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By T. L. Joseph

THE committee appointed to investigate the application of oxygenated air to the blast' furnace believes, after a careful study of the problem, that this enriched air will increase hearth temperature, tonnage, flexibility of operation, and quality of pig iron made, and that fuel consumption will be decreased. These improvements are supported by theoretical evidence; but a practical trial of the process is necessary to establish more definitely the magnitude of benefits realized. The commercial application, however, may profitably be preceded by a test on a smaller scale. A small furnace will, in general, respond to the enriched air in the same way as a commercial furnace and the magnitude of the benefits to be gained from varying additions of oxygen can be fairly well established at relatively little expense. A new experimental furnace, being built jointly by the Bureau of Mines and the University of Minnesota, at Minneapolis, will have a capacity of about 6 tons and will riot require more than 700 cu. ft. of natural air per minute. Its hearth is 36 in. in diameter and its height about 32 ft. Enough oxygen to enrich the blast to the extent recommended by the committee can be obtained from a small oxygen unit. It might even be cheaper to perform preliminary experiments with tanks of oxygen obtained from regular, dealers. A procedure in making the test that suggests itself is to start with operation on normal air; then to use blast, enriched in several steps. Systematic temperature measurements of the tuyeres, slag, and metal would reveal any changes in hearth temperature. When these changes become large enough, the burden may be gradually increased to just within the breaking point and the furnace brought back to normal, if possible, by the addition of oxygen. Such a test would show what might be expected in the way of a decrease in fuel consumption and the time taken to "straighten up" the furnace by means of oxygen. The new furnace at Minneapolis is so equipped that the furnace process can be observed from the stock line to the iron notch. We have been taking gas samples at various elevations in the furnace to study combustibility of the fuel and the reducing power of the gas. If either of these is affected by removing inert nitrogen, the change can easily be measured.

Jan 11, 1924

By AIME AIME

ALMOST as many attended the annual dinner this year as last, when the presence of Mr. Hoover was such an attraction that almost two-thirds more than had ever attended before were present. Only by putting the late comers at tables in the balcony could everybody be accommodated. Past President De-Golyer was the toastmaster and in opening the post-prandial exercises referred to the regrettable fact that this was the last of the long series of dinners which have been held at the Waldorf, as the hotel will be torn down to give way to an office building before another year. To the delight of the gathering "Oscar" appeared and, in a delightfully brief but characteristic speech, referred to the long association that had existed and hinted that a new Waldorf-Astoria may arise, where the Institute could continue to gather annually in an enlarged replica of the room they had met in so long. Before taking up the presentation of the medals, Mr. DeGolyer referred to the Institute's "Legion of Honor," the 34 men who have been members continuously for over fifty years. For various reasons only five of them, W. S. Ayres, F. G. Corning, Henry D. Hibbard, A. F. Schneider and Arthur Thacher, could be present. They were all seated at the speaker's table, and W. S. Ayres, 56 years a member, as the dean of the group, was called on to respond for them all. He said: "The introduction I have just received would indicate that this particular group of men to which I belong is considered by the chairman to be a group of real antiques. Possibly you are questioning the accuracy of his judgment. I hope you are, although there may be some first-sight evidences tending to substantiate the view held by the chairman.

Jan 1, 1929

By H. Le Chatelier

SILICA brick are indispensable in the manufacture of steel because they alone are able to withstand the high temperature of regenerative furnaces. All attempts to replace silica brick by other refractory materials for this purpose have failed, but the reason for this failure has remained obscure; we shall give an explanation later in this paper. Before the war, silica brick employed in France came principally from abroad, for which reason, since the beginning of hostilities, certain French steel works have been seriously handicapped. Our attention was first directed to the question by M. Bred, Engineer of the Teil Works. With him, we began certain investigations, at first using our laboratory and the furnaces of neighboring steel works. The larger part of our experiments, however, have been made in the laboratory of the Faculty of Sciences at the Sorbonne. For the heating of our samples, we are deeply obliged to MM. Charpy, Yeatmann and Guérineau. In undertaking these studies, our first aim has been to render assistance to French industry, by indicating, as precisely as possible, the necessary conditions for the manufacture of high-grade brick; but at the same time we have intended to give an example of the manner in which scientific methods may be put to practical application in the solution of industrial problems. Although our work has been confined to samples of only a few grams, we are nevertheless convinced that our information can be directly utilized by brick-works of which the output is measured in thousands of tons

Jan 9, 1918

By H. l. Burghoff, E. C. Bohlen

The work reported in this paper was carried out to supplement the existing information concerning directional properties and recrystallization textures of annealed brass sheet and strip. These characteristics are of direct interest when the forming and drawing properties of such material are being considered. Among those who have made contributions in this field are Bass and G1ocker;l Bauer, Göler and Sachs;2 Phillips and Samans;3 Pratt;4 Price;5 Cook;6 Richards;7 Brick;8 and Brick and Williamson.9 These investigators have found, in general, that in brass strip that shows directional variations in properties, tensile strength has a minimum value and elongation has a maximum value at 45' to the rolling direction. The most pronounced directional properties have been found in material given the greatest reductions in rolling followed by high annealing temperatures. Recrystallization texture of brass has been variously reported as (II3)[II2], (ooi)[ioo], and a combination of (II0)[II5] and traces of the primary rolling texture, (110)[112]. The directional studies have been very informative, but actual tests appear to have been confined to material in its final condition. Tests at intermediate stages have received little attention although previous history of some materials has been partly considered. Perhaps the most comprehensive investigