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By Charles Luner

ALTHOUGH the kinetics of the atmospheric oxidation of tin have been studied,1-3 the kinetics in pure oxygen have not been reported. This note presents some results of the kinetics of the oxidation of tin foil in pure oxygen. The tin foil used in this investigation was 99.78 pct pure, the two major impurities being Pb (0.17 pct) and Sb (0.024 pct). The foil was degreased and air-dried prior to oxidation. The air-formed film was estimated by coulometric reduction4 of the surface oxides to be about 25A. The samples, which were in strip form and had a total geometric surface area of about 300 sq cm, were first evacuated at room temperature in an oxidation bulb to 1 X 10 -5 mm Hg and subsequently degassed for 1 hr at the temperature of the experiment. Spectroscopically pure oxygen was then introduced into the bulb. The rates of oxidation were measured by following the rate of pressure change due to oxygen consumption in a closed system, the volume of which was sufficiently large so that the pressure change during an experiment was 10 to 15 per cent of the total pressure. An oil-mercury manometer,5 with a sensitivity of 3 X x mm Hg (which corresponds approximately to 5 X 10 -7 gm of oxygen) was used to measure the pressure change. The oxidation bulb was heated by an oil-bath and controlled to within -10.3 C. The reproducibility of the rates was good, as determined by the coincidence of rates at 190oC for duplicate experiments. Fig. 1 shows the oxidation curves in the temperature range 168 to 211.5oC at 8 mm Hg pressure. The effect of pressure on the rate of oxidation at 190°C is also shown. The rate of oxidation was not markedly affected by changes in pressure in the range 4 to 9 mm Hg, except perhaps at the lowest pressure, 4 mm Hg, where after about 70 min there appeared to be a decline in the rate, as compared with the rate at the higher pressures. At the lower tem- perature, 168oC, and for short reaction times, it is difficult to distinguish between a linear relationship and a slight curvature in the oxidation rate. However, for longer times, there was a somewhat larger indication of curvature. The samples after oxidation were gold-colored in appearance. The oxide that was formed at 170°C was identified as a-SnO by reflection electron diffraction. This is in agreement with results obtained by other workers.6, 7 The rate data best fitted the logarithmic-oxidation rate law, w = K1n ln(1 + -t/to) [1] where w is the weight of oxygen consumed, t is the time, and K In, and to are constants. First estimates to were obtained according to the method of Taylor Thon8 and were then employed to obtain the best simuItaneous estimates of to and K In, that would fit the logarithmic expression. These estimates were found numerically, so that the residual variance could be minimized. The calculations were performed on an

Jan 1, 1961

President MRS. THOMAS T. READ 9 Windmill Lane Scarsdale, N. T. First Vice-President MRS. FELIX E. WORMSER Acorn Lane Larchmout, N. T. Second Vice President MRS. W. SPROTT BOYD The Carlyle, Madison Ave. and 76th Street New York, N. Y. Third Vice-President MRS. LOREN W. KEMP El Chico, Plainfield Avenue Metuchen, N. J.

Jan 1, 1944

By Zay Jeffries

Rearmament superimposed on buying sprees by the public, caused a general shortage of metals in 1911. and the rare metals were no exception; they also shared with the more common metals the uncertainty of future demand. In general, the apparent undersupply of metals is a favorable condition for the realization of sleeping possibilities of the rare metals, especially if the supply can he made sufficient to take care of the possible new demand. Many changes in metal usage in 1941 were forced because of shortages. When such changes are in the direction of the economic trend there is a speeding up in the tempo of the inevitable change, but when the forced changes are against the economic trend they are likely to be shortlived. In any event, the latter is not a solid foundation on which to build a future business.

Jan 1, 1942

By Newell G. Alford

With the workable area of coal prospected and known as to workability and quantity and sampled and tested for desired quality comes the determination of the projection and method of working. The best method will be the one supplying the greatest degree of safety, the most merchantable product, the minimum average cost per ton with the largest yield of recoverable coal. Based on coal elevations, taken at the bottom of the seam on all known outcrop exposures, prospect openings or drill holes, coal contours are made on the map to be used in developing the mining plan. The contour interval should be as close as available information will permit. For general utility in layout of mining, haulage, drainage and ventilation, a map scale of 400 ft. per in. is preferable. In mountainous sections, location of the main out- crop opening or hoisting shaft is often limited by the available railroad route and amount of land level enough for a plant site. In level country, where a tipple and hoisting shaft may be placed at will, choice of the plant site should depend on the minimum average underground haul for the total coal to be worked to the new

Jan 1, 1932

By D. Perry, G. W. Binkley, G. K. Dumbauld, F. A. Brooks

A new cementing technique has been developed which is particularly applicable to permanent-type well completion operations. The technique makes use of the accelerating effect of calcium chloride on setting time and strength development of cement cake deposited in squeeze cementing. An unique feature is that the accelerator is applied after the unaccelera-ted cement slurry has been squeezed and the excess has been reversed from the well. Laboratory data on the accelerating effect of calcium chloride applied to the fi1ter cakes of three low-water-loss cementing compositions demorzstrate that the procedure results in relatively rapid development of strength and impermeability of the cement cake. Simulated squeeze-ceinenting tests made in the laboratory likewise corroborated the practicality of the procedure. The laboratory tests showed that a newly developed oil-emulsion cemerzting composition is more susceptible to acceleration of set than are modified cements containing high percentages of bentonite. The acceleration procedure has been used successfully in field operations. INTRODUCTION Nature of Problem In squeeze-cementing operations, a substantial amount of time is consumed in waiting on the cement to develop strength after it has been squeezed into the well. Frequently, an interval of 18 to 24 hours or longer is required for the development of strength sufficient to prevent failure of the cement during subsequent operations in the well. Reduction of this waiting-on-cement time offers appreciable savings both in time and in money. A particular type of squeeze-cementing operation to which an increasing amount of attention has been given is encountered in permanent-type well completion operations wherein perforations are to be squeezed off1. In this procedure, it is customary to pump the cement slurry down the tubing and out into the perforated section through a retractable extension pipe. Squeeze pressure is then applied, which forces the cement slurry into the perforations and causes the build up of a compact filter cake of cement within the perforations. The excess slurry remaining in the hole is then removed by reverse circulation. The extension pipe is then retracted, and, if a new interval is to be perforated, a perforating gun is run through the tubing. The newly perforated interval may then be tested by swabbing. In such operations, it has been customary to allow approximately 20 hours or so for hardening of the cement squeezed into the perforations. This time interval is usually measured from the time that the cement is reversed out of the hole to the time that subsequent swabbing is started. If the cement has not developed strength at the commencement of swabbing, the pressure differential caused by swabbing results in failure of the squeeze job. At the time that the work described in this report was initiated, particular consideration was given to the reduction of waiting-on-cement time in squeeze cementing by the permanent-type completion technique. Consequently, much of the experimental work was directed to this specific objective, though the process which was developed for acceleration of strength development has possible application in other than permanent-type completion operations. Method of Attack Although quick-setting cements

Jan 1, 1957

By Freeman Bishop

This year the metal mining industry is in for some difficult decisions as the nation struggles to control inflationary pressures resulting from higher production costs and a money-squeeze policy. Re- clouding these problems will be campaign oratory as Congress seeks reelection. Charges will be hurled back and forth between a Republican White House and a Democratic Congress. Inflation and Vietnam will be the big one. Hut pollution i. coming on strong. President Nixon has formed a new Council on Environmental Quality although he already had named a similar unit within his Cabinet six months ago. Both are charged with bringing 1.0 bear all of the Federal Government's talents on the focal points of antipollution measures The biggest task will be to find out how many different "units" are currently mixed up in these efforts.

