The experiments were performed on two alloys: Al-1 wt pct Cu and A1-5 wt pct Cu. The purity of the aluminum was 99.99 pct and the copper 99.999 pct. The results obtained with both alloys were similar. In the Bower and Flemings type of experiments the apparatus employed to obtain rapid solidification against a surface was similar to that used by those authors. The liquid was drawn by partial vacuum into the thin section mold cavity. Plate casts were 5 cm wide and usually 7.5 cm high. The thicknesses of the cast were 0.1 and 0.3 cm. Two different materials were used for the mold, copper and nuclear-grade graphite. The internal mold surfaces were polished and left uncoated for some experiments. In other experiments, the copper or graphite surface was coated with a thin film of lampblack material. In some of these particular experiments one of the mold walls was left with an uncoated region (usually in the form of a cross). The conventional ingots were cast in graphite or copper molds. In different experiments the mold walls were sometimes uncoated or coated with lampblack material. The results obtained in conventional and Bower and Flemings copper molds were compared with those obtained with copper molds coated with a very thin film of graphite; the results obtained were essentially similar. The size of the conventional ingots was 5 cm diam and 7 cm high in all cases. The cast surfaces produced by the Bower and Flemings type of experiments and conventional methods were observed macroscopically and microscopically without any metallographic preparation. As Biloni and Chalmers showed," the observation of the chill surface can give considerable information about the structure and segregation substructure.

Jan 1, 1969

By G. Wranglen

On account of the possibility of isolating carbides in steel it is generally assumed that the electrode potential of iron carbide is more noble than that of ferrite.1,2,3,4,5 Differences from 0.032 V1 to 0.4 V4 have been recorded. However, it is important to realize that the more noble behavior of cementite in relation to ferrite is not an issue of thermodynamics but of reaction kinetics. Theoretically, cementite is less noble than ferrite, which is a direct consequence of its thermo-dynamic instability. With the value ?F°298 = +4700 cal per mol for the free energy of formation of cementite6 it is easily calculated that the electrode

