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By E. C. Bitzer

The primary object of the work described in the following pages was to simplify the equipment in the separating circuit of the heavy-media process by substituting a spiral classifier for the separatory cone. Mechanical considerations were the leading attraction and the best that was hoped for on metallurgical performance was that the new vessel would give results equal to those obtained by conventional equipment. Tests have demonstrated in commercial operation on iron ore that the mechanical advantages of the spiral separator are about as predicted; also, the metallurgical performance is superior to the cone on the ores treated. Treatment of iron ore involves the separation of two products: a concentrate that sinks and a float product that contains true float material plus a controlled division of interfering middling. The middling material is heavier than the average specific gravity of the separating medium. Recent work with the spiral separator on Tri-State zinc ore showed that the middling material had to be recovered as concentrate because this fraction contained the bulk of the zinc in the ore. It has been demonstrated that it is possible to make three products with the new separator on an ore such as this: a float tailing, a float middling, and a high- grade heavy sink product. It appears from this last work that the new separator has definite mechanical and metalluigical advantages over any type of separating cone for treating feed that contains large amounts of material of a specific gravity close to that of the separating medium. However, either type of separator should perform equally well, metallurgically, on feed that is free of middlings. Each series of experiments with the spiral separator has required additional work to fully develop the possibilities of the machine. For this reason the paper is divided into chronological parts. History of Development A drag-type classifier was first proposed as a substitute for the cone separator by Butler Brothers technicians during the initial tests with galena medium at Crosby, Minn., in 1937. The desire for finding a substitute for the cone arose from trouble with interfering middlings and certain operating disadvantages of the cone. The possibility of using a spiral classifier was also suggested at this time by Emmett Butler and C. J. Abrams. However, inability to satisfactorily recover fine galena, which was used as a medium, terminated all development work at Crosby. During the winter of 1937--1938 investigation started on magnetic medium with concurrent development of the inverted or closed-top cone, which was found necessary to eliminate iron-ore middlings with the float product. About

Jan 1, 1949

By Harry J. Morgan

One of the greatest improvements in drilling equipment has been the development of hard facing metals which are welded by electricity or by acetylene to form a facing which protects the steel of the bit from abrasive wear. The main desirable characteristics of hard facing metals are resistance to abrasive wear, resistance to shock and perfect bond with underlying metal. Resistance to abrasion offered by various metals shows many anomalies. Compounds containing carbon, silicon and boron are the most important hard substances. Carbon, as diamond, silicon carbide and especially the carbides of iron, chromium and tungsten are the outstanding hard products in common use. Tungsten carbide is probably the most commonly used. It is made in the electric furnace and it is important to get the right amount of carbon and the correct crystalline structure in order to obtain the greatest hardness and greatest resistance to abrasion. It may be obtained in three main divisions: wrought, cast and casehardened. Insert hard metals are common. The method of application varies, but it is generally welded to the bit, placed in channels or in drilled holes and covered with a hard surfacing metal. Robinson' has given a very complete article on the use of inserts. Gregg and Küttner2 has discussed the metallography of tungsten carbides and given a good bibliography of the subject,. The time and expense of large-scale testing, together with variations in results, led to the development of a laboratory testing machine for determining the abrasive-resisting qualities of different metals. This machine consists of a motor-driven 40-grain, alumina-base corundum wheel, 8 in. dia., rotating at 30 r.p.m. It is run wet and dressed with

Jan 1, 1930

By E. R. Parker, E. A. Smith

Metallurgists and engineers have always been interested in the mechanism of high-speed deformation because metals are rapidly deformed in various applica-tions and manufacturing processes. The deformation of metals by impact loads has recently engaged the attention of a number of investigators. Many of their results have not been disclosed but some of the published investigations1-8 have shown that the tensile strength, yield strength and elongation generally increase with increasing strain rate. The investigation reported herein is an attempt to determine the reason for this increase in strength and elongation. found to depend upon the strain rate. In the bars broken at high speeds, the slip bands appear to be more numerous. This might account for the higher strength as well as the greater elongation. Experimental Procedure Single crystals of copper (approximately 99.98 per cent) were made in graphite molds by the conventional method of lowering the mold out of the hot zone of a hydrogen furnace at a rate of one inch per hour. Solidification progressed from the bottom upward, forming a single crystal. The crystals were about 0.30 in. in diameter and 4 in. long. They were