Jan 1, 1970

By G. Cartaud, F. Osmond

We have already devoted two previous memoirs to this question. In the firstL we collated and discussed the existing literature on the subject; in the second: we described the crystalline forms obtained by the reduction, at different temperatures, of ferrous chloride by hydrogen or by zinc-vapor. The conclusion from these researches was that the three allo-tropic states of iron—a, stable below A2; , stable between A2 and A3; and , stable above A3—all crystallize in the cubic system. The differences observed were such as are customarily encountered in the crystallographic records of many minerals of which allotropic varieties or isomerides are not known, and did not conform to the ordinary definition of polymorphism. It is, however, improbable that allotropic transformations, which are placed beyond doubt by a series of positive facts, do not involve some changes in the intimate structure. As a matter of fact, the crystals we did obtain were too small to allow of a precise examination, and this might introduce an element of uncertainty in the firm establishment of our conclusions. Professor H. Le Chatelier mas even led to think from some of our results that r-iron could very well be a rhom-bohedron simulating a cube, and not a true cube, and it will be remembered that the crystalline form of bismuth was for a long time incorrectly regarded as cubic. Allotropy does not, however, necessarily involve such a deduction. Without departing from the cubic system at all, a whole

Jan 1, 1907

By Michael Tenebaum

IN a previous investigation1 the authors studied the effect of pressure on the reduction of iron ores by hydrogen. With hydrogen as a reducing agent, the rate of reduction was increased substantially by increasing the pressure from 1 to 2 atmospheres. The results with hydrogen prompted the present study of the effect of pressure on reduction with carbon monox-ide and with mixtures of carbon monoxide and nitrogen. FEATURES OF REDUCTION PROCESS The gas stream in the lower part of the blast furnace always contains sufficient concentrations of reducing gases to complete reduction provided sufficient time is allowed for the reaction to proceed. Reducing gases react immediately with the iron oxide on the surface of lumps of ore. However, as the unreduced surface recedes from the easily accessible exterior of the lump, the reaction proceeds by virtue of the diffusion of the gases into and out of individual pieces. The rate of diffusion of gases, which undoubtedly plays an important role in the reduction of iron ores, depends on several factors, most impor-tant of which are: (1) molecular weight or density, (2) pressure, (3) tem-perature, (4) concentration gradient. Thus, the rate of reduction of a lump of iron ore at any temperature will depend not only on the specific reaction rate but also upon: (1) available surface of unreduced iron oxide, (2) rate of diffusion of the reducing gas to the reacting surface, (3) rate of effusion of the gaseous products of the reaction from the reacting surface, (4) adsorption of the gases on the reacting surface.

Jan 1, 1939

By W. O. Philbrook, A. H. Jolly, T. R. Henry

In the course of a study of slag-control methods, the authors devised a laboratory technique by which the basicity of basic open-hearth furnace slags could be estimated with sufficient accuracy to make the method of possible interest for slag-control purposes. The process consisted of measuring the slight basicity of an extract of the powdered slag in water. The procedure was presented, for the benefit of those who might care to experiment with it, in a paper submitted in the 1944 McKune Award Contest and presented at the 1944 Open-hearth Conference in Pittsburgh.' Interest expressed at that meeting and favorable operating experience with the method at a neighboring plant, as described in a related paper by Michael Tenenbaum and C. C. Brown,; have encouraged us to present further details of the development, technique, and pitfalls of the method and some additional data not included in our first report. At the outset it must be admitted that this method of estimation of slag basicity is not perfect; neither is any other that we know of. It is subject to somewhat greater errors than would be desirable, but compares favorably with other techniques in this respect. It has the disadvantage that it places the final determination of slag basicity in the hands of a laboratory technician rather than the furnace oper- ator, although it can be operated in a control laboratory adjacent to the furnaces. It requires close attention to certain details, as do most laboratory procedures. On the favorable side, it eliminates the "human factor" of personal judgment inherent in estimation from pancakes or powdered samples. The procedure can be placed in practice much more rapidly and presents much less of a training problem than visual methods of estimation. The principle and operation of the method are so simple that it would not be surprising if others have experimented with the same or similar procedures, but we are not aware of any prior publication of details. Our own shop has been operating fairly successfully for several years with the aid of slag pancakes. Since the past year or two have not been favorable for the expenditure of time and energy where the need was not urgent, we have not introduced the new practice for actual slag control and hence do not have extensive operating data. In presenting this method, therefore, we make no claims as to theoretical justification nor guarantees as to practical applicability, but offer it as an empirical observation. We believe it has sufficient merit to warrant its investigation by those just instituting a slag-control program or in search of supplementary methods for judging slag basicity Principle of the Method It is well known that when burnt lime or slaked lime is shaken up with water it

