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By W. C. Bleimeister

The rock salt deposits of the U. S. occur in five major basins: 1) the Eastern Basin (which includes parts of Michigan, Ohio, Pennsylvania, New York, West Virginia, and Ontario) ; 2) the Gulf Coast Basin (the northern rim of which includes parts of Alabama, Mississippi, Louisiana, Arkansas, and Texas, while its southern rim includes parts of the Isthmus of Tehuampetic and the Yucatan Peninsula of Mexico), 3) the Southwestern Salt Basin (which includes parts of Kansas, Colorado, Oklahoma, Texas, and New Mexico), 4) the Williston Basin (which under- lies parts of North Dakota, South Dakota, Montana, and Saskatchewan), and 5) the Green River Basin (whose periphery underlies parts of Wyoming, Utah, and Colorado). The greatest salt production in the U. S. is obtained from the Eastern Basin,-particularly from the areas of Michigan, Ohio, and Ontario. In 1958 the salt production from these areas amounted to 8.7 million tons or 35.3 pct of the combined total produced in the U. S. and Canada. Of the 24,286,000 tons produced by Canada and the United States, 6,443,000 tons were in the form of rock salt from dry mining, while 17,843,000 tons were produced from wells in the form of artificial brine, the result of dissolving the rock salt formation by fresh water. Three important factors lie behind the location and development of this salt mining area:

Jan 5, 1961

By Robert Corcoran, George Wiener

A study of the orientations and microstructure of 3 pct Si Fe alloys after deformation and recrystallization has been made. The components found after deformation agreed with recently published work on single crystals, being primarily (001) [110], (111) [110], and (111) {112}. A pronounced effect of temperature of recrystalliza-tion was found on microstructure and orientation. Low temperature recrystallization was interpreted in terms of low angle boundaries which resulted in the retention of a large amount of the deformation texture. High temperature recrystallization was interpreted in terms of high angle boundaries which gave rise to new components. No simple angular relation between the deformation and high temperature recrystalliza-tion textures could be detected. DEFORMATION and recrystallization behavior of 3 pct Si-Fe has been the subject of scientific investigation for many years. The fact that it is a single phase body-centered-cubic alloy from room temperature to the melting point permits study over a wide range of temperature without the complications of phase transformations. There is an important commercial interest in this material as well, since it is widely used in the electrical industry. In the present work the deformation and recrystallization behavior of poly crystal line silicon iron has been studied with the primary purpose of evaluating the effect of a second phase impurity on both processes as well as the effect of temperature on the recrystallization characteristics. With regard to deformation, the emphasis has been placed on a study of the crys-

Jan 1, 1957

By K. A. Kiselev, V. I. Zelentsov, V. P. Nebera

INTRODUCTION Most works on flotation of ions and precipitates from solutions have been summarized recently (1-3). Flotation is more desirable than thickening or centrifuging because of higher recovery, productivity, simplicity of apparatus and better economics in general. Electrolytic flotation that utilizes gases is more favorable than other flotation processes because of the following: higher dispersity of gas bubbles, low coalescence of the bubbles, possibility of gradual regulation of the dispersity and other parameters of flotation (4-5). Flotation from solutions is mostly based on the use of alkaline reagents as precipitants (5). Flotation from acid solutions is less common. We used multicomponent solutions with more than 2-3 components, unlike previous research methods. Acidic flotation allows recirculation of solutions to previous operations such as leaching, etc. REAGENTS FOR PRECIPITATION Electroflotation was studied over a wide range of pH with the addition of ferrocyanide, oxyquinoline, hydroxide and carbonate precipitants. In recent works (1,2,6,7) on flotation of Ni, Cu, Zn from alkaline solutions, mostly ferrocyanides were applied. Our choice was oxyquinoline because of the following: 8-oxyquinoline is a nonspecific reagent for many metals, it is readily soluble in acids and alkalis, oxyquinolates of the studied metals are in soluble compounds, the reagent works over a wide range of pH, it is widely available, oxyquinolate precipitates are stable when exposed to air, are readily floatable, and are easily converted to oxides of the metals by sintering.