Jan 1, 1944

By E. A. Smith, E. R. Parker

Metallurgists and engineers have always been interested in the mechanism of high-speed deformation because metals are rapidly deformed in various applica-tions and manufacturing processes. The deformation of metals by impact loads has recently engaged the attention of a number of investigators. Many of their results have not been disclosed but some of the published investigations1-8 have shown that the tensile strength, yield strength and elongation generally increase with increasing strain rate. The investigation reported herein is an attempt to determine the reason for this increase in strength and elongation. found to depend upon the strain rate. In the bars broken at high speeds, the slip bands appear to be more numerous. This might account for the higher strength as well as the greater elongation. Experimental Procedure Single crystals of copper (approximately 99.98 per cent) were made in graphite molds by the conventional method of lowering the mold out of the hot zone of a hydrogen furnace at a rate of one inch per hour. Solidification progressed from the bottom upward, forming a single crystal. The crystals were about 0.30 in. in diameter and 4 in. long. They were

Jan 1, 1944

A cooperative service for engineers and their employers under the direction, of the American Institute of Mining and Metallurgical Engineers; American Society of Civil Engineers; American Society of Mechanical Engineers; and American Institute of Electrical Engineers, and with the cooperation in Chicago of the Western Society of Engineers, and in San Francisco of the California Section of the American Chemical Society and the Engineers Club of San Francisco. For information as to men available or positions open, address the nearest office. New York Walter V. Brown Manager, 31 West 39th St., Telephone Penn. 9220 Chicago A. Krauser, Manager, Room 1736, 53 West Jackson Boulevard, Telephone Harrison 1238 San Francisco Newton D. Cook, Manager, Room 715, 57 Post . St., Telephone Sutter 1684 UNITED ENGINEERING SOCIETY This is a corporation organized by the American Institute of Mining Engineers, American Society of Mechanical Engineers and the American Institute of Electrical Engineers to hold the title and administer the property at 29 West 39th St. In 1916 the American Society of Civil Engineers was admitted, and each society now holds an equal one-fourth interest in the ownership, occupancy, and administration of the building. The value of this property is estimated at two million dollars. A. I. M. E. representatives are : Arthur S. Dwight, J. Vipond Davies and J. V. N. Dorr. ALFRED D. FLINN, Secretary, 29 West 39th St., New York City. ENGINEERING FOUNDATION This is a fund established by the United Engineering Society in 1915 with a gift of $200,000 from Ambrose Swasey. Subsequent gifts had increased the fund to $600,000 on Jan. 1, 1927. The income, of the fund is used to further research in science and engineering and to advance the profession of engineering and the good of mankind. A. T. M. E. representatives are: H, M. Boylston, J. Vipond Davies, Galen H, Clevenger. ALFRED D. FLINN, Secretary, 29 West 39th St,, New York City.

Jan 1, 1928

G. SHERBURNE ROGERS,* Washington, D. C. (written discussion?).- We are indebted to Captain Lucas for an interesting contribution to the literature of the salt-dome oil fields, and especially for his suggestion that a more aggressive method -of prospecting be adopted. The occasional discovery of new fields on, the Gulf Coast is in itself sufficient to show that the oil possibilities of the region are by no means exhausted, and those who have studied the area most thoroughly are the most optimistic regarding its future. Nevertheless, the search for new fields, according to present methods, involves the expenditure of great sums of money annually, for the proportion of dry holes to producing wells drilled yearly in the Gulf Coast region is much' greater than in most areas, even if all the wells drilled in what is commonly regarded as proved territory are included. Not only are the present methods of locating new domes very uncertain, but when a dome is discovered there is no assurance that it will be oil-bearing; or, if so, whether the oil occurs in the cap-rock, in the sands above it, or in some small isolated lens of sand far down on the flanks of the salt mass. As Captain Lucas points out, about all we positively know is that the domes are there and that some of them are oil-bearing; their origin is a matter of controversy and the original source of the oil is conjectural. Under these conditions, it is not surprising that the search for oil is conducted more or less blindly and that dry holes are common. Many wells are drilled each year in an endeavor to find oil at depths of 2000 or 3000 ft. (609 to 914 m.) or less, in locations which most geologists would condemn without hesitation. As Captain Lucas suggests, the money spent in this way might be used to far better advantage in, drilling one deep well in a carefully selected locality. Opinions may differ as to whether such a, well would find oil, and many geologists will probably believe that the chances are against it, yet all will agree that the boring, whether it finds oil or not, will probably throw light on the origin of the domes and on the source and mode of accumulation of the oil, and will therefore be of great interest, not only to the scientist, but to the oil operator.

Jan 10, 1918

A permanent exhibition of mining machinery has just been opened in the Grand Central Palace, New York City. The exhibits include: Aerial tramways, amalgamation, assaying and laboratory appliances and supplies, blast furnaces, coal, coal-breaker plant, coal excavation, coal products, compressed-air plant, concentrating, crushing, cyanidation, distillation, drainage and pumping, drilling, earth excavation, electrical supplies, explosives, fire prevention, flotation, general supplies, hoisting, hygiene, welfare, iron products, leaching, mechanical conveyors, metal products, natural gas, petroleum, petroleum products, electric, steam, hydraulic, gas, air, and internal-combustion engines, power machinery, preparation of coal, pumping, refining, roasting, rock excavation, rotary drilling; boring, safety appliance, screening and washing, sizing and classifying, smelting, storage of coal, storage of petroleum, surface transportation, surveying, underground timbering, underground trans-port, ventilation, mine. This exposition is operated by the Merchants and Manufacturers Exchange of New York for the purpose of showing under one roof all lines of machinery and mechanical appliances. As for as possible, the exhibits will be shown in operation. The Advisory Committee is as follows: General Howard R. Ward and H. C. Parmelee. Coal and Coke.-Prof. H. H. Stoek, Samuel A. Taylor, Edwin Ludlow. Petroleum and Gas.-Frederick G. Clapp, Ralph Arnold.¬ Extraction of Metals.-Charles W. Merrill, E. Gybbon Spilsbury. Refractories.-Kenneth Seaver.

Jan 12, 1919

By E. C. Robertson

Observations of faults in mines, at outcrops, and in the laboratory lead to the conclusion that the displacement d of a fault increases irregularly but monotonically with the thickness t of its associated fault gouge and breccia, not including adjacent undisplaced jointed rock. The general trend of data points has a slope d/t of about 100. (The correlation coefficient of a logarithmic regression line is r = 0.94.) The rather wide scatter of the points can be accounted for by inaccuracies in measurement of d and t, and by variation in the conditions at faulting of confining pressure, rock type, water pressure, and deformation history. Limestone is an exception to the relation. Until the data can be corrected and refined, the relation should be used only qualitatively for estimating displacement of ore bodies in mines. The suggested relation is based on observations of 48 steeply- dipping normal and reverse faults and nine small flat-dipping thrust faults, with displacement less than 5 km (3 miles). It does not apply to large strike-slip and low-angle overthrust faults because their large displacements are poorly determined and their breccia thicknesses are widely variable.