Jan 1, 1945

By F. F. Frick, Frederick Laist

In a leaching process, having obtained the copper in solution, the choice of the precipitation method is influenced by the following factors: 1. Availability of precipitant. 2. Adaptability to the leaching process. 3. Final product desired. 4. Regeneration of leaching solutions. 5. Fouling of solutions. There are three general classes of precipitation methods: 1. The use of iron, scrap or sponge. 2. Electrolytic deposition. 3. The use of some gas or reagent by which the copper is obtained, usually in the form of an intermediate precipitate which requires further treatment. For example, the precipitation of, the copper as Cu2Cl2 from chloride solutions; with SO2 gas. The use of iron is adapted to almost any process. It has the great advantage of extreme simplicity, and the recovery of the copper and any values present in a highly concentrated, easily treatable form. The disadvantages are the cost in isolated places, the uncertainty of the scrap-iron market, and the fouling of the leaching solutions. The latter is a serious factor, when a reagent such as salt is used in them, which makes necessary their re-use. Where applicable, electrolytic deposition is very attractive. The copper is obtained in a form directly marketable, there is a regeneration of acid and no fouling of solutions. Unfortunately, chloride solutions do not lend themselves to electrolysis. An entirely satisfactory anode material has not yet been discovered, although magnetite, apart from being rather brittle, seems to answer the requirements fairly well. The use of a method of the. third class is involved in many special

Jan 1, 1915

By H. Rush Spedden

R. T. Hukki has extended his study of ball mill grinding at supercritical speeds with an excellent mathematical analysis of tumbling mill grinding. When he speaks of supercritical speeds he is referring to the original Fahrenwald critical-speed formula. He said that, as an example of the use of supercritical speeds, if a fine grinding mill of any type is wet-grinding ore of 3.5 sp gr with steel balls at a certain conventional subcritical speed, the same power input and capacity should be obtainable with autogenous medium of 3.5 sp gr at a speed 100 to 120 pct of the critical in a grate- type mill of the same effective size. In addition, he introduced what he calls the base mill concept which, he stated, makes it possible to compare performances of mills of different sizes grinding with a metallic medium or with an autogenous medium of any specific gravity and at any speed. He showed the use of this concept and explained how it makes possible the evaluation of mill sizes and motors for any grinding purpose at any accuracy well within the conventional standards of design in milling practice. He further stated that the maximum capacity in pilot plant mills with various media, either metallic or autogenous, has always been found to be within the supercritical speed range. In his discussion of this paper he substantiated these findings with statements showing the increased capacity obtained in a milling plant in Finland which followed his principles.

Jan 7, 1960

TULSA, the host of the Petroleum Division this year, is the oil metropolis of the Mid- Continent and gateway of the Southwest. It has risen in less than three decades from a dusty cattle town of less than 1000 population to its present-day status of a modern, wide-awake and prosperous city of close to 150,000, with an assessed realty valuation of approximately $100,000,000. Oil was discovered near Tulsa in 1901, and with it came th.2 development of the Mid-Continent field, one of the richest in the world. Tulsa from the start has been the center of operations, and its location on foul- and aggressive application of the airplane to oil-field requirements tends to fix this status as production is developed farther and farther afield. That Tulsa is far more than an ephemeral oil town is punched into the newcomer's- especially the Easterner's-mind, as he is whisked by taxi from the railroad station to the Hotel Mayo. The cicadalike pounding of the riveters on the steel skeletons of many skyscrapers, mounting upward to fill the gaps in an already well-developed skyline, dispels the feeling of a new atmosphere and puts him back on Forty-second Street, Michigan Boulevard or whatever his own particular "Main Street" may be along which an American city is being remade. Practically every company of any importance operating in the Mid-Con-