Jan 1, 1980

By W. G. Fischer, S. R. Felde

Trona ore at the Westvaco, Wyo., mine of FMC Corp. has been obtained by room-and-pillar methods since the mine began operation. The flat- lying, 10-ft thick trona (Na2CO3.NaHCO3.2H2O) is covered by 1500 ft of weak shale and sandstone, and extraction of pillars on the retreat quite often throws large amounts of weight onto development workings. Weak shales in the roof and floor fail rapidly, and the mine ribs slough to such an extent that mining often becomes very difficult. When this occurs, efficiency goes down, costs go up, and the risk to men and machinery increases greatly. Difficult mining conditions in the early '60s forced a re-evaluation of all presently known mining techniques in bedded deposits. Many room-and-pillar mining plans were compared with the system in use at that time, but none of them offered a better solution to the roof control problem. Longwall techniques were also seriously considered, but machinery was not available that would cut the hard trona seam and still maintain the productivity obtained from room-and-pillar sections. However, since roof control in the longwall methods appeared to be more satisfactory than that found in room-and-pillar techniques it was believed that a new technique using the longwall principle and based on rock mechanics should be tried rather than previously known pillaring methods.

Jan 4, 1966

Discussion of the paper of THEODORE P. HOLT, presented at the Salt Lake meeting August, 1914, and printed in Bulletin No. 91, July, 1914, pp. 1699 to 1708. F. S. SCHMIDT, Salt Lake City, Utah.-Any furnace that can make a chloridizing roast to yield an extraction of 92 to 93 per cent. and do this at a cost of less than 24c. per ton in a 10-ton unit opens great possibilities for the treatment of certain classes of ores. This cost does not include the salt and will be reduced to about 16 1/2c. per ton in the 35-ton furnace which are now being designed. On a trial run the roaster treated 9.6 ton: of Ontario stope fillings crushed to pass a ¼ -in. opening. The ore is well adapted to chlorination with the exception of insufficient sulphur and occasional days of high lime, but is not adapted to any other process The following is an analysis of the crude ore: Ag, 9.52; Au, 0.029 oz. Pb, 0.71; Cu, 0.11; SiO, 79.4; Zn, 0.57; S, 1.00; Fe, 7.9; Mn, 0.89 CaO, 1.20 per cent. The composition of the mix was: Per Cent. Dry crude ore : 83.4 Moisture 4.4 Salt 8.3 Coal dust 2.3 Pyrite, 70 per cent. pure 1.6

Jan 11, 1914

By E. J. Hall

(Butte Meeting, August, 1913.) THE iron-nail method of assaying has been used for a number of years, but has not met with the approval of all assayers. The method possesses advantages which may be given as follows : (1) no preliminary treatment is required ; (2) a lead button of proper size can be obtained (3) it is economical. On, the other hand, it has its disadvantages, which may be summed up as follows: (1) it is not applicable to ores containing large amounts of impurities other than sulphur, as practically all the base metals will contaminate the lead button ; (2) the slag is unsatisfactory in the larger number of fusions; (3) the method was known to give low silver results under certain conditions and the gold results were questionable. It was with the idea of determining the extent of this latter disadvantage that the following investigation was undertaken. It is well known that the fusion obtained in the lend assay is far more satisfactory than that in the " nails method " for gold and silver. The principal difference in the charges as a class is the presence of considerable reducing agent in the lead charge, and a limited oxidizing action in the nails charge, due to PbO. The possibility of improving the nails fusion by simulating the lead charge was the reason for using argol in some tests, even though there were reasons for expecting this would have -au objectionable effect on the results.