Jan 1, 1984

By J. E. Papin

Morenci ores contain as an average about 0.015 pct molybdenite, MoS2. Incidental to the concentrating operations applied for the recovery of copper minerals, approximately two-thirds of the molybdenite is floated and appears in the final copper concentrate. The economic importance of molybdenum and the success achieved in its recovery in milling operations elsewhere encouraged research directed toward its recovery in marketable form. Several procedures are utilized to effect separation of molybdenite from copper and iron sulphides, but only two have wide application. In the better known of these two methods the molybdenite in the copper concentrate is depressed in a flotation operation using soluble starch as the depressant. The tailing from this treatment thus becomes a low-grade molybdenite concentrate which after thickening, filtering, and low temperature roasting is repulped with water and subjected to additional flotation steps for recovery of the molybdenite. A thio-phosphate collecting agent is employed in flotation of the copper minerals. Presumably the stability and lasting effects of that collector type necessitated the practice of depressing molybdenite followed by subsequent roasting to insure elimination of copper and iron sulphides from final molybdenite concentrate.

Jan 2, 1955

By I. L. Barker

ALTHOUGH valuable information has been pub-lished on the important problems of slag losses with which every copper metallurgist has to contend, a great deal of money is still being wasted in copper smelters all over the world, through metal being irretrievably lost in reverberatory slags. When smelting a relatively low-grade pyritic concentrate together with a proportion of direct-smelting oxi- dized ore, as is done in Oroya, slag volumes are of necessity high, and even a relatively clean slag, say of 0.5 pct Cu, means a loss of almost 4 pct of all the copper charged, or over $1,000,000 annually at present output and prices. While it is known that such losses can often be reduced by allowing the slag time to settle, with or without addition of a reducing agent such as coal or pyrite, the facilities for such treatment are not always available in a plant of old design working to capacity under severe space limitations. Nor is it easy under such conditions to run large scale tests which may endanger the smooth flow of production for considerable periods without yielding

Jan 1, 1958

By Robert L. Russell, Henry W. Zimmerman

The Bunker Hill mine in the Coeur d'Alene mining district at Kellogg, Idaho, has been a major producer of Pb-Ag-Zn ores since its discovery in 1887. The mine has produced over 29 million tons of ore from some 20 to 25 veins and ore zones and now covers an area approximately 1 mi long by 0.5 mi wide. The active section of the mine extends from 2500 ft above sea level to 1600 ft below sea level. Ore production is presently at the rate of about 1700 tpd. A 2-mi adit, the Kellogg tunnel, at the 2500 elevation provides access to the main shaft area. Ore is hoisted to the adit level through a 5000-ft. 50º-inclined shaft extending to the lowermost haulage level 1200 ft below sea level. Primary shaft service for men and materials is supplied by three major internal inclined shafts equipped with double-drum hoists. Present production requires ten levels to serve for main line track haulage. These range up to 5000 ft in length and are either 200 or 400 vertical ft apart. Also, many intermediate levels exist throughout the mine.

Jan 1, 1971

By John W. Rushton

What role does maintenance play in the design of a new mineral processing facility? Consider the fact that most new plants never reach design capacity the first year-or the second, third, or fourth years. The fact is, according to data collected from several plants which have started up in the last ten years, mill throughput and equipment availability doesn't peak, on the average, until the fifth year.

Jan 3, 1978

By AIME

PROBABLY no greater world traveler has ever been Chairman of one of the Institute's Divisions than Henry Frederick Hebley. To begin with, he was born almost as far away as possible-in Christchurch, New Zealand, Dec. 15, 1893. There he grew up, studying mechanical engineering at the local Seddon Memorial Technical College. Then he went over to Sydney, Australia, for a bit of work before sailing for the U.S.A. in 1915. After a few months as draftsman in a San Francisco office he moved over to Clarkdale, Ariz., in the engineering department of the United Verde copper smelter, which had just gone into operation. But the war was on, and Henry thought he belonged in France with the Canadian Engineers, the United States still remaining aloof from the conflict, and that was the last the copper industry saw of him. After almost two years in France he was wounded, convalesced in England and Canada, and then went back to his native New Zealand to design concrete factory buildings. But soon the United States called again, and this time he landed in Salt Lake City with the Oregon Short Line R.R. Co. Then to Chicago in 1920. where he really got into the coal industry for good, working for the Allen K Garcia Co. on the design and operation of coal mines, beneficiation plants, and combustion equipment; and joining the Institute.