Jan 1, 1950

By Victor A. Phillips

A series of strips of a Ni-12.7 at. pct A1 alloy were Prepared containing cubical y'(NisAl) precipitates with edge lengths from 60 to 500A. A particle-free solution-tveated strip was included for cornparison. They weve cold-rolled 95 pct and the effects of particle size on the isochronal (1/2 hr) annealing behavior between 300° and 950°C studied (by hardness and light and electron microscopy). It ulas inferred that the particles deformed with the lnatvix becoming lamellae which remained coherent. Comparison with published data fov pure nickel showed that aluminum greatly re-tavded softening and recrystallization, but it made little difference whether or not particles were present. The presence of pakticles led to a heterogeneous distribution of precipitates after annealing at 700" to 750°C. Recovery was not detected. Recrystallization occurred by the growth of new grains into unrecrys-tallized material. In a previous study by the author,' the growth of Ll2-type ordered yl(Ni3Al) precipitates was followed in Ni-12.7 at. pct A1 alloy as a function of aging at 600" and 700°C. The particles were showo to be cubical in shape in all sizes from 50 to 3000A and remained coherent. This work was used as a guide in preparing the starting structures for the present study of the effect of these particles on the annealing behavior of heavily cold-rolled strip. Another question of present interest was whether dislocation and particle hardening were additive, since the structures before rolling ranged from solution-treated to peak-aged to overaged. Also, precipitation might occur on annealing after cold-rolling. Reference may be made to other papers2"5 for previous work in this relatively unexplored field and only some recent work will be mentioned her:. phillips2 studied the effect of deformable 0 to 590A-diam cobalt particles on a Cu-3.23 pct Co alloy rolled 95 pct and found that the particles, which rolled out into thin lamellae, impeded softening and recrystallization. Tanner and servi3 likewise studied the annealing of cold-swaged Cu-2 pct Co alloy containing 150A-diam particles and found impeding effects. Haessner et a1.,4 on the other hand, found that incoherent 2-p-diam non-deformable particles of B4C (0.04 vol pct) tended to increase the rate of recrystallization of copper rolled up to 95 pct reduction. They attributed this to the formation of new grains at the particle interfaces. Humphreys and artin' found that nondeformable silica particles in copper rolled to 30 pct reduction accelerated recrystallization if the particle spacing was large and retarded it if the spacing was smaller. Haessner et a1 4 also studied a rolled Ni-Cr-A1 alloy; however, the particles of y'(Ni3Al)-type precipitate were not put in before rolling, but separated during the isothermal annealing at 750°C. No previous work appears to have been carried out on the effect of y' (Ni3A1) particles on the annealing of Ni-A1 alloy. Hornbogen and ICreye7 redetermined the solubility c of aluminum in nickel as a function of temperature T and showed that it was given by c = 32.6 exp(-1940/RT). This relation gives aluminum solubilities of 15.1, 14.2, 12.0, and 10.7 at. pct at 1000°, 900°, 700°, and 600°C, respectively. The phase precipitated from the nickel-rich solid solution is fcc y1 (Ni3A1) which has a Cu3Au -type ordered structure8 and remains ordered up to 1000°C.B EXPERIMENTAL PROCEDURE The alloy used was identical with that used before. Chemical analysis showed 6.27 wt pct (12.71 at. pct) Al, the principle impurities being 0.065 pct Fe, 0.022 pct Co, 0.020 pct Cu, and 0.004 pct C. Bar stock of 1 in. diam was cold-swaged to % in. diam, cold-rolled to 0.300-in.-thick strip, and annealed at 900°C in dry hydrogen. It was cold-rolled to 0.100-in. thickness and solution-treated for 1 hr at 1000°C while sealed in a quartz tube in argon, quenching in iced brine with the aid of a device to snap off the nose of the tube. Lineal analysis gave an average grain size of 0.055 mm. Pieces of strip were aged at 700°C in vacuo for 30 min, 51/4 hr, and 1 week to produce nominal average particle widths of 60, 150, and 500A, respectively, as known from the previous work.' The average diamond pyramid hardness was determined. The heat-treated strips were rolled from 0.100 to 0.005 in., a reduction of 95 pct, and the rolled strips stored at about -5°C. Small pieces were annealed within 1 week for 30 min at temperatures from 300° to 950° ±2°C in a horizontal vacuum furnace. Strips were withdrawn into a cooling zone, giving an estimated initial cooling rate from 950°C of about 50°C per sec. Average diamond pyramid hardnesses were determined on a lightly electropolished spot on the surface of each strip using 300-g load. Each point on the softening curves represents a separate annealed specimen. Sections containing the rolling direction were examined by optical metallography. Selected specimens were electrothinned to the center plane' and examined by transmission at 100 kv in a Siemens Elmiskop I electron microscope. It is well-known that changes in the structure tend to occur when a deformed strip is electrothinned below a thickness of a few hundred angstroms, although this is less serious with a material such as nickel which has a high melting point, and also is apt to be less serious when particles are present. Observations were nevertheless confined to thicker regions of the foils with estimated thicknesses over 1000A. No changes were observed due to beam exposure.

Jan 1, 1968

Masjid-i-Su1aiman.—There have been no new developments in the Masjid-i-Sulaiman oil fields during the year 1938. In spite of the age of this field, the fall in dome pressure shows no appreciable variation from the low rate of about 0.3 lb. per sq. in. per million tons net production. Drilling has been limited to deepening old wells and to new wells required for maintenance of production and general reservoir control. The rate of offtake has been reduced over the past few years, partly because of depletion of the oil column, and it is expected that future offtake from the Masjid-i-Sulaiman field will be stabilized for some years at around the present figure of 3,000,000 tons per annum. Haft Ke1.—An exploratory well to test deeper formations in the Haft Kel field has proved the existence of productive conditions in the Eocene, which underlies the Asmari limestone (the main producing horizon). Drilling to the northwest in the white-oil springs area has revealed the presence of a separate structure with productive potentialities. One well with a satisfactory production rate has been completed. Offtake from the Haft Kel field has steadily increased since it first came on to production in 1929. Naft-i-Shah.—Production from this field has continued to supply market requirements in northwest Iran. The policy of returning surplus products to the reservoir, which was adopted at the beginning of 1936, has been continued.