Jan 6, 1913

By Valentine R. Garflas

The Mexican oil fields, during 1921, produced in round numbers 203,000,000 bbl. of which 176,000,000 bbl., or 86 per cent., were exported, the bulk of these exports, or about 73.3 per cent., going to the United States. The Mexican exports were divided by grades as follows: Light crude, 47.0 per cent.; heavy crude, 22.0 per cent.; tops, 3.5 per cent.; fuel oil from light crude, 24.0 per cent. The balance, or 31/2 per cent., includes the bunker fuel shipments and the coastwise trade in Mexico, which is not classified as to grades. The figures show that, in importance, the light-oil fields form about 75 per cent. of the Mcxican petroleum industry. The production of the Panuco field has followed the general history of the American fields, and its gradual decline, which is at present foreshadowed, may be estimated as well as its ultimate economic life. On the other hand, the behavior of the light-oil fields to the south is unlike any in the world so far discovered, and as a result we have concentrated overproductions followed by sudden droughts, both sometimes equally unexpected. The coming in of two or three gushers within adequate pipe-line facilities will flood the market with 100,000 bbl. or more a day, while the flooding by water of a particular pool will, in a few weeks, remove from the market one-half the total production of the Mexican fields.

Jan 1, 1923

By Valentine R. Garflas

The Mexican oil fields, during 1921, produced in round numbers 203,000,000 bbl. of which 176,000,000 bbl., or 86 per cent., were exported, the bulk of these exports, or about 73.3 per cent., going to the United States. The Mexican exports were divided by grades as follows: Light crude, 47.0 per cent.; heavy crude, 22.0 per cent.; tops, 3.5 per cent.; fuel oil from light crude, 24.0 per cent. The balance, or 31/2 per cent., includes the bunker fuel shipments and the coastwise trade in Mexico, which is not classified as to grades. The figures show that, in importance, the light-oil fields form about 75 per cent. of the Mcxican petroleum industry. The production of the Panuco field has followed the general history of the American fields, and its gradual decline, which is at present foreshadowed, may be estimated as well as its ultimate economic life. On the other hand, the behavior of the light-oil fields to the south is unlike any in the world so far discovered, and as a result we have concentrated overproductions followed by sudden droughts, both sometimes equally unexpected. The coming in of two or three gushers within adequate pipe-line facilities will flood the market with 100,000 bbl. or more a day, while the flooding by water of a particular pool will, in a few weeks, remove from the market one-half the total production of the Mexican fields.

Jan 1, 1923

By F. F. Lines

IT is not the intention of the writer to enter into a discussion of the relative merits of the duplex process as compared with the straight scrap and pig iron process, working under the same conditions, but rather to present in a general way several modifications of the former process, and then describe the method adopted by the Maryland Steel Co., as best suited to local conditions, and also to meet the metallurgical problem presented in the removal from the iron of an unusual constituent-chromium. The principal factors to be considered in deciding whether or not duplexing should be employed are: (1) Chemical constituents of pig iron. (2) Variety and quantity of steel to be produced. (3) Relative cost of pig iron and scrap. (4) Regularity of operation. (5) Capital to be invested. (6) An existing Bessemer plant. Having decided to adopt the duplex process, several combinations may be used, viz.: (1) Acid-lined converter with basic open hearth. (2) Acid-lined converter with electric furnace. (3) Basic-lined converter with basic open hearth. (4) Basic-lined converter with electric furnace. (5) Basic open hearth with electric furnace. The combination of an acid-lined converter with a basic open-hearth furnace is the one most commonly employed, and as it is the one best adapted to the conditions encountered at the plant of the Maryland Steel Co., we will briefly outline the advantages and disadvantages of the different methods of working.