Jan 1, 1946

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

Jan 1, 1961

By Fred C. Bond

COMPRESSION TESTS THE standard method of determining the crushing resistance of rocks consists of crushing prepared shapes under slow compression, and expressing the ultimate crushing resistance at the load causing failure in pounds per square inch of crossectional area perpendicular to the crushing force, with the height approximately equal to the diameter. One-inch cubes or cylindrical drill cores are commonly used. Cubes and drill cores are cut by a high-speed steel disk with diamond dust embedded in the edges, and running under a water spray. Such a saw will cut one square inch or more of hard stone per minute. An oiled, spherical, swivel compression block of small diameter should be used to equalize the pressure. Each sample is crushed between sheets of cardboard or blotting paper extending about one-half inch beyond the edges of the stone. A cloth is wrapped around it to prevent dangerous explosive shattering. It is probably preferable to place the swivel block below the specimen, with either a rigid head or another swivel block above. Whatever the arrangement, the conditions should be selected that will develop the maximum crushing strength of the specimen, even though its top and bottom planes may not be precisely parallel. The cardboard pads may be dispensed with if the ends of the specimens are polished smooth. The use of lead pads was discontinued because of the observed tendency to split the material. The samples are weighed and measured before breaking, and the density is calculated. Cubes that contain bedding planes or veinlets are usually placed with these vertical and parallel to the crushing force, in order to develop the maximum resistance possible. A number of compression tests were made on Canadian ores, by Forrest Nagler, of the Allis-Chalmers Manufacturing Co., and are listed alphabetically in Table 1. These tests were made on one inch cubes or on diamond-drill cores approximately one inch in diameter and one inch long. The drill cores represent virgin rock, while the cubes may have been previously weakened by explosives. Compression tests have been made in the Allis-Chalmers Milwaukee Laboratory on a number of ores and other materials. These are listed alphabetically in Table 2. In test No. 1339, on limestone from the Hanna Coal Co., comparison was made between 2 by 2-in. diamond-drill core segments and one-inch cubes cut from the cores in the same strata. Results for the cylinders are tabulated directly below those for the cubes. The bedding planes were normal to the compressive force in breaking the cylinders and parallel in breaking the cubes, which accounts for the lower strength obtained from the cylinders. The percentage of net linear compression at the ultimate pressure was measured in test No. 1055 for Fontana TVA quartzite as 0.30 for cube A, and 0.37 for cube D.

Jan 1, 1946

By G. T. Higgins

PREVIOUS workers1,2 have found evidence of exaggerated grain growth or secondary recrystallization on annealing sponge zirconium at temperatures high in the a, phase field, but no details of the orientation relationship between the secondary grains and "as-recrystallized" matrix were reported. In other hexagonal metals, namely dilute Mg-A13 and Cd-zn4 alloys, secondary recrystallization has been observed in which the secondary grains are related to the primary recrystallized structure by rotations about the c axis. These rotations are thus comparable with the rotations about the (111) axis observed in the secondary recrystallization of fcc metals. In the current work secondary recrystallization has been observed on annealing iodide zirconium at 800°C and the associated changes in crystallographic texture have been examined. The material employed was arc-melted iodide zirconium of the following composition: Impurity O H Fe Hf Pb I Ni C1 A1 ppm by wt 130 5 230 98 23 28 200 39 30 This was received as 0.25-in. plate, and, prior to the annealing studies, was cold-rolled to 0.040 in. Specimens 1 in. sq were chemically polished and annealed for various times at 800°C in a vacuum better than 5x 10-6 Torr. For metallographic examination specimens were first chemically polished and then anodized8 to enhance contrast between the grains when examined under polarized light. Changes in crystallographic orientation associated with the development of secondary grains were followed by (1011) and (0002) pole-figure determinations using a conventional Schulz goniometer in reflection. Filtered Cr Ka radiation was employed and great care was taken to avoid spurious re- sults due to the close proximity of the Bragg angles for the (1011) and (0002) reflections. Figs. 1 and 2 illustrate the change in grain structure on annealing at 800°C. After 24 hr the structure has ceased to be equiaxed due to the development of certain grains in preference to others. It is notable that the secondary grains do not grow to the extent observed in sponge zirconium.1,2 This appears to be due in part to the fact that normal grain growth is inhibited in the less pure sponge zirconium, with the result that the driving force for secondary recrystallization remains high, while at the same time the number of grains able to develop in the presence of the impurities is also smaller. As a consequence, in sponge zirconium those grains that do develop preferentially are able to grow into the fine -grained matrix without impingement, while in iodide zirconium the preferential growth of many grains leads to early impingement. The pole figures determined for specimens annealed for 5 min and 24 hr at 800°C are illustrated respectively in Figs. 3 and 4. These indicate that the dominant feature of the initial recrystallized texture consists of basal planes at an angle of 321/2 deg to the sheet surface, with a (1120) axis lying parallel to the

