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By Nicholas J. Grant, Noboru Komatsu

Metallographic and X-ray studies were made of oxide dispersion strengthened Cu-12 vol pet SiO2 and Cu-3.5 vol pet Al2O3 alloys following time exposures at temperatures approaching the melting. point of the matrix metal. Changes in hardness, oxide particle size and crystal structure were studied to determine the time-temperature stability of these alloys. An interpretation of the mechanism of oxide agglomeration is proposed. One of the most striking features of dispersion strengthened metal-metal oxide alloys is their stability at elevated temperatures, both with respect to recrystallization and maintenance of mechanical properties after exposure at high temperatures. A small amount of work has been done on the re-crystallization phenomenon in dispersion hardened metal-metal oxide alloys'l and several theoretical treatments have been advanced regarding the stability of these alloys by Lenel and Ansell,8 and by Grant and his co-workers.9, 10 This paper reports on metallographic and X-ray studies following various heat treatments of Cu-AI2D3 and Cu-SiO2 alloys at elevated temperatures and the effect of subsequent cold work on the recrystallizalion temperature. An interpretation of the recrystallization behavior of this type of alloy, based on the decomposition and agglomeration of oxides, is proposed. EXPERIMENTAL PROCEDURE Cast ingot bars of copper-1.59 pet Si and Cu-0.77 pet Al, 7/8 in in diam, were annealed in argon for 80 hr at 1000CC for homogenization. The homogenized rods were machined into fine chips and ball milled. Milled particles in the range minus 20 to plus 60 mesh were separated for internal oxidation. The internal oxidation was accomplished by the same method used by Preston and Grant,9 except that the oxidalion temperature for the Cu-Si alloy was 750°C, and for the Cu-A1 alloy was 800°C. These powders were then hydrogen-reduced at 450°C, compacted in a copper container, evacuated at room temperature to 0.04 µ, and sealed for extrusion. They were extruded at 1400°F (760°C) with a ram speed of 55 in. per min for an extrusion ratio of 15.6 to 1 to give a rod 0.38 in. diam by about 3 ft long.

Jan 1, 1962

By Nicholas J. Grant, Klaus M. Zwilsky

EVER since the unusual high temperature creep resistance and structure stability of SAP (Sintered Aluminum Powder) and similar aluminum-alumina alloys were reported,'," there has been a need to determine whether other metal-metal oxide (or other hard stable particle) alloys, not so ideal as the Al-Al 2 O 3 system, would show similar high temperature strength and stability. Of the many possible methods of obtaining a metal-metal oxide alloy,a one that offers many practical and theoretical advantages is the simple mechanical blending of metal powders with hard stable particles, followed by pressing, sintering, and hot extruding. With this purpose in mind copper powder and silica and alumina were selected for experimentation because these materials are readily available, cheap, reliable, and lend themseives te the simplest processing and testing. Starting Materials—Two sizes of electrolytically deposited copper powders were used, a —200 mesh powder referred to as A powder in this investigation and a —325 mesh powder referred to as C powder. Silica was added in the form of pure Potter's flint from which a —10µ fraction had been separated. Alumina of the a variety was used in two size ranges. The first was a —10µ fraction separated from a coarser aggregate, the second a commercial product of 0.3µ average diam manufactured by Linde Air Products. Preparation of Powders—Five-hundred gram batches of A copper with 1, 3, and 10 volume pct of each of the three oxides mentioned above were prepared, as well as C copper containing 1, 3, and 10 volume pct of —lop silica. Powders were weighed out carefully and blended by ball milling in air for 24 hr. Since this treatment resulted in surface oxidation of the copper, the charge was hydrogen reduced at 260°C for 5 hr. The next step consisted of hydrostatically compacting the powder into a shape suitable for the required hot working. For this purpose a slug about 11/2 in. in diam and 31/2 in. in length was produced by placing the mixed powders into a rubber sleeve, holding in a perforated steel canister, and rubber stoppering at the ends; the assembly was then subjected to a hydrostatic pressure of 50,000 psi. The air was evacuated from the assembly prior to pressing in order to prevent