Jan 1, 1939

Masjid-i-Su1aiman.—There have been no new developments in the Masjid-i-Sulaiman oil fields during the year 1938. In spite of the age of this field, the fall in dome pressure shows no appreciable variation from the low rate of about 0.3 lb. per sq. in. per million tons net production. Drilling has been limited to deepening old wells and to new wells required for maintenance of production and general reservoir control. The rate of offtake has been reduced over the past few years, partly because of depletion of the oil column, and it is expected that future offtake from the Masjid-i-Sulaiman field will be stabilized for some years at around the present figure of 3,000,000 tons per annum. Haft Ke1.—An exploratory well to test deeper formations in the Haft Kel field has proved the existence of productive conditions in the Eocene, which underlies the Asmari limestone (the main producing horizon). Drilling to the northwest in the white-oil springs area has revealed the presence of a separate structure with productive potentialities. One well with a satisfactory production rate has been completed. Offtake from the Haft Kel field has steadily increased since it first came on to production in 1929. Naft-i-Shah.—Production from this field has continued to supply market requirements in northwest Iran. The policy of returning surplus products to the reservoir, which was adopted at the beginning of 1936, has been continued.

Jan 1, 1939

By J. C. Branner

DuriKg the past two or three years I have seen statements regarding the first discovery of fullers' earth in this country that seem to require correction or modification. One appears again in the Mineral Resources of the United States for 1909, part II., p. 738, where it is said that 'fullers' earth was firat discovered in the United States at Quincy, Fla., in 1893." In this connection the following bit of unpublished history concerning fullers' earth in the State of Arkansas is worthy of attention. In April, 1891, when I was State Geologist of Arkansas, a Swede named John Olsen, formerly a copper-miner in Michigan, but then living south of Little Rock, brought me a sample of what he thought mas fullers' earth. He reported that it was from near the town of Alexander, the locality being 1 S. 13 W., section 8, SW. quarter of the SE. quarter. My chemist, Dr. R. N. Brackett, analyzed the material, and reported: Per Cent. Silica,.....SiO2 .... 63.19 Alumina,.... A12O3 .... 18.76 Iron,.....Fe2O3 .... 7.05 Lime,.,...CaO .... 0.78 Magnesia,.... MgO .... 1.68 Potash,.... K2O ,... 0.21 Soda,.....Na2O .... 1.50 Loss on ignition,........7.57 100.74 Water at 110° to 115° C. = 7.84. Another sample from about the same locality, also brought by John Olsen, on analysis by Dr. Brackett gave :