Jan 1, 1967

By Fred C. Bond

The Standard method of determining the crushing resistance of rocks consists of crushing prepared shapes under slow compression, and expressing the ultimate crushing resistance at the load causing failure in pounds per square inch of cross-sectional area perpendicular to the crushing force, with the height approximately equal to the diameter. One-inch cubes or cylindrical drill cores are commonly used. Cubes and drill cores are cut by a highspeed steel disk with diamond dust embedded in the edges, and running under a water spray. such a saw will cut one square inch or more of hard stone per minute. An oiled, spherical, swivel compression block of small diameter should be used to equalize the pressure. Each sample is crushed between sheets of cardboard or blotting paper extending about one-half inch beyond the edges of the stone. A cloth is wrapped around it to prevent dangerous explosive shattering. It is probably preferable to place the swivel block below the specimen, with either a rigid head or another swivel block above. Whatever the arrangement, the conditions should be selected that will develop the maximum crushing strength of the specimen, even though its top and bottom planes may not be precisely parallel. The cardboard pads may be dispensed with if the ends of the specimens are polished smooth. The use of lead pads was discontinued because of the observed tendency to split the material. The samples are weighed and measured before breaking, and the density is calculated. Cubes that contain bedding lanes or veinlets are usually placed with these vertical and parallel to the crushing force, in order to develop the maximum resistance possible. A number of compression tests were made on Canadian ores, by Forrest Nagler, of the Allis-Chalmers Manufacturing CO., and are listed alphabetically in Table I. These tests were made on one-inch cubes or on diamond-drill cores approximately one inch in diameter and One inch long. The drill cores represent virgin rock, while the cubes may have been previously weakened by explosives. compression tests have been made in the Allis-Chalmers Milwaukee Laboratory on a number of ores and other materials. These are listed alphabetically in Table 2. In test NO. 1339, on limestone from the Hanna Coal Co., comparison was made between 2 by 2-in. diamond-drill core segments and one-inch cubes cut from the cores in the same strata. Results for the cylinders are tabulated directly below those for the cubes. The bedding planes were normal to the compressive force in breaking the cylinders and parallel in breaking the cubes, which accounts for the lower strength obtained from the cylinders. The percentage of net linear compression at the ultimate pressure was measured in test No. 1055 for Fontana TV A quartzite as 0.30 for cube A, and 0.37 for cube D.