Jan 1, 1958

By A. M. Kivari

OPERATIONS at the cement plant of the Permanente Corporation, in the hills about 45 miles south of San Francisco and 12 miles west of San Jose, are interesting to the members because of the adoption of modern hydrometallurgical methods for handling and beneficiating raw materials. Closed-circuit grinding, classification, hydro-separation, flotation, agitation, and thickening are familiar terms at this cement plant. These methods make it possible to process refractory limestone into suitable materials for the manufacture of modern cements. Construction of the plant, having originally a design capacity of 7000 bbl. of cement per day, was started in June 1939, and the first clinker was ground on the following Christmas Day. At present the capacity is about 12,000 bbl. of finished cement per 24 hr., most of the production being low-heat cement.† About 3130 tons of limestone, 620 tons 0f clay and 100 tons of gypsum are required daily for this output. Occasionally iron oxide is added to the clay to obtain the desired composition. This, together with the gypsum, is purchased from outside sources. Up to the present time, the corporation has produced low-heat, normal, moderate heat, moderate-sulphate-resisting, high-early-strength, oil-well, modified-oil-well, and plastic cements. Most of the present production is for Shasta Dam, near Redding, Calif., the total demand being 5,800,000 bbl, of cement. Following are some of the cement requirements of the Shasta Dam specifications: [PERCENT Chemical composition: Loss in ignition2.25 Insoluble residue0.75 SO32.25 MgO5.00 Uncombined lime in clinker (CaO)1 .25 Percentage of iron oxide to alumina ratio1.5 Compound composition: Tricalcium silicate (3CaO.Si02)Not more than 3,5 Dicalcium silicate (2CaO.Si02)Not less than 40 and not more than 65 Tricalcium aluminate (3CaO.Al2O7)Not more than 7 Tetracalcium aluminoferrite (4CaO.A12O3.Fe203) Not more than 0 Fineness:] The average specific surface in the bin sampled shall be not less than 1800 sq. cm. per gram and no individual sample less than 1600 sq. centimeters. Compressive strength: The average compressive strength-in pounds per square inch of three mortar cubes composed of one part cement and 2.75 parts fine testing sand, by weight, shall be equal to or greater than the following:

Jan 1, 1941

By William Marsh Baldwin

TWO of the most useful and important equations available to the metallurgist for the study of plastic deformation of metals are the Huber-von Mises-Henckyl-~ and the St. Venant7-10 equations. Huber-von Mises-Hengky Equation The Huber-von Mises-Hencky equation answers the question: When does plastic flow occur in metal that is subjected to a multi-axial stress? It occurs, according to this equation, when the three principal stresses,t UI, u2, and u3 satisfy the equation: (<ri - <r2)2 + (<r2 - <rsY + (ff! - <r3)* = 2Ki [i] Here K is the yield strength of the material as determined in an ordinary tensile test. If the quantities ul, 52, andas are assigned to the coordinates of a Cartesian three-dimensional system, this expression describes a cylinder whose axis of symmetry is inclined at equal angles to the three coordinate axes4s6 (Fig. I). The radius of this cylinder is .\/%K. For the purpose of simplicity, it is sometimes advantageous to ascribe the values al/K = sl, az/K = s2, UD/K = SJ to the three coordinate axes instead of the principal stress alone. In this case, Eq. I becomes (*i - s*)1 + (s2 - S3)2 + (si - SiY = 2 [2] and the radius of the cylinder becomes \/%. In the latter method of representation, a point lying inside the cylinder indicates that the metal will react elasti-cally, whereas a point lying on the cylindrical surface indicates that the metal will behave plastically. Some of the geometric features of this cylinder are worthy of study. Let us inquire first as to what interpretation may be placed upon what we will choose to call the "circles of latitude" of the cylinder (L in Fig. I) and the "meridians" of the cylinder (M in Fig. I). Circles of Latitude Circles of latitude are formed by allowing a plane, passing perpendicular to the cylinder axis, to intersect with the cylinder. Any point, P, on this circle is presumed to have the coordinates sl, SZ, and s3. The coordinates of the point resulting from the intersection of the plane and the cylinder axis will be a, a, and a (since the cylinder axis is equally inclined to the three coordinate axes). L?t US now pass a line through the point on the circle and the point on the axis.

Jan 1, 1946

By William Marsh Baldwin

TWO of the most useful and important equations available to the metallurgist for the study of plastic deformation of metals are the Huber-von Mises-Henckyl-~ and the St. Venant7-10 equations. Huber-von Mises-Hengky Equation The Huber-von Mises-Hencky equation answers the question: When does plastic flow occur in metal that is subjected to a multi-axial stress? It occurs, according to this equation, when the three principal stresses,t UI, u2, and u3 satisfy the equation: (<ri - <r2)2 + (<r2 - <rsY + (ff! - <r3)* = 2Ki [i] Here K is the yield strength of the material as determined in an ordinary tensile test. If the quantities ul, 52, andas are assigned to the coordinates of a Cartesian three-dimensional system, this expression describes a cylinder whose axis of symmetry is inclined at equal angles to the three coordinate axes4s6 (Fig. I). The radius of this cylinder is .\/%K. For the purpose of simplicity, it is sometimes advantageous to ascribe the values al/K = sl, az/K = s2, UD/K = SJ to the three coordinate axes instead of the principal stress alone. In this case, Eq. I becomes (*i - s*)1 + (s2 - S3)2 + (si - SiY = 2 [2] and the radius of the cylinder becomes \/%. In the latter method of representation, a point lying inside the cylinder indicates that the metal will react elasti-cally, whereas a point lying on the cylindrical surface indicates that the metal will behave plastically. Some of the geometric features of this cylinder are worthy of study. Let us inquire first as to what interpretation may be placed upon what we will choose to call the "circles of latitude" of the cylinder (L in Fig. I) and the "meridians" of the cylinder (M in Fig. I). Circles of Latitude Circles of latitude are formed by allowing a plane, passing perpendicular to the cylinder axis, to intersect with the cylinder. Any point, P, on this circle is presumed to have the coordinates sl, SZ, and s3. The coordinates of the point resulting from the intersection of the plane and the cylinder axis will be a, a, and a (since the cylinder axis is equally inclined to the three coordinate axes). L?t US now pass a line through the point on the circle and the point on the axis.

Jan 1, 1946

By Lewis A. Delano, Harold Rabling

It has been generally recognized that, owing to the extreme friability of galena, fine grinding has a tendency to cause excessive sliming of the mineral, so operators of lead mills have attempted to avoid this condition by commencing concentration at as coarse sizes as any mineral is freed. Jigging has been the basis of the milling process, making a clean coarse concentrate and a large amount of tailing, which was considered sufficiently low-grade to be rejected. However, developments and improvements in concentration processes are everywhere changing the low-grade tailing of yesterday into material worth re-treating today. Investigations of the work of the Hancock jig on the Bonne Terre ore have shown that the best results to be expected will give a tailing assaying 0.75 per cent. lead; the average for all conditions and grades of ore will be between 0.80 and 0.90 per cent. By crushing the jig tailings in ball-mills and retreating by tables and flotation, a tailing of considerably lower grade can be made; the problem then becomes an economic one of increased crushing costs versus higher recovery. In considering the entire elimination of jigging, the increascd smelting charges due to a greater amount of slime galena will be counterbalanced by the lower operating cost, increased recovery, and the many advantages of a simpler flow sheet. In developing these problems in the Bonne Terre mill of the St. Joseph Lead Co., a long series of tests has been carried out covering every stage of crushing and concentration, and a large number of possible flow sheets were considered and tried. Only the final results and a few comparisons will be given here. At the same time, a careful and detailed cost-keeping system has enabled us to compare milling costs with the various Bow sheets, and to calculate the economics of the problem with great accuracy. Concentration Problem The ore occurs as widely scattered deposits of galena disseminated through limestone; it has a specific gravity of 2.8 and the following composition: Pb, 4.00 per cent.; Fe, 3.00 per cent.; Zn, 0.32 per cent.; S, 3.10 per cent.; MnO2, 0.73 per cent.; SiO2, 4.20 per cent.; Al2O3, 3.20 per cent ; CaO, 28.60 per cent.; MgO, 16.85 per cent.; CO2, 36.00 per

Jan 1, 1922

By Rex B. McLellan, W. A. Oates

FROM a consideration of the application of the Gibbs-Duhem equation to multicomponent systems arken&apos; derived the following equation applying to dilute solutions of a solute, 2, dissolved in a binary solution, 1-3:

Jan 1, 1969

By W. I. Duvall, D. E. Stephenson. Discussion by R. G. K. Morrison

R.G.K. Morrison (Chairman, Dept. of Mining Engineering and Applied Geophysics, McGill University, Montreal, Que. Canada) - The authors have introduced a subject, the intensive study of which has awaited scientific developments. These are now such as to justify a thorough review of our thinking on the causes and control of rockbursts. The formulae developed in the paper, the comparison between rockbursts and earthquakes in figure 1 and the energy data relating to explosives serve as an effective foundation. In the paper this writer is quoted as suggesting that energy of the order of 10 x 10 11 ft. lb. may have been released in some of the heaviest rockbursts in the Kolar Gold Field. He now hastens to add that such an estimate has no scientific validity. It arises only from a casual comparison of surface and underground effects of the medium heavy bursts, referred to in the paper and estimated by Jones at 3.0 x 1010 ft.lbs., with those of obviously greater magnitude. In any case, we have the estimate by Jones above, that by a team of seismologists 1 on the Witwatersrand of 10 x 1010 ft.lbs., that by Coates of 3.8 x 10" ft.lbs., also referred to in the paper, that by Blan-chard2 for the catastrophic rockburst at Springhill, N.S., of only 7.4 X 107 ft. lbs., and finally the range covered by Cook, referred to in the paper. It is probable also that data for the heavy rockburst at Merkers3 in the WERRA potash area of Germany are available as it was recorded on seismographs from Moscow to Spain. It is the writer&apos;s impression that some standardization is present in the estimates above for 10 x 10 10, 3.8 x 1010 and 7.4 x 107 ft.lbs., respectively. The latter, for Springhill, represents a relatively low order of magnitude. It is obvious that any energy estimate must be related to the local geometry of openings at the time of the event. It is also obvious that any explanation of the causes of rockburst must be capable of providing a wide range of energy. However, we must remember that the energy release is an effect indicating magnitude. The cause lies with the mechanism initiating the primary failure, generating the seismic activity, to which much of the damage is probably due.