Jan 4, 1915

By E. J. Quinn, M. F. Fogler

In a recent paper, Rawdon and Mutchlerl gave some exceptionally interesting results on the Brinell and scratch hardness of severely cold-worked metals. In their work, they found that, on continued cold rolling, the metal hardened up to a particular point and then reversed and became softer; this was true for both Brinell and scratch hardness values. The generally reported behavior2 of metals, with respect to Brinell tests on cold-worked material, is that the metals harden up to a certain point and then, on further cold rolling, no change in Brinell hardness occurs. Jeffries and Archer3 state that there is little difference between the scratch hardness of annealed and cold-worked metals; the work of Faust and Tammann4 also indicated no difference between the hardness of annealed and cold-worked copper. Rawdon and Mutchler found, when they plotted the reduction ratio (initial thickness divided by thickness after rolling) against the hardness value for the cold-rolled material, that the hardness number increased up to a reduction ratio of about 3 and then decreased and became even smaller than that for the annealed metal. This behavior was reported for both scratch and Brinell hardness; Figs. 1 and 2 show their results for Brinell hardness on the metals for which they published data. This is an exceptionally interesting phenomenon, if it occurs under all conditions of rolling, and would have an important bearing on the practice of cold

Jan 1, 1925

By Frank Firmstone

In 1871, two furnaces at the Glendon Iron Works, which had been blown out on account of the "coal strike," were altered from the open-top plan with side flues for collecting the gas, to closed tops with cup and cone. In one furnace the suppression of the side flues permitted a considerable alteration in the profile, but in the other (No. 5) no change in this respect was made; the side flues were simply bricked up and new ones cut through the sides close to the top. This furnace was in blast over four years, and we can, therefore, form a pretty good idea of the effect of the alterations on the furnace process. The principal dimensions are; Height 72'; greatest diameter, 18'; diameter at tuyeres, 8'; diameter of top, 10'; diameter at stock line (point at which the top of the materials is kept), 11'; cubic contents, 11,900 cubic feet. The table below shows the average results for periods of twentysix weeks each. 1st, of the open-topped furnace; 2d, of the furnace with the first charger used, which was an ordinary cup and cone (diameter of cone 5' 2") 3d, with the charger used ever since, a " double " cone 7' 5" diameter outside, having a central opening 3' in diameter. The diagram (Plate 11) shows the daily variations, in the grade of the irons for the same periods.*

By David A. Summers, Clark R. Barker, Marian Mazurkiewicz

In May 1975 the U.S. Bureau of Mines contracted with the University of Missouri-Rolla, Rock Mechanics and Explosives Research Center to develop a Hydrominer modification to a longwall shearer unit, wherein the rotating pick-laced drums and connecting gear drives are replaced by a water jet cutting ahead. The concept of the water jet cutting head is based on using the high localized energy of the water jets to isolate a slice of coal by cutting a slot under, at the back of, and at the top of the web. The plow blade of the head then advances into the cut and wedges the coal cantilever over onto the conveyor [(Fig. 1)]. There were several potential advantages foreseen for the system; perhaps the most significant were the elimination of coal dust from the working area and the ability, with a variation in nozzle geometry, to cut webs of greater depth with a small increase in haulage horsepower. The University initially designed the head, based on experiments carried out in the laboratory, under an earlier Bureau of Mines contract. The experiments showed that it was more advantageous to work at a pressure of 68.9 mPa (10,000 psi) with an estimated flow rate of 3.15 X 10 - 8 m3/s (50 gpm) than go to the higher pressures and lower flow rates which have been advocated elsewhere.