Jan 1, 1947

By Fred C. Bond

The Standard method of determining the crushing resistance of rocks consists of crushing prepared shapes under slow compression, and expressing the ultimate crushing resistance at the load causing failure in pounds per square inch of cross-sectional area perpendicular to the crushing force, with the height approximately equal to the diameter. One-inch cubes or cylindrical drill cores are commonly used. Cubes and drill cores are cut by a highspeed steel disk with diamond dust embedded in the edges, and running under a water spray. such a saw will cut one square inch or more of hard stone per minute. An oiled, spherical, swivel compression block of small diameter should be used to equalize the pressure. Each sample is crushed between sheets of cardboard or blotting paper extending about one-half inch beyond the edges of the stone. A cloth is wrapped around it to prevent dangerous explosive shattering. It is probably preferable to place the swivel block below the specimen, with either a rigid head or another swivel block above. Whatever the arrangement, the conditions should be selected that will develop the maximum crushing strength of the specimen, even though its top and bottom planes may not be precisely parallel. The cardboard pads may be dispensed with if the ends of the specimens are polished smooth. The use of lead pads was discontinued because of the observed tendency to split the material. The samples are weighed and measured before breaking, and the density is calculated. Cubes that contain bedding lanes or veinlets are usually placed with these vertical and parallel to the crushing force, in order to develop the maximum resistance possible. A number of compression tests were made on Canadian ores, by Forrest Nagler, of the Allis-Chalmers Manufacturing CO., and are listed alphabetically in Table I. These tests were made on one-inch cubes or on diamond-drill cores approximately one inch in diameter and One inch long. The drill cores represent virgin rock, while the cubes may have been previously weakened by explosives. compression tests have been made in the Allis-Chalmers Milwaukee Laboratory on a number of ores and other materials. These are listed alphabetically in Table 2. In test NO. 1339, on limestone from the Hanna Coal Co., comparison was made between 2 by 2-in. diamond-drill core segments and one-inch cubes cut from the cores in the same strata. Results for the cylinders are tabulated directly below those for the cubes. The bedding planes were normal to the compressive force in breaking the cylinders and parallel in breaking the cubes, which accounts for the lower strength obtained from the cylinders. The percentage of net linear compression at the ultimate pressure was measured in test No. 1055 for Fontana TV A quartzite as 0.30 for cube A, and 0.37 for cube D.

Jan 1, 1947

By E. Eichen, G. S. Ansell. L. R. Sefton

A Technique for the Preparation of Thin Films of Two-Phase Alloys Suitable for Use in Transmission Electron Microscopy In order to obtain foil sufficiently thin to permit transmission electron microscopy of two-phase alloys, particularly alloys in which the second phase is present as a very finely dispersed second phase, a technique has been developed to permit the thinning of these materials without either the large degree of pitting present in the electrochemical or chemical thinning process or the slicing of the second phase particles accompanying the mi-crotoming process. The metal or alloy to be thinned is first ground to initial sheet thickness of approximately 0.002 in. by hand grinding on 4/0 emery paper. This starting sheet of material is then reduced in cross section by an air-abrasion technique using an S. S. White dental abrasive unit. This unit consists of a supply of compressed CO, which provides a stream of high velocity gas impinging on the metal surface. Incorporated in the machine is a hopper-type of device in which fine abrasive particles of alumina are introduced into this high velocity gas stream. The abrasive particles are irregular in shape, approximately 30 across. If any particles are introduced into the sample during thinning, they should be readily observable. Impingement of this gas abrasive mixture on the metal surface causes rapid removal of the metal in a rather uniform manner. The rates of metal removal may be adjusted by both regulating the gas pressure and amount of abrasive material introduced into the gas stream. By moving the gas stream abrasive mixture slowly about the specimen or sheet surface, a large area of the sheet may be uniformly reduced to a thickness which is then suitable for use in transmission electron microscopy. Attendant with this metal removal is a result in cold working of the metal surface due to the impingement of the abrasive particles. The resultant foils, therefore, if made from materials which are desirable to view in the annealed condition, have to be subsequently heat treated. If the alloy from which these foils have been made has been initially heavily worked or deformed during manufacture, then no subsequent heat treatment is, necessary as in the case of the SAP-type alloys. Following this initial abrasive thinning technique, the material is then given a final electropolish which is just sufficient to remove any oxide which has formed on the metal surface during the abrasion technique. Care has to be exercised in this technique to make sure that none of the attendant problems associated with the chemical or electrochemical removal process are encountered. An electrolyte solution which has been found suitable for aluminum-aluminum oxide SAP materials is one containing 78 ml of perchloric acid, 120 ml of distilled water, 700 ml of ethanol, and 100 ml of butylcellosolve. The current density used is 1 amp per sq cm and a polishing time of 3 sec on each side of the foil is used. Extreme care must be used in choosing the current density and time to ensure that just the oxide film on the specimen is removed. Times or current density which are greater than this will lead to perforation of the film due to the removal of the A1,0, particles or a complete loss of the film due to complete solution of the matrix. Once the oxide film is removed the specimens must be kept in alcohol until placed in the microscope to prevent any further oxidation. Fig. 1 shows -an electron micrograph at X28,000 of a thin foil of an aluminum-aluminum oxide SAP-type alloy prepared using this technique. The alloy consists of a matrix of commercial purity aluminum containing a very finely dispersed second phase of aluminum oxide flakes. In the electron micrograph, the dark patches are the aluminum oxide particles. The lighter portions of the micrograph are the aluminum matrix. Within the aluminum matrix, the dislocation structure of the alloy is clearly visible. This structure consists of intersecting twin boundaries and single dislocations. No abrasive particles were observed in the samples. In addition, thin films of commercial purity aluminum were prepared using this method and observed in the electron microscope. Here also, there was no evidence of abrasive particles introduced in the samples. The technique presented provides a satisfactory method for the production of thin films of aluminum-aluminum oxide SAP-type alloys for use in transmission electron microscopy where none of the usual thinning techniques appears to be satisfactory.

Jan 1, 1962

By A. T. Sweet, C. E. Plummer, H. W. St. Clair, S. F. Ravitz

The ammonium sulphate process for recovering alumina from clays was proposed by Rinman, Buchner, and others many years ago, and more recently various modifications have been investigated both here arid abroad.l-Is The process, as it is being investigated by the Bureau of Mines, involves the following essential steps: (I) sulphating the alumina in the clay by baking with ammonium sulphate at approximately 4m°C., (2) leaching with water to extract aluminum sulphate and ammonium sulphate, (3) crystallization of ammonium alum, (4) conversion of the alum to aluminum hydroxide by the ammonia gases given off during the baking, and (5) calcining the aluminum hydroxide to alumina. The over-all reaction between kaolinite (the most important alumina mineral in most clays) and ammonium sulphate during the baking step may be expressed as follows: Al2O8.2SiO2.2H2O + 4(NH4)2SO4 = (NH4)2SO4.A12(SO4)3 + 6NH3(g) + SH2O(g) + 2SiO2 [i] There is definite evidence. as is shown later. that the aluminum occurs in the baked product as anhydrous ammonium alum rather than as aluminum sulphate, provided the baking temperature is not much above 4o0°C. It is probable that the reaction takes place in the following steps: (NH4)2SO4 = NH3 -(- NH4HSO4 [2] Al2O3.2SiO2.2H2O + ;}NH4HSO4 = A12(SO4)3 + 3NH3 + 5H2O + 2SiO2 [3] A12(SO4)3 + (NH4)2SO4 = (NH4)2SO4.A12(SO4)3 [4] In onc modification of the process, the ammonium sulphate is first decomposed according to Eq. z, and the clay is treated with the resultant ammonium acid sulphate. Reaction I is highly endothermic. On the basis of the best available data, the following values have been estimated for the changes in heat content and free energy in calories per mol: -AH = 331,040 - 34T -AF = 331~040 - 78.3T log T - 671.8T The heat required' at 25OC is 320,900 cal. per mol, or 5650 B.t.u. per pound of alumina. The theoretical equilibcium pressure of NHa, based on the free-energy equation given above, increases very rapidly as the temperature rises above 3o0°C., and reaches one atmosphere at 43s°C. Ammonium alum solutions are almost ideal for crystallization. A saturated solution of ammonium alum contains 126. grams of AlzOa per 1000 grams of water at 90°C. and only 16.5 at 20 C. Hence most of the alum crystallizes out when the

Jan 1, 1944