Jan 1, 1928

By A. B. Kinzel

THE year 1936 has been an eventful one in the iron and steel industry. Renewed industrial activity has brought with it many new problems. These problems have generally involved the question of increasing capacity without sacrifice of economies and quality developed in the less active previous years. The nature of the iron ore used and the effect of its porosity and other physical characteristics on the capacity of the blast furnace has been reviewed by the U. S. Bureau of Mines. The whole question of handling raw materials and methods of charging furnaces has been intensively studied, with the result that capacity has been in- creased without affecting the quality of

Jan 1, 1937

INTRODUCTION The first installation of large, commercial, high gradient-high field cannister and matrix magnetic separators for removal of impurities from kaolin was made in 1973 (1). Since then the technology and equipment have been widely adopted for clay processing with about 12 units in commercial use. These new separators have filled a need, caught the imagination of many and become a technology worth fighting for. A fight has occurred, and a resolution on royalties for kaolin processing, at least, has been achieved. LIMITATIONS TO APPLICATIONS OF MAGNETIC SEPARATORS Other than the use of these magnets on kaolin clay, no other application has yet achieved widespread adoption. Dr. Iannicelli blames inertia, and1 would agree that it is a factor. There are other reasons too, and if they are examined, they may isolate problems that R&D can significantly assist in solving. I'd like to break the problems into two areas. Machine limitations - the mineral properties are there but performance is insufficient or uneconomic. Separation limitations - the mineral properties aren’t there, but the magnetic separation would perform well if the properties were there (size is right; concentration is right, etc).

Jan 1, 1979

By R. T. Mishler

Silver-gold. mine, in northern Mexico, with arrow veins in rhyolite. One fourth area developed has been ore. Deposits average 20 in. wide and 73 oz. silver per ton; diluted in mining to 40 oz. per ton. Developed by drifts and raises at 100-ft. intervals. Samples cut every 5 ft. Ore and waste sampled separately to make combined stoping width 3 or 3 1/2 ft. Ore reserves figured to sloping width; high assays not modified. Tonnage and assay of ore extracted higher than estimates. Ore stoped principally by cut and fill method. Cars from each stope counted and sampled. Cars check tonnage to concen¬trator within 1 per cent.; silver assay 9 per cent. high. Tonnage and assay from scopes corrected to agree with feed to concentrator. Profit or loss for each slope estimated monthly. THE Lucky-Tiger mine is a silver-gold property, situated at El Tigre, in the northeastern part of Sonora, Mexico, at, an elevation of 6000 ft. in the Sierra Madre Mountains. It is 30 miles by wagon road from the Esqueda station on the Nacozari railroad. Since its discovery in 1903, the mine has produced forty million ounces of silver. The ore has averaged 40 oz. silver and 0.25 oz. gold per ton. Copper, lead and zinc have been of minor importance, having averaged 0.4 per cent., 1.1 per cent., and 1.5 per cent., respectively. The richness of the ore,, combined with its occurrence in narrow veins, required the use of the more expensive methods of mining.

Jan 2, 1925

By George Espey, George Sachs, G. B. Kasik

IT has been reported frequently that the hardness and strength vary over the cross section of cold-worked, particularly cold-drawn, material. Brass rod and wire usually have been found to possess a maximum strength and hardness near the surface.1,2 According to Sachs,' the center fiber has about the same strength as a wire stretched by the same amount in a tensile-test machine, the strength increasing toward the surface (Fig. I). These differences are particularly large for wire given a small reduction on drawing through a die with a wide opening. However, with increasing reduction and hardness, a tendency to form a thin soft surface skin becomes apparent. On the contrary, copper wire has usually been found to possess a soft surface skin3-5 and it has been reported by Harris3 that during the cold-drawing of hot-rolled wire the surface layer becomes increasingly softer than the core, while the layer of maximum strength moves toward the core, it being found near the surface at first. The increase of strength and hardness from the core to the skin is readily explained by the observation that, in addition to the stretching, the layers of a rod or wire are sheared more the closer they are to the surface.1,6-8 However, the presence of a soft surface layer can be attributed only to an annealing effect. The source of such a softening might be the extremely high temperature that originates from the friction between