Jan 1, 1979

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. K. Abraham

In recent years there has been interest displayed in the precipitation phenomena occurring in austenitic alloys based on the binary Fe-Ni system.1'2 Previous communications have been extended covering the kinetics of clustering in the Fe-Ni-Ti system and the effect of cluster size on subsequent mechanical properties.3'4 To a great extent the question of coherency, which has a dominant role in determining the mechanical properties, is dictated by the degree of misfit between the precipitate and matrix. Thus, the change in lattice parameter of the matrix with composition is an important variable that should be examined. The lattice parameter, ao, of austenite was determined for Fe-29.75 Ni-1 to 6 Ti and Fe-27 Ni-1 to 10 Ti alloys in this study. The alloys used in this investigation were melted in a vacuum induction furnace from a starting stock of plast iron (99.95), electrolytic nickel (99.9), and ti- tanium sheet (99.5) in a MgO crucible. The alloy compositions in atomic percent are given in Table I and their relative position in the Fe-Ni-Ti ternary is indicated in Fig. 1. The chemical analyses were taken from the homogenized bulk materials treated in a manner related earlier.3 A diamond file was used to obtain powder from the bulk. To remove the stresses induced by filing, the powders were austenitized at 1875°F for

Jan 1, 1969

By Paul Berggreen

LIST OF PUBLICATIONS In the Bibliography titles of publications are replaced by corresponding symbols in this list. American A-1. Transactions of the American Institute of Mining Engineers, New York. A-2. Journal of the New York Microscopical Society, New York. A-3. Journal of the Franklin Institute, Philadelphia, Pa. A-4. The Metallographist, Boston, Mass. A-5. The Electrochemical and Metallurgical Industry, New York. A-6. Bulletin of the American Institute of Mining Engineers, New York. A-7. The Iron Trade Review, Cleveland, Ohio. A-8. The Journal of Physical Chemistry, Ithaca, N. Y. A-9. The Physical Review, New York. A-10. Van Nostrand's Electric Engineering Magazine, New York. English E-1. Proceedings of the Institution of Mechanical Engineers, London. E-2. Journal of the Iron and Steel Institute, London. E3. Proceedings of the Institution of Civil Engineers, London. E-4. Journal of the Chemical Society of London, London. E-5. Philosophical Magazine, London. E-6. Proceedings of the Royal Society of Edinburgh, Edinburgh., E7. Carnegie Scholarship Memoirs, London. E-8. Proceedings of the Royal Society of London, London. E-9. Chemical News, London. E-10. Philosophical Transactions of the Royal Society of London,, London. E-11. Transactions of the North-East Coast Institution of Engineers and Shipbuilders, Newcastle-on-Tyne E-12. Iron, London. E-13. Nature, London. E14. English Mechanic and World of Science, London.