Jan 1, 1913

By Donald D. Carr, Lawrence F. Rooney

Perhaps no other mineral commodity in this volume has as many uses as limestone and dolomite. These carbonate rocks are the basic building blocks of the construction industry, the material from which aggregate, cement, lime, and building stone are made. Carbonate rocks, and their derived products, are used as fluxes, glass raw material, refractories, fillers, abrasives, soil conditioners, ingredients in a host of chemical processes, and much more. Although the use of limestone and dolomite goes back before recorded history, new uses and products are continually being found. Carbonate rocks form about 15% of the earth's sedimentary crust and are widely available for exploitation. Found extensively on all continents, they are quarried and mined from formations that range in age from Precambrian to Recent. Reserves of carbonate rock are large and will last indefinitely, although high-purity deposits may be absent or have limited availability in certain areas. Limestone and dolomite are so useful and so abundant that in 1981 about 644 million tons were produced in the United States. In fact, about 75% of all stone quarried or mined in the United States was carbonate rock. Sand and gravel was the only mineral commodity produced in greater quantity. In this chapter we have sought to provide the general reader an overview of carbonate rocks, their composition, distribution, production, and uses, with emphasis on developments since 1960. In doing so we borrowed extensively from our report on the applied geology of limestone and dolomite (Rooney and Carr, 1971). The literature on the limestone and dolomite resources of the United States and Canada is so vast and diverse that one can easily become mired down in print. We tried to list those references that are easily accessible and that provide the economic geologist with a starting point for more intensive study. The table listing selected references on limestone and dolomite resources in Canada and the United States reflects our attempt to be selective rather than exhaustive and to direct the reader to the best sources of detailed information. Geology Mineralogy The principal carbonate rocks used by industry are limestone and dolomite. Limestones are sedimentary rocks composed mostly of the mineral calcite (CaCO3) and dolomites are sedimentary rocks composed mostly of the mineral dolomite (CaCO3 • MgCO3). Aragonite (CaCO3), which has the same chemical composition as calcite but a different crystal structure, is economically important only in modern deposits, such as oyster shells and oolites. Aragonite is metastable and alters to calcite in time. Some other carbonate minerals, notably siderite (FeCO3), ankerite (Ca2MgFe (CO3)4), and magnesite (MgCO3), are commonly found associated with limestones and dolomites but generally in minor amounts. Because of their similar physical properties, the carbonate minerals are not easily distinguished one from the other. Specific gravity,

Jan 1, 1983

By J. J. Kramer, G. W. Wiener, K. Foster

The effects of the primary grain size and sheet thickness on the secondary growth rates of grains with (100) surface planes were studied in 3 pct Si-Fe sheets. This secondary grain growth was carried out under conditions in which the {100} plane had the lowest surface free energy. The value of the surface energy difference, between the (100) plane and the random matrix planes was found to he only about 3 pct of the grain boundary energy, indicating that most of the driving force for secondary growth is supplzed by grain boundary energy. A method for obtaining cube texture in 3 pct Si-Fe sheets by a secondary recrystallization process has been reported.' It has been demonstrated that a difference in surface free energy between the (100) plane and other planes is responsible for this growth, where the (100) plane has the lowest surface energy. A semiquantitative relation has been derived for secondary grain growth in sheets where primary grain growth has proceeded until the grains have grown through the sheet and the average grain diameter in the plane of the sheet is from one to two times the sheet thickness. Then, the linear growth rate, G, for the secondary grains can be given by where M is the grain boundary mobility, is the grain boundary free energy, is the average primary grain radius, A is the average difference in surface free energy between the (100) plane and planes of other orientations, t is the sheet thickness, and C is a term first proposed by zener6 which acts as a negative driving force, the effect of inclusions in holding up grain boundary motion. Since the problem of grain growth being discussed is under conditions where the matrix grain size is at least equal to the sheet thickness, the radius r is, of course, a function of the sheet thickness. The term B/r is the grain boundary driving force normally associated with inclusion inhibited or texture inhibited secondary recrystallization. Here, however, the term is modified to account for the fact that growth occurs in thin sheets. The term is the additional driving force available because of the difference in surface free energy. The purpose of the present work has been to evaluate the driving force terms of the growth equation by studying growth rates of (100) secondary grains as a function of sheet thickness and primary grain size. From these data it has been possible to determine the relative values of grain boundary energy, surface energy difference, and the inclusion term, C. EXPERIMENTAL PROCEDURE A 3 pct Si-Fe alloy was melted and cast under a helium atmosphere using electrolytic iron and a pure commercial grade of silicon as raw materials. The alloy was hot and cold rolled to a thickness of 0.6 mm, and samples approximately 5 in. long by 1 1/4 in. wide were cut from the cold-rolled sheets. Four different primary grain sizes were obtained