Jan 1, 1967

By D. B. Williams

For the first time in the history of the Venezuelan petroleum industry production exceeded 200 million barrels. The total production for all fields amounted to 205,430,869 bbl., which is more than 9 per cent of the world&apos;s 1939 total. This is an increase of over 15 million barrels or 8.0 per cent above the 1938 figure, which, compared with the slightly less than 2 per cent increase of the 1938 figure over 1937, shows the marked activity in Venezuela during the past year. The Maracaibo Lake fields are still the predominating factor in Venezuelan production, showing an increase of approximately 9½ million barrels over last year&apos;s figure and accounting for 71.8 per cent of Venezuela&apos;s total. Lagunillas continues to hold precedence as a single field, having yielded 47.1 per cent of the accumulative total and 39.4 per cent of 1939&apos;s total. This field showed an increase of slightly more than 3½ million barrels over 1938. Tia Juana, the second largest field, attained a record production, increasing its percentage of the Venezuelan total from 23.4 in 1938 to 23.7 in 1939. The La Rosa field, which includes Punta Benitez and Ambrosio, declined from 13.7 to 12.0 per cent; Bachaquero, the southernmost Lake field, which came into regular production at the end of 1938, contributed over 31/3 million barrels. Quiriquire, in eastern Venezuela, ousted La Rosa as the third largest producing field, and, although production increased by 11/3 milliorl barrels, percentage of the total declined from 13.2 to 12.9. Mene Grande, the oldest field, declined from 6.6 per cent in 1938 to 5.9 in 1939. Tem-blador produced for a whole year for the first time and yielded 3,647,867 bbl. The Colon district, in the Maracaibo Lake area, comprising the Tarra-Los Manueles fields, showed slight increases, as also did Cumarebo and Pedernales. Construction of the 16-in. pipe line from Oficina to Puerto La Cruz (Guanta), the longest line of this size in the world, was completed toward the end of the year and this new field in eastern Venezuela started shipping oil in December. This field is operated by the Mene Grande Oil Co. and was credited with a production of 2,347,625 bbl. in 1939. Jusepin field, some 25 miles southwest of Quiriquire in eastern Venezuela,

Jan 1, 1940

By D. B. Williams

For the first time in the history of the Venezuelan petroleum industry production exceeded 200 million barrels. The total production for all fields amounted to 205,430,869 bbl., which is more than 9 per cent of the world&apos;s 1939 total. This is an increase of over 15 million barrels or 8.0 per cent above the 1938 figure, which, compared with the slightly less than 2 per cent increase of the 1938 figure over 1937, shows the marked activity in Venezuela during the past year. The Maracaibo Lake fields are still the predominating factor in Venezuelan production, showing an increase of approximately 9½ million barrels over last year&apos;s figure and accounting for 71.8 per cent of Venezuela&apos;s total. Lagunillas continues to hold precedence as a single field, having yielded 47.1 per cent of the accumulative total and 39.4 per cent of 1939&apos;s total. This field showed an increase of slightly more than 3½ million barrels over 1938. Tia Juana, the second largest field, attained a record production, increasing its percentage of the Venezuelan total from 23.4 in 1938 to 23.7 in 1939. The La Rosa field, which includes Punta Benitez and Ambrosio, declined from 13.7 to 12.0 per cent; Bachaquero, the southernmost Lake field, which came into regular production at the end of 1938, contributed over 31/3 million barrels. Quiriquire, in eastern Venezuela, ousted La Rosa as the third largest producing field, and, although production increased by 11/3 milliorl barrels, percentage of the total declined from 13.2 to 12.9. Mene Grande, the oldest field, declined from 6.6 per cent in 1938 to 5.9 in 1939. Tem-blador produced for a whole year for the first time and yielded 3,647,867 bbl. The Colon district, in the Maracaibo Lake area, comprising the Tarra-Los Manueles fields, showed slight increases, as also did Cumarebo and Pedernales. Construction of the 16-in. pipe line from Oficina to Puerto La Cruz (Guanta), the longest line of this size in the world, was completed toward the end of the year and this new field in eastern Venezuela started shipping oil in December. This field is operated by the Mene Grande Oil Co. and was credited with a production of 2,347,625 bbl. in 1939. Jusepin field, some 25 miles southwest of Quiriquire in eastern Venezuela,

Jan 1, 1940

By Enid C. Plante

To extend our knowledge of the flotation behavior of sulphide minerals, the response of the following minerals to ethyl xanthate as collector was studied by captive bubble and cylinder flotation tests: antimonite (Sb2S3), arsenopyrite (FeAsS), covellite (CuS), rnarcasite (FeS2), orpiment (As&.), pyrrhotite (FeS) and tetrahedrite (4CU2S, Sb2S3). Lollingite (FeAs2) was also exarnined to determine if its behavior could be correlated with that of pyrite or rnarcasite (FeS2. Experimental Method Mineral for Flolation and Contact Tests Mineral was prepared in the manner a1ready described1 and its behavior both freshly ground and "oxidized" was studied. Tests in which the mineral was allowed to oxidize for various periods showed that a uniform response to xanthate was reached in two days or less. Oxidation Products The soluble oxidation products from most of the above minerals were measured and their effect on the flotation of the mineral studied. The mineral samples were wet ground to minus-52 mesh and deslimed, and 20 g of this material placed in 200 ml of distilled water of a measured pH value, and CO2-free air bubbled through each suspension at a constant rate (about I bubble/sec) for 5 days. It has been shown1 that the size of the mineral is unimportant in the rate of formation , oxidation products and that probably the supply of oxygen to the mineral is the rate-determining step. At the end of 5 days the pH value of the &apos;supernatant liquid was measured again, the mineral filtered off and the soluble products determined. Methods for estimation of sulphur acids, ferrous and ferric iron and copper have already been described.l No satisfactory method was found for antimony. Arsenic was estimated as the arsenate.2 Flotation of "Unoxidized" Minerals with Ethyl Xanthate as Collector Fig I to 3, 4. 6, show the effect of alkali and cyanide as depressants for the minerals with 25 mg potassium ethyl xanthate per liter as collector at 35°C. Wark and Cox8 have shown that with ethyl xanthate as collector, galena, pyrite and chalcopyrite show a greater tolerance to cyanide and hydroxyl ions at room temperature than at 35°C Covellite (Fig I), marcasite (Fig 2) and pyrrhotite (Fig 3) behave similarly. The independence of the curves for pyrrhotite at 35°C with respect to cyanide

Jan 1, 1949

By Robert G. Woolery, S. Ramachandran, James A. Weber, Donald J. Hansen

Union Carbide began looking seriously at heap leaching in 1971. At that time some 1.6 million tons of mineral averaging 0.40 kg U3O8 /t) (0.80 lb U3O8) were stockpiled at various sites around the Gas Hills, Wyoming, uranium facility. Several alternatives for economically exploiting these reserves were considered and heap leaching seemed the most attractive. At the time, Western Nuclear Inc. was operating a heap leaching project nearby in which the low-grade ore was leached with sulfuric acid, the product liquor treated in an on site solvent extraction circuit, and the stripped product liquor re-acidified and recycled. The operators were most generous in allowing us to visit their site and in answering our questions. They were also helpful in discussing the problems associated with heap leaching. Their experience confirmed our belief that it was possible to operate a heap leach profitably on material too low grade for conventional milling. Based largely on what we had learned from Western Nuclear&apos;s experience, we undertook a program involving a laboratory study to determine the characteristics of the mineral stockpiles, as related to heap leaching, and to conduct a pilot heap leach adjoining our Gas Hill mill. Basically the pilot heap construction and leach procedure were similar to those described in the literature l, 2 with certain modifications to permit detailed monitoring of the operation. In May 1972, the decision was made to construct a test heap. The UCC plant at Gas Hills, Wyoming was selected as the most appropriate site for the following reasons: (1) The necessary equipment for heap construction was readily available. (2) Stockpiles of mineral from the various mining sites were on hand: (3) Construction of the heap could be made on an abandoned tailings pile minimizing problems associated with environmental approval. (4) Proximity of the mill would allow product streams to be absorbed into existing circuits. (5) Necessary utilities were available. (6) Tailings water from the existing circuit could be used for leaching. A program for the pilot heap leach was developed with the following primary objectives. (1) To confirm the data obtained in bench-scale tests particularly on uranium recovery, acid usage, and ore permeability. (2) To evaluate plastic liners used for base preparation. (3) To investigate heap configuration variables. (4) To determine heap leach amenability of the different mineral sources. (5) To establish the economics of heap leaching low-grade ores.

Jan 1, 1979

By Wllliam D. Davis

C OMMERCIAL production of oil in northeastern Oklahoma began in 1897 and in the next two decades this area became one of the greatest oil districts of the time. Its importance is now secondary, but thousands of wells in this area have produced uninterruptedly for more than thirty years. They are now classified as stripper wells. By means of what is known as water flooding their L. production can be considerably in- creased. This practice consists in injecting water under pressure into the sand surrounding an oil well, thus displacing the oil in the pores of the sand and forcing it into the oil well.

Jan 1, 1940

By F. D. Mahone

Much crude oil, as produced from the well, carries varying amounts of water, which may be present as free water in globules sufficiently large to settle out, in time, if the fluid is allowed to stand, or as an emulsion formed by myriads of minute water particles, each surrounded and entrapped by a film of oil through which it cannot break under the action of gravity alone. Such an emulsified mixture of oil and water is commonly termed "cut oil." When such an emulsion is subjected, under proper conditions, to the influence of a high-potential alternating-current field, the minute water particles rupture the enveloping oil films and coalesce into larger water droplets this procedure continuing until all the water is freed into drops of such size that they readily settle out. This action has been photographed by the micro-moving-picture camera; under the microscope, the breaking-up of the emulsion, as described, is seen to be accomplished in a few seconds. The low power requirements of the process, from records of commercial plants, substantiate the theory that the action is that of a multitude of electrical condensers in series, rather than that of a number of conducting paths. The minute water particles serve as the metallic elements, or plates, of the condensers and the separating oil acts as the dielectric. Such surface charges as the particles may have are removed, and the intervening oil is broken, probably electrically by the voltage and mechanically by the attractive force between adjacent oppositely electrified particles. The principle of breaking up an emulsion under the influence of an alternating electric field was discovered by F. G. Cottrell and Buckner Speed, through experiments conducted, at the University of California, which resulted in a plant being installed on the property of the Lucile Oil Co. in the Coalinga field, California, early in 1909. This plant was able to reduce 14-per cent. emulsion to less than Pper cent. with commercial success. Standard Cottrell Apparatus The present standard Cottrell apparatus consists essentially of the electric treater and a settling or trap tank. The treater is a galvanized-iron tank approximately 3 ft. in diameter and 10 ft. high, which con-

Jan 1, 1924

By M. C. Flemings, A. A. Tzavaras

Analytical and experimental procedures are descrihed for quantitative determination of volume-fraction microporosity in metals by mimorarlio-graphg. The analysis assumes spherical pores but allows for the observed fact that pores or portions of pores smaller than a given thickness do not project an image on the film. Volume-fraction microporosity was measuured in cast low-alloy steel and shown to vary from 0.6 x 10-4 to 10 x 10 depending on mode of solidification and on whether the material was air- or vacuum-cast. The aim of work described herein was to develop a method of quantitative measurement of the volume fraction of microporosity in cast metals. Microporosity, present in nearly all castings and ingots, is always interdendritic in nature and may be large enough to be seen on a polished surface with the naked eye. More generally, it is smaller in size, and its detection more difficult. Three techniques might be considered for measurement of microporosity: 1) lineal analysis of a polished metallographic surface, 2) density measurement, or 3) quantitative microradiography. As will be shown later, volume fractions of porosity in directionally solidified castings may be the order of 10-4 to 10-3; such small amounts of porosity are difficult to identify and measure on a polished surface. Density measurement is also not a suitable technique (for alloys) when the volume fraction of porosity is low. This is because the density of the base metal is often not known within the necessary accuracy, due to microsegregation or partial phase transformations. In general, it is not possible to completely eliminate microsegregation without also altering the porosity. Because of the limitations of the foregoing techniques, quantitative microradiography was employed to determine amount of porosity. In recent work, microradiography has been found to be useful for qualitative measurement of porosity, including determination of size and shape of individual pores;&apos;)&apos; however, quantitative determination of amount of porosity has not been attempted. I) CALCULATION OF VOLUME-FRACTION POROSITY The following analysis employs procedures similar to those of Cahn and Nutting3 and Hilliard.4 Major simplifications are that pores are assumed to be spherical and to be present in sufficiently small quantities that no overlapping occurs. A basic difference from the previous treatments is that the limited "sensitivity" of microradiography is considered. Assume first 1) cavities are spherical and of uniform diameter, 2) cavities are randomly distributed, 3) volume-fraction porosity and specimen thickness to pore radius ratio are sufficiently small that overlapping of the projected images of cavities is negligible, 4) sensitivity is limited (i.e., holes or portions of holes of less than a given thickness do not project an image on the film). The sensitivity, is defined as: where 5 = minimum thickness of void from which an image will be projected on the film and t = specimen thickness. Now, from Fig. 1, it is possible to distinguish between two different types of holes. These are 1) holes whose centers lie within the region t/2 > X > 6/2, where X is distance from one surface of the specimen (positive into the specimen), and 2) holes whose centers lie within the region (6 — r) < X < 6/2, Holes whose centers lie outside X = (6 -r) project no image on the film. These two types of pores are considered separately below. Type 1 Pores. When 6 is greater than 0, the image of a spherical cavity of radius r appears on the film as a circle of radius a which is smaller than r. From geometry, Fig. 1: a2=r2-52/4 [2] where a = radius of image of pore on film and r = radius of pore. Since the pores are randomly distributed and spherical V =4/3pr2Nv [3] where V = volume fraction of voids and Nv = number of pores per unit volume and the number of images of Type 1 pores per unit area of film, N&apos;A, is

Jan 1, 1965

By C. R. Simcoe, T. J. Koppenaal

The effect of direct and alternating currents on the quench aging behavior in an Al-4 pct Cu alloy has been investigated by use of resistivity measurements. The reaction rate increases with direct current density in the investigated range of 1000 to 3000 amps per sq cm. Alternating current of a specific frequency is observed to decrease the reaction rate by a factor of about two. ErDMANN-JESNITZER et al.,1,2 investigated the effect of direct and alternating current on the quench and strain aging behavior of low-carbon iron. In both cases they observed that direct current accelerates the aging reaction and that an alternating current can completely inhibit the aging process. The purpose of the present research was to investigate these phenomena in the quench aging behavior of an Al-4 pct Cu alloy and to determine the correlation, if any, between the increase in the observed reaction rate and possible heating effects accompanying the aging with direct current. EXPERIMENTAL PROCEDURE The aluminum-base alloy used in this investigation contained 3.98 wt pct Cu (1.72 at. pct) with impurities of 0.003 pct Si, 0.002 pct Fe, and 0.001 pct Mg. The alloy was rolled into a ribbon about 0.36 mm thick and 3.7 mm wide. The ribbon was split end from end with the ends being used as electrical contacts and the central unsplit section, about 5.3 cm in length, serving as the specimen. Solution treatment was accomplished by quenching from a salt bath at 520° ± 2°C into water at 25° ±0.5°C; the specimen was immediately transferred to a liquid nitrogen bath. All aging was done at 75° ± 0.2°C in a rapidly stirred ethylene glycol bath. Resistivity measurements were made by the double potentio-metric method employing a standard resistor; for purposes of convenience, the resistance measurements were made at 77°K. The transfer of the specimen from the aging bath to a liquid nitrogen dewar was accomplished in less than 1 sec. The aging kinteics were studied with the specimen being aged under the influence of direct current, alternating current, and without any type of current. The amount of heating caused by direct currents was investigated by soldering a thermocouple on the specimen surface and measuring the temperature change after applying various current densities. The temperature was observed to increase (from 75°C, the aging temperature) about 0.8°, 3.0°, and 8.5°C with direct currents of 1000, 2000, and 3000 amp per sq cm, respectively. When employing alternating current, the circuit was monitored with an oscilloscope and adjustments made to produce a normal sine-wave pattern. RESULTS Prior investigations3&apos;4 in the aging characteristics of A1-4 wt pct Cu have shown that the resistivity initially increases, reaches a maximum, and then decreases to values significantly lower than the as-quenched resistivity. This type of behavior is seen in Fig. 1 which shows the resistivity at 77°K as a function of aging time at 75°C observed in this investigation. At this aging temperature, the resistivity maximum is seen to occur in about 1 to 1-1/2 min and it further decreases to the as-quenched value in about 24 min. The behavior observed with the application of direct currents of 1000, 2000, and 3000 amp per sq cm during aging is shown in Fig. 2. With increasing current densities, (+) ?pmax decreases and the rate of the aging process increases. The time necessary to reach the as-quenched resistivity value decreases from 24 min for aging without current to about 16, 10, and 7 min for aging with 1000, 2000, and 3000 amp per sq cm direct current, respectively. Fig. 3 shows the results obtained when two changes were made during the aging with 2000 amp per sq cm

Jan 1, 1963

By S. D. Dahlgren

ORDERED G.P. zones having the cesium chloride structure were found to exist in the bcc iron-rich grains of an Fe-Au-Cu alloy that had been supersaturated with approximately equal atomic percentages of gold and copper, and aged at 400° and 350°C. Streaks and superlattice spots in electron diffraction patterns revealed the presence of the ordered zones in the aged material. The ordered Ll2 structure is commonly found for precipitates in fcc metals (e.g., Ni3A1 in nickelL7&apos;) but it is uncommon to find precipitates in bcc metals having the cesium chloride structure. The formation of the G.P. zones caused age hardening of the grains. Samples containing 3.8 at. pct each of gold and copper (with the remainder being iron) were annealed at 95@ or 1125°C in quartz capsules and were quenched by breaking the capsules under water. X-ray diffraction patterns revealed two solid solutions in the quenched samples. One solid solution was bcc and the other was fcc. The microstructure consisted of iron-rich grains of 0.3 mm diam surrounded by a yellow gold-copper-rich grain boundary network. The Au-Cu phase diagram %hows continuous solid solubility of gold and copper with ordered phases forming below 410°C. None of the ordered Au-Cu phases have the cesium chloride structure. Both Fe-Au and Fe-Cu phase diagrams3 show extended miscibility gaps and only terminal solid-solution phases. Consequently, it is reasonably certain the iron-rich grains consisted of an a-phase terminal solid solution, and the grain boundary network consisted of a gold-copper-rich terminal solid solution. Lattice parameters of the quenched solid solutions were consistent with the suggestion that the quenched phases were terminal solutions. The lattice parameter of the bcc phase (2.879A) obtained upon quenching from 950°C was higher than that (2.866A) for pure iron. The fcc phase in this sample had a lower lattice parameter than that for a 50 at. pct Au and 50 at. pci Cu solid solution, i.e., 3.866 compared to 3.877A. The lattice parameter for the 50 pct Au and 50 pct Cu solid solution was interpolated from data for Cu-Au solid solutions.4 More gold and copper were soluble in iron at 1125°C than at 950°C as indicated by a 0.012A increase in the bcc lattice parameter for a sample quenched from 1125°C. After the alloy had been quenched from 950° and 1125°C, the bcc lattice parameters were 2.879 and 2.891A1 respectively G.P. zones having the cesium chloride structure-which formed during low-temperature aging—were detected by electron diffraction and observed with electron transmission microscopy. In Fig. 1, the asymmetrical streaks parallel to ( 100) directions indicate that platelike G.P. zones had formed parallel to (100) planes of the matrix. The direction of streak asymmetry shows that the bcc unit cell of the G.P. zones was larger than the bcc cell of the matrix. The ordered cesium chloride structure is indicated by low-intensity superlattice spots at 010 positions which are nonallowed for bcc structures. The superlattice spots are streaked; therefore they are from the G.P. zones and are not caused by rel-rod effects of a thin matrix phase. The appearance and size of the zones observed in electron transmission microscopy and the appearance of the asymmetrical streaks in the electron diffraction patterns for the Fe-Au-Cu alloy were the same as those observed for a similarly treated Fe-Au alloy.&apos; Ordered G.P. zones were detected also for an Fe-Au-Cu sample aged only at 400°C. The production of the ordered cesium chloride structure zones by low-temperature aging of super-

Jan 1, 1968

By J. F. Butler

Boron nitride, BN, has been identified in boron low-carbon steels by means of light microscopy, electron microscopy and diffraction, and chemical analysis. This boron nitride is responsible for strain aging suppression in these steels through the removal of nitrogen from solution; however, small oxidizing potentials which result in deboronization In the austenitic temperature range also result in boron nitride decomposition and the subsequent occurrence of nitrogen strain aging. THE addition of boron to low-carbon steels is an effective means of eliminating the detrimental effects of strain aging;&apos;,&apos; however, the mechanism by which boron suppresses strain aging has not been established. In studying the effect of heat treatment on the strain aging of boron low-carbon steels, Butler3 found that no detectable nitrogen was present in the ferrite solid solution after various heat treatments even though the total nitrogen analyses of the steels were 0.003 pct N. Apparently the function of boron in suppressing strain aging is the removal of nitrogen from solution to form a relatively stable second phase. A clue to the identity of this phase was found by Speight4 who extracted from an aluminum-killed boron steel an acid insoluble residue which contained boron and nitrogen in proportions corresponding to the compound, BN. Shyne and Morgan5 found that the addition of nitrogen to a hardenable boron steel lowered its hardenability in a manner which suggest-d the presence of nucleating particles (presumably BN) even at high austenitizing temperatures. Although this indirect evidence for the presence of boron nitride in boron steels has been found, the compound was not identified metallographically as a separate phase in these steels. Because boron has an affinity for oxygen comparable to that of silicon,5 boron steels must be thoroughly killed with aluminum in order to prevent the reaction of boron with oxygen.7 The affinity of boron for oxygen also is demonstrated through the ease of deboronization of a boron steel in an oxidizing atmosphere. Digges, Irish, and Carwile8 found that a mixture of wet natural gas and air caused both deboronixation and decarburization of a boron steel at 1900°F. The boron content rose at the surface of the steel due to the formation of boron oxide. Shyne and Morgan9 encountered deboronization at much lower oxygen potentials; loss of boron occurred in steels treated at 1750o F under argon purified to 0.0014 pct 0, even though decarburization did not occur. Boron oxide, B2O3, is much more stable than the nitride, BN, as is indicated by the standard free energies of formation at 980oC: -235 kcal per mol of B2O3 (liquid) and -28 kcal per mol of BN (crystal). It is evident that the oxygen potential must be kept low in the presence of BN in order to prevent its decomposition and the subsequent formation of B2O3&apos; The purpose of the work described in this paper was to identify the nitride phase responsible for the removal of nitrogen from solution and to study its stability under oxidizing conditions. IDENTIFICATION OF BN In order to identify the phase containing boron and nitrogen, several alloys high in boron and nitrogen were made up in a small vacuum furnace. In alloys 3 and 4, Table I, electrolytic iron was used as a charge material. Boron additions were made in the form of 18 pct B ferro-boron after the iron was molten. In the case of alloy 3, the charge was solidified at this point; for alloy 4, nitrogen at 1 atm pressure was admitted over the melt before it was

Jan 1, 1962

By S. Arthur Krom

(New York Meeting, February, 1912.) THE James diagonal-plane slimer is specially adapted to handle the finest slimes, but it will also handle sands as coarse as 40-mesh. The saving efficiency of this machine is due to the original construction of the deck, and to the rapid reciprocating movement imparted to it by the head-motion. The deck consists of a plurality of connected planes, having a certain fixed ratio of inclination one to another. These planes intersect each other diagonally to the stroke-line of the table and are arranged so as to give the pulp on the table a double treatment. This double concentration performed by the diagonal-plane deck produces cleaner concentrates and tailings than those obtained by the operation of two separate machines. The action of the diagonal planes settles, combines, and holds all the concentrates in one compact mass, sharply defined from the gangue, and easily cut away without loss. Many slime-concentrating machines distribute the feed-pulp for a distance of 4 or 5 ft. only, and upon a very limited settling-surface. This results in a thick, heavy deposit, from which it is impossible to stratify the values and wash, away the gangue, the resulting products being dirty concentrates, and tailings carrying high values. The diagonal-plane slimer distributes the feed-pulp for a distance of 10 ft., and upon a settling-surface having an area of 40 sq. ft.; in other words, it spreads the pulp thinly on the table, which allows the metallic values to settle through the gangue quickly, forming a bottom stratum from which the thinly-distributed overlying stratum. of gangue is easily brushed away by the feed-water without disturbing the underlying concentrates. Referring to Fig. 1, plane A is the main settling-section, of the table. The feed pulp flows gently down this plane and is

Jun 1, 1912

By F. F. McINTOSH

STEEL is a general name applied to the alloys of iron and carbon. These alloys always contain , other elements such as manganese, silicon, sulfur, and phosphorus. Manganese and silicon are usually considered to be alloying elements. Sulfur and phosphorus are regarded as impurities. Tradition has damned them both and, in addition to classifying them as impurities, has established the general impression that many of the ills of steels are the result of the presence of one or both of these elements. Metallurgists are inclined to question the soundness of this tradition. The fact that one blast-furnace plant is devoted entirely to the production of ferro-phosphorus which is used to rephosphorize basic open-hearth steel, and that sulfur is added to many heats of steel, indicates that these so- called impurities might also be classed as alloying elements, and that the tradition which damns them may not be altogether fair and well founded. A critical search through the technical literature on the effect of phosphorus on steel will disclose many references to its harmful effect. Most of these are general in character, but there has been a strong tendency to accept this traditional belief in the harmful effect of the element.

Jan 1, 1926