Jan 6, 1914

By John W. Burd

A system is described for the simultaneous deposition of epitaxial layers on as many as eight substrates. A high degree of uniformity of both physical and electrical characteristics is achieved in the films. Variation of film thicknesses is consistently less than ±10pct within a wafer and from wafer to wafer within a run with the variation typically on the order of 55 pct. Composition variation of GaAs1-x PX layers within a wafer and from wafer to wafer within a run is consistently less than 51 pct. Electrical evaluation of the films by several techniques indicates excellent doping uniformity within a wafer and from wafer to wafer within a run. Mobilities for lightly doped GaAs films at 300°K are consistently >6000 cm2 v-1 sec-1 and mobilities > 7000 cm2 v- 1 sec-1 are regularly attainable. Techniques for the preparation of material with carrier concentrations from 1 x 1015cm-3 to 1 x 1019 cm-3 n-type and 5 x 1016 to 5 x 1018 cm-3 p-type are discussed. METHODS for the preparation of 111-V compounds by vapor phase reactions have been extensively reported in the literature.1-6 Almost all of the apparatus described for these various methods are suitable for processing one or at the most a very limited number of wafers simultaneously. With the recent rapid advances in the use of vapor grown GaAs for microwave oscillators and GaAs1-xPx as visible light emitters the requirements for these materials are steadily increasing. In order to satisfy these requirements it is necessary to move from a laboratory scale apparatus to one which is capable of processing a large number of wafers simultaneously. Desirable features would be a high degree of uniformity among the wafers and good reproducibility from run to run. The apparatus to be described fulfills these requirements very well. DISCUSSION The various methods reported in the literature can be classified under three headings: 1) closed tube, 2) open tube, and 3) the close-spaced method. Of these three the open-tube method is the most amenable for scale-up to a manufacturing process. It is the most versatile and the various operating conditions can be more precisely controlled than with the other two methods. A number of chemical reactions may be used to achieve vapor-phase growth of 111-V compounds. Sev-era1 of the more generally used reactions are shown in Fig. 1. All of these reactions have the following points in common: 1) generation of a volatile group III(Ga) species by the reaction of the transport agent (halide or HC1) with either Ga or GaAs, 2) introduction of the Group V(As and/or PI component, 3) a method of adding dopant, if desired, and 4) a region in which deposition from the vapor will occur and form as a single crystal epitaxial film on the substrates. The laboratory scale reactors permit the hot re-actant gases to flow into the relatively cooler deposition zone and pass successively over the several substrates which are arrayed along the long axis of the tube parallel to the gas flow. With this arrangement the composition of the reactant stream is continually changing as solid material is deposited on each successive substrate. As a result of this changing gas composition the reaction driving force also changes from substrate to substrate and the degree of uniformity of layer thickness, doping level, and so forth, is poor. This effect can be partially overcome by imposing a controlled temperature gradient along the deposition region to compensate for change in gas composition. However, even when this is done variations in layer thickness on the order of 30 to 40 pct are common and as high as 50 pct are frequently experienced between adjacent wafers in the tube. To expand this arrangement to a large number of wafers would only increase the nonuniformity from the first to last wafer in the line. From the above discussion the two undesirable features of changing gas composition and temperature gradient become evident. A reactor system which eliminates or minimizes these undesirable features is one in which the apparatus is mounted vertically as shown schematically in Fig. 2. The vertical mounting permits the disposition of a number of substrates on a suitable support so that all wafers are at the same vertical height in the furnace and hence at essentially the same temperature. By using only a single row of wafers the reactant gas mixture passes over only one substrate in its path through the reactor. Thus the two undesirable features of changing gas composition and temperature gradient are minimized. An additional design feature which further minimizes temperature variations is rotation of the substrate holder. Rotation serves to integrate any radial temperature gradient existing around the resistance heated furnace. A photograph of a reactor assembly at the completion of a run is shown in Fig. 3. MATERIAL PREPARATION Apparatus. Although any of the several chemical systems shown in Fig. 1 are adaptable for use in this apparatus the one generally used is System 2, the hydride synthesis system. This system has been de-

Jan 1, 1970

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 C. L. Sollenbeger, R. B. Greenwalt