Jan 1, 1963

Two sessions during the recent AMC Mining Convention in Los Angeles, September 23-26, served to update industry personnel on the status of health and safety regulations in the US. As reflected by the American Mining Congress resolution on mine safety and health, "Based on experience with the federal Coal Mine Health and Safety Act of 1969 and the federal Mine Safety and Health Act of 1977, (AMC) does not believe that laws designed to force compliance with regulations through the imposition of criminal or civil penalties will result in safer mines. (AMC) feels that the government's participation will be much more productive if greater emphasis is placed on research, training, and inspections aimed primarily at assisting operators and employees in recognizing and eliminating hazardous conditions and practices.

Jan 11, 1979

By L. F. Mondolfo, W. T. Collins

A study of the relationship between undercooling for nucleation and structure in Sn-Cu alloys with 0.1 to 5 pct Cu has shown that in hypereutectic allojls the halo of tin that surrounds the primary crystals of Cu3Sn5 is larger, the larger the undercooling for nucleation o,f the tin. This increase of halo size results in a decrease of coupled eutectic, and, in alloys far from the eulectic composition, may produce its complete disappeavance, with the formation of a divorced eutectic structure. This was confirnred by the excrrnination of other alloys in which divorced eutectic slructuves are formed, and leads to the conclusion that they ave only an extrenle case of halo forrtzalion , which results when the two phases freeze one at a time and solidification of the first is completed Defove the second starts. It was also found that under proper conditions of nucleation all types of eutectic structures can be formed in the sartte system , and therefore divorced eutectics, like normal and anomalous, are not characteristic of the syslett~, but are mainly controlled by nucleatiorz. Dizlovced eutectics are formed when the phase that tutcleates the eulectic vequires a large undevcooling for ils nucleation and when the cotnpositiorz of the alloy is far from the eutectic., on the side of the primary phase that does not nucleate the other phase. It is recommended that the tevm "divorced" be used in preference to degenerate because it is more desct-iptice of the morphology and mode of forinalion of the structures. ThE variety of structures found in eutectic alloys has been extensively investigated and classified. The most accepted classification is the one by ~cheil,' in which three different types of eutectic were distinguished: 1) normal, 2) anomalous, 3) degenerate (divorced). ATornlal eutectics are typified by the simultaneous growth of the two phases ("coupling") by which the two phases appear as interpenetrating crystals. The presence of a crystallization front, in which the two phases grow side by side, creates the eutectic grains, with the boundaries where the fronts meet. The presence of eutectic grains is the .distinguishing feature of a normal eutectic, according to Scheil. Straumanis and Brakss2 examined the Cd-Zn system and showed that there was a crystallographic relationship between the phases. Later, others4 also investigated additional systems and found definite crystallographic relationships in the coupled eutectics. The anornalous eutectic shows much less coupling than the normal; the two phases are intimately mixed but 'grow without a uniform crystallization front—a consistent crystallographic relationship— and the eutectic grain is conspicuously absent. As in the normal eutectics faster rates of growth result in a finer structure, but there is not the typical uniform spacing of normal eutectics. The degenerate eutectic shows no coupling; in fact the two phases attempt to minimize their area of contact and to form separate crystals. It has been suggested5" that slow cooling may favor this type of structure. Scheil believes that normal eutectics are formed when the two solid phases are present in more or less equal proportions, whereas both anomalous and degenerate eutectics form when one of the phases is present only in small amounts. spengler7 extended much farther this qualitative relationship between the eutectic type and the ratio of the two phases, and added a relationship to the melting point of the constituents. On this basis he proposed two equations for determining into which of Scheil's classifications an alloy belongs. The first equation is: where TI is the melting temperature of the lower-melting component, Tp of the higher-melting component, and Te the eutectic temperature. The second equations is: where is the volume percent of the lower-melting phase and $2 of the higher-melting phase at the eutectic composition. If 0 and/or 4 are in the range 0.1 to 1, a normal eutectic is formed; if in the range 0.01 to 0.1, anomalous; if less than 0.01, degenerate. Although the examples given by Spengler show a good agreement with the formulas, chadwick found that the Zn-Sn eutectic is normal to all growth rates, even though the volume ratio is 12/1, and Davies9 reports that the A1-AlgCo2 eutectic is normal, with a volume ratio of more than 30/1. Many more discrepancies of this type can also be found. Neither Scheil nor most of the other investigators have considered nucleation as a factor in the formation of divorced eutectics. Daviesg states that divorced eutectics form when neither phase acts as

Jan 1, 1965

By W. Rostoker, R. P. Elliott

TWO intermediate phases enter into equilibrium with the primary solid solutions of titanium.' The TiMn2 phase was identified by Wallbaum2 as of the C14 type isomorphous with MgZn2. Contrary to Maykuth, et al.,¹ the phase occuring at about the 50-50 atomic proportion has been shown to derive from a peritectoid reaction.:' A 30 day anneal at 900°C of an alloy containing 52 wt pct Mn developed sufficient of the new phase to give a clear and predominant diffraction pattern. The powder pattern was taken in a 14 cm diameter powder camera using filtered Cu Ka radiation. In all, 75 lines were recognized and measured. Interplanar spacing and observed intensities for the first 26 of these are given in Table I.

Jan 1, 1954

By John V. Beall

Early this year at the University of Arizona in Tucson, a survey was made of student opinion about the minerals industry. Over 100 of the three page questionnaires were completed and these were analyzed by the following categories: 40 Mining Engineering students, 20 Geological Engineering with 2 Geophysical Engineering students, 15 Geology students, 7 Metallurgical Engineering, 26 Underclassmen, 29 Graduate students and a composite of 84 total students. Not all of the results of the survey were predictable. After graduation there is a strong preference toward going to work in the mineral industries. The next most popular options, but trailing the first choice greatly, was graduate work or employment in another industry. A smattering of other choices were for teaching, government or research. None checked the box for drop out.

Jan 1, 1971

By Gerhard Derge

THE orientation relationships resulting from allotropic transforma-tions and the formation of segregate structures in metals and alloys have been the subject of the eight earlier papers in this series1. A brief summary of orientation studies has also been given by Sachs2. A survey of these papers discloses that the factors that determine the orientation relationship of a precipitated phase to its parent solid solution, as Well as the outward form and appearance of the new phase, are not completely understood. It is now evident that crystallographically analogous systems, as a rule, exhibit the same type of Widmanstätten figure and orientation relations, so that useful information is not to be expected from examination of a new alloy involving lattice combinations of which the orientation relationships are already known. Therefore, the determina-tion of the relations existing between lattice types that have not already been studied seems to be the most promising mode of attack upon the problem; both of the systems reported in this paper represent new com-binations of lattice types.