Jan 1, 1942

By G. B. Kasik, George Sachs, George Espey

IT has been reported frequently that the hardness and strength vary over the cross section of cold-worked, particularly cold-drawn, material. Brass rod and wire usually have been found to possess a maximum strength and hardness near the surface.1,2 According to Sachs,' the center fiber has about the same strength as a wire stretched by the same amount in a tensile-test machine, the strength increasing toward the surface (Fig. I). These differences are particularly large for wire given a small reduction on drawing through a die with a wide opening. However, with increasing reduction and hardness, a tendency to form a thin soft surface skin becomes apparent. On the contrary, copper wire has usually been found to possess a soft surface skin3-5 and it has been reported by Harris3 that during the cold-drawing of hot-rolled wire the surface layer becomes increasingly softer than the core, while the layer of maximum strength moves toward the core, it being found near the surface at first. The increase of strength and hardness from the core to the skin is readily explained by the observation that, in addition to the stretching, the layers of a rod or wire are sheared more the closer they are to the surface.1,6-8 However, the presence of a soft surface layer can be attributed only to an annealing effect. The source of such a softening might be the extremely high temperature that originates from the friction between

Jan 1, 1942

By Thomas M. Chance

All gravity methods for the separation of ore from gangue, or of slate and other refuse from coal, are based upon differences in the falling velocities, in some fluid medium such as air or water, of the materials to be separated. As all materials falling in a vacuum have the same velocity, independent of the size, shape, weight or specific gravity of their individual particles, it would be more accurate to describe the operation of these methods as depending upon the retardation of falling velocities effected by the resistance of a fluid medium, this retardation being greater for small or light particles than for large or heavy particles. This generalization is true also of those appliances utilizing centrifugal force to replace or to supplement the action of gravity. The separation of materials of different specific gravities by means of a fluid having a specific gravity greater than that of the lighter particles and less than that of the heavier particles has not been applied commercially, or on a large scale, to the separation of ores or to the washing of coal, the method being limited to laboratory experimental work or to laboratory determinations for the purpose of checking up the work of jigs, classifiers, and other types of concentrating appliances. A solution of zinc chloride has thus come into general use in the laboratory to separate coal, bony coal, and slate, both to check up the work of coal-washing plants and for the purpose of making tests preliminary to the designing of coal-washing plants. The use of a heavy solution of some chemical in water has often been proposed for making such separations, especially in connection with the washing or preparation of coal. Practically insuperable difficulties, however, have prevented the commercial development of any such process, the difficulties being both physical and financial. The cost of the chemical used to make high-gravity solutions is usually prohibitive, and the freeing of the coal from all traces of the chemical is found to be practically impossible. Such solutions inevitably penetrate the individual lumps and particles of coal, transfusing into the pores and saturating the joint-planes, and very large quantities of wash water

Jan 1, 1918

Bethlehem Steel Co. has just brought an all-new iron ore mine into production at Marmora, Canada, about 120 miles east of Toronto. High grade pellets produced at the mine from open-pit magnetite ore travel 64 miles by rail to the port at Picton, then go by Lake boat to help supply Bethlehem's Lackawanna, N. Y., plant. At full production about half a million tons of pellets a year will be shipped, and mining will be at a scale of more than a million tons per year of ore. Aeromagnetic surveys carried out in 1949 by the Ontario Dept. of Mines and the Canadian Geological Survey revealed an anomaly that interested Bethlehem geologists. By 1951 the company had put down some 40 diamond drillholes ranging from 460 to 1800 ft to block out the magnetite replacement deposit which lies in pre-Cambrian limestone below about 130 ft of Paleozoic limestone. The orebody, roughly 2100 ft long and up to 400 ft wide, averages about 37 pct iron, too low for direct shipment. Not only construction of concentrating and pelletizing facilities, but 20 million tons of stripping lay ahead before production could start