PERHAPS the most widely used dispersants or gangue depressants in nonmetallic flotation are sodium silicates, which vary in silica-to-soda ratio from 1 to 3.75. Typical manufactured silicates in order of decreasing solubility and increasing amounts of silica are Metso, silica-to-soda ratio of 1.00; D, 2.00; RU, 2.40; K, 2.90; N, 3.22; and S-35, 3.75.* References in flotation literature1,2 to the use of sodium silicates are often weak because they fail to mention the type of silicate used. Metso and silicate N have occasionally been mentioned, but when the type of silicate is not mentioned, it is usually assumed to be N, the cheapest of the soluble silicates and the one recommended by sodium silicate manufacturers as a flotation agent. In the All is-Chalmers Research Laboratories a systematic study was made of the effect of different alkali-silica ratios on the concentration by flotation of two scheelite ores. One of these was a high grade ore from the Sang Dong mine in Korea. The effect of such factors as pH; addition agents; and conditioning time, temperature, and pulp density on the flotation efficiency of this ore have been described previously. The other ore was a low grade ore from Getchell Mines Inc., Nevada. The mineralogy and techniques of concentrating this ore have been described by Kunze. Hereafter these ores will be referred to as the Korean and Nevada ores. Experiments were made with both to determine the effect of three factors—-type of silicate, concentration of silicate, and pH of the pulp—on recovery and grade of tungsten in a rougher concentrate. Average WO, content of the Korean ore was 1.50 pct and of the Nevada ore 0.27 pct. The predominant tungsten mineral in both ores was scheelite, which was accompanied by a small amount of powellite. The powellite and scheelite were finely disseminated through both ores and required a —200 mesh grind for liberation. Major gangue minerals in the Korean ore, in decreasing order of abundance, were amphi-boles, quartz, biotite, garnet, fluorite, and calcite. Bulk sulfides composed about 3 pct of the total weight. Gangue in the Nevada ore, in descending order of abundance, was garnet, alpha quartz, calcite, phlogopite, wollastonite, and amphiboles. Sulfide minerals were 3 to 4 pct of total weight. Batch flotation experiments were made with 500-g samples of ore, each sample wet-ground to 90 pct passing 200 mesh. The finely ground ore was floated in a Fagergren batch cell at 25 pct solids. The natural pH of the Nevada ore was 8.9 and of the Korean ore, 8.5. The D, RU, K, N, and S-35 sodium silicates were obtained in colloidal dispersions with varying amounts of water. The most alkaline, Metso, was in dry powdered form. For convenience in addition, 5 pct solutions by weight were prepared from each of the silicates, on the basis of dry sodium silicate dissolved in the correct amount of distilled water. Chemical analyses of the various silicates are given in Table I, together with the pH of the 5 pct solutions. A preliminary bulk sulfide float was made with secondary butyl xanthate as the collector and pine oil as the frother. The WO] analysis of the sulfide concentrate was nearly 1 pct for the Korean ore and about 0.1 pct for the Nevada ore. The tungsten contained in the sulfide concentrate constituted about 3 pct of the total tungsten in each ore. No effort was made to recover these tungsten values. The scheelite was floated with oleic acid. Adjustments in pH were made with sulfuric acid or sodium carbonate. A 1 pct solution of 85 pct Aerosol OT was sprayed on the froth and sides of the cell during the scheelite float to aid in dispersing the minerals and to decrease the entrapment of gangue particles. Six tests were planned for each of the six types of silicate in which concentrations of 1, 2, and 4 1b of silicate per ton of dry ore were investigated at both 6.5 and 10 pH. All tests were made at room temperature. The performance of each silicate was judged from the grade and recovery of WO, in the scheelite rougher concentrate. Tungsten recovery was calculated on the basis of the scheelite remaining in the ore after the preliminary sulfide float. Testing of each silicate at three levels of concentration and two levels of pH required 36 tests with each scheelite ore. Variance analyses were performed on the concentrate grades and recoveries to determine whether or not the type of sodium silicate, the concentration of sodium silicate, or the pH significantly affected recovery or grade. Results Concentrate Grade: A variance analysis of the concentrate grades for the Korean ore showed that concentration of the silicate and pH of the ore pulp were major factors in producing a high grade concentrate. Also, the silica- to-so da ratio was important as an interaction with pH. The concentrate grade vs silica-to-soda ratio is plotted in Fig. 1. The curves show that the concentrate grade improved with an increase in concentration of sodium silicate and also