Jan 1, 1937

By R. I. Jaffee, H. R. Ogden, D. J. Maykuth

IN THE past year, Jaffee and Campbell&apos; and Finlay and Snyder2 reported on the mechanical properties of titanium-base alloys, some of which were in the same ranges of composition as are covered in this paper. In this paper, evidence confirming that given by Finlay and Snyder on the effects of carbon, oxygen, and nitrogen on titanium will be presented; and, in addition, new data will be given on the effects of these elements on the flow properties and phase transformation of titanium. Materials and Preparation of Alloys The preparation and general properties of iodide titanium have been adequately described elsewhere.&apos; , As-deposited iodide titanium rod, prepared at Battelle, of Vickers hardness less than 90 was employed as the base metal in the present work. This was the same material as that used by Finlay and Snyder.2 The probable analysis reported by them for standard quality metal holds here also: N 0.005 pct, 0 0.01 pct, C 0.03 pct, Fe <0.04 pct, A1 <0.05 pct, Si <0.03 pct, and Ti 99.85 pct. Carbon was added in the form of flake graphite supplied by the Joseph Dixon Crucible Co. Oxygen was added in the form of c.p. grade TiO, powder, produced by J. T. Baker Chemical Co. Nitrogen was added in Ti3N4 powder, supplied by the Remington Arms Co. Individual ingots weighed 7 or 8 g. Carbon, oxygen, or nitrogen was added by placing the corresponding powder in a capsule made from as-deposited iodide titanium rods and melting the capsule with the balance of the charge. The charge was are-melted with a tungsten electrode on a water-cooled copper hearth under a partial vacuum of very pure argon (99.92 pct minimum). Melting was practically contamination free. Vick-ers hardness increases of less than 10 points were normal for unalloyed iodide titanium control melts. Nitrogen analyses of are-melted iodide titanium showed a nitrogen content of 0.005 pct, about the same as is present in the as-deposited rod. No tungsten pickup was found in a melt of iodide titanium analyzed for tungsten. Weight losses in melting nitrogen-free alloys were very small and varied consistently from nil to 0.015 g (0 to 0.2 pct). This permitted the use of nominal composition for these alloys. Chemical analyses made for carbon, which can be analyzed conveniently by combustion methods, justified this procedure. Where nitrogen was added, considerable splattering took place. Here it was necessary to analyze for nitrogen by the Kjeldahl method. The ingots were hot rolled at 850°C to about 0.045 in. thick. After hot rolling, the strips were descaled by mechanical grinding, and then given a cold reduction of 5 to 10 pct to insure a uniform thickness throughout the length of the specimen. The edge strips and the tensile strips were annealed in a vacuum of 1x10-4 mm Hg pressure for 3 1/2 hr at 850°C and furnace cooled. Methods of Investigation Hardness Measurements: At least five Vickers hardness measurements were taken using a 10-kg load on each sample in the following conditions: (1) top and bottom of each ingot, (2) top and bottom surface of as-rolled and annealed sheet, and (3) on cross-section of annealed sheet and all quenched specimens. Tensile Tests: Tensile tests were conducted on Baldwin-Southwark testing machines having load ranges of 600 or 2000 lb. Tests were made on 1-in. gauge-length specimens, 3 1/4-in. overall length, 1/2 in. wide, 0.040 in. thick, with a reduced section 1 1/4 in. long and 0.250 in. wide. Two SR-4, A-7 strain gauges, one mounted on each side of the specimen, were used to measure the strain over a limited range to determine the modulus of elasticity. After the modulus of elasticity readings had been taken, load vs. strain readings were taken, using only one strain gauge, at increments of 0.0001 in. until the yield points were passed and then at 0.001-in. increments to the limit of the strain-gauge indicator (0.02 in.). Strain readings above 0.02 in. per in. were taken every 0.01 in., using dividers to measure the strain between the 1-in. gauge marks until the maximum load had been reached. Crosshead speed, when using the SR-4 gauges, was 0.005 in. per min, and, when using dividers, 0.01 in. per min. Flow Curves: Flow curves were determined using the true stress-true strain data obtained during the tension test. The usefulness of this type of information has been dealt with very adequately elsewhere by L. R. Jackson,&apos; J. H. Hollomon,6 and many others. Flow curves of true stress vs. true strain could be converted to the more conventional cold-work curve of 0.2 pct offset yield strength vs. percentage of cold reduction by means of the transformation, 1/1 = 1/1-R, where R is the fraction reduction in cold working. Thus, the true strains corresponding to percentage reduction can be calculated, and the 0.2 pct offset yield strengths scaled off the — 6 curve by taking the true stresses corresponding to the values of 6 + 0.002 strain. Heat Treatment: For the transformation studies, the alloys were heat treated in a horizontal-tube furnace using a dried 99.92 pct argon atmosphere, and quenched into water. Essentially no contamination was found after several hours of heat treatment at temperatures up to 1050°C. Metallography: Specimens were prepared in the

Jan 1, 1951