Jul 1, 1955

By F. V. Lenel, G. S. Ansell, J. A. Dromsky

The growth of aluminum oxide particles in a nickel matrix was studied eve?. the temperature vange of 2140° to 2470°F. The instability of the dispersed alumina was shown to be independent of the crystal structure of the alumina. The activation energy for the growth of the dispersed alumina was found to be 84.7 1 2.0 kcal. The particle radius increased as a function of time. These results indicate that the growth is not diffusion controlled. It is believed that the rate controlling mechanism is the dissolution of the aluminum and oxygen atoms into the nickel lattice. THE strength properties of alloys which consist of a finely dispersed second phase in a metallic matrix depend upon the spacing between the second phase particles. It is therefore desirable to achieve very fine dispersions in these alloys. Furthermore, to retain the properties these very fine dispersions must be stable during fabrication and service of the alloys. The best known of the dispersion strengthened materials, the SAP type alloys, which consist of a dispersion of aluminurn oxide in aluminum, have exceptionally good stability up to the melting point of aluminum. There is evidence, however, that other dispersion strengthened alloys, even those consisting of refractory oxides in a metal matrix, may be less stable. This investigation is concerned with the stability of Ni-Al2O3 alloys in the temperature range in which these alloys are usually fabricated. The mechanical properties of Ni-Al2O3 alloys at elevated temperatures have been previously investigated by Crelnens and rant,' and Gregory and Goetzel.2 The behavior of these alloys in stress rupture tests appears to indicate that at temperatures below 1800°F they are highly stable. There is some doubt, however, as to their stability at the higher temperatures used during the conventional fabrication. Cremens and Grant, in preparing their test alloys, cousolidated, by powder metallurgical techniques, nickel powders as fine as 0.13 µ diam and alumina powders as fine as 0.018 µ. Metallo- graphic examination of the alloys following fabrication revealed that none had interparticle spacings of less than 2 µ. Considering the size of the original component powder particles, it is likely that the dispersions coarsened during fabrication. Gregory and Goetzel, in their studies of extruded alloys of 80 pct Ni—-20 pct Cr matrixes with nonmetallic dispersion, observed a definite coarsening of the alumina dispersions in alloys sintered at 2280°F as cantrasted to those sintered at 2000oF. Similar observations on the spheroidization and growth of thoria particles finely dispersed in a nickel matrix were made by D. K. Worn and S. F. Marton.3 As a result of such coarsening, much of the effort expended in the preparation of very fine powder mixtures would be lost. The mechanical properties of the alloys which had experienced coarsening would be expected to be poorer than if the original dispersions had been retained. EXPERIMENTAL PROCEDURE Ni-Al2O3 alloys were produced from powder prepared by a coprecipitation technique. Aluminum hydroxide and nickel hydroxide were coprecipitated from chloride solutions of the metals. The mixed hydroxides were calcined to form metal oxides and the nickel oxide in the mixture was selectively reduced to nickel by treating it in hydrogen. Specimens were compacted from the resultant powder which consisted of a fine, uniform mixture of aluminum oxide and nickel particles. The compacts were sintered by resistance hot pressing4, a densification technique which requires exposure times of the order of only a second or less at elevated temperatures. A conventional sintering process was not used, since the temperature required for densification would have to be in the region in which the stability of the dispersion was to be studied. A series of hot pressed specimens were treated in hydrogen at temperatures from 2140o to 2470°F (1171o to 1355oC, for times up to 120 hr. Changes in the microstructures were studied by electron microscopy using the two-stage preshadowed carbon replica method.5 In performing a lineal analysis on a series of micrographs from each specimen it was found more convenient to determine the mean free path between alumina particles rather than particle radii as the parameter of growth. Although these quantities are directly proportional for only spherical particles, the alumina particles in these alloys

Jan 1, 1962