Jan 1, 1959

By G. A. Chadwick, D. Jaffrey

The morpho1ogies and orientation relationships of the phases in the Sn-Zn and A1-A13Ni eutectic systems were examined by electron microscopy and X-ray diffraction techniques. In each alloy the "transition" from the lamellar to the fibrous morphology was found to be one of scale, not of type. The minor phase in both systems exhibited certain well developed facets which were not affected by changes in the ingot solidification rate. The crystallographic relationships displayed by the pairs of phases in both systems were also insensitive to the growth rate. In the Sn-Zn alloy, the unique relationship of: growth direction - II [1201 Sn - II [01101 Zn and ribbon interface plane 11 (101) Sn 11 (7012) Zn was determined. The Al-Al3Ni alloy phases did not possess any particular orientation relationship, though the Al3Ni phase invariably grew in the [010] direction and exhibited the same set of facet planes. These results are discussed in relation to current eutectic growth theories and explanations of the "lamellar to fibrous transition". THE lamellar to fibrous transition that occurs in many eutectic alloys has been the subject of considerable speculation and experimental study. In some alloys it can be induced solely by an increase in the solidification rate,'-3 whereas in others the transition supposedly occurs only if the lamellae are forced to grow out of the overall ingot growth direction.4-6 he cause of this latter type of transition has been attributed to deviations of the lamellae from their low energy habit planes;4'5'7 fibers are produced because the sustaining force for lamellar growth (a low energy boundary) is destroyed. Implicit in these explanations is the assumption that fibers are circular in cross-section and completely lacking in low energy inter-phase interfaces. The "natural" growth rate dependent transition has been studied less thoroughly although Tiller8 has attempted a theoretical explanation of it. Tiller's arguments are not completely satisfactory9 but his suggestion that the relative undercoolings of the solid/liquid interface for lamellar and fibrous morphologies are growth rate dependent cannot be totally discounted; it is possible, for instance, that the relative interfacial undercoolings could alter and produce the observed morphology change if the orientation relationships between the phases and the associated interphase bound- ary energies were sensitive to growth rate. Salkind et al." have reported finding a change in the orientation relationships in the A1-A13Ni system accompanying the lamellar to fibrous transition, but contradictory evidence has also been reported for this3'" and another system,12 so the position remains unclear. In an attempt to clarify matters a study was made of the "lamellar to fibrous" transition in the Sn-Zn and A1-A13Ni eutectic systems; the morphologies of these two selected systems are quite similar when viewed by optical microscopy. In the present research the morphologies and morphology changes were investigated by electron microscopy. The orientation relationships existing between the eutectic phases were also determined for both morphologies in both eutectic systems. EXPERIMENTAL PROCEDURE The materials and method of alloy preparation and ingot solidification for the Sn-Zn system have been reported previously.2 In this investigation nine horizontally grown ingots of the highest purity (99.9997 pct) were used. The temperature gradient in the melt was not intentionally varied and was approximately 10°C per cm. Seven growth rates between 1.3 cm per hr and 20 cm per hr were imposed. The A1-A13Ni alloys were prepared from "Spec. Pure" nickel and 99.995 pct aluminum by melting the components in an open alumina crucible and casting the melt into the cold graphite mold. Six ingots of the Al-Al3Ni alloy were unidirectionally solidified at growth rates from 1 cm per hr to 12 cm per hr under high purity argon. A typical ingot was 20 cm long, 1 cm wide, and 0.75 cm to 1.5 cm thick. Samples taken from the bars at positions 12 cm from the nucleation end were examined by conventional orthogonal-section metallo-graphic techniques. When required, samples were mounted for X-ray diffraction analysis using the Laue back-reflection technique with a finely focussed X-ray source. The surfaces of the A1-A13Ni specimens were prepared by mechanically polishing them down to the 1 µ diamond pad stage followed by an electropolish in 80/20 methanol/perchloric acid solution at 0°C and 20 to 30 v. The Sn-Zn specimens were repeatedly polished on an alumina pad and etched in hot dilute (2 pct) nitric acid until the diffraction spots were found to be sharp. Thin films of the alloys were prepared for observation in an electron microscope by spark machining thin discs (0.03 to 0.04 in. thick) from longitudinal and lateral sections of the bars and elec-trolytically thinning them via a jet polishing technique. For the A1-A13Ni eutectic alloy, an 80/20 mixture of ethanol/perchloric acid at 40 v and 20°C was found to be satisfactory. A solution of 70/20/10 methanol/perchloric acid/butylcellosolve at 25 v and 20°C was used on the Sn-Zn alloy. For the former alloy the jet nozzles (cathodes) and the disc clamps were of aluminum;

Jan 1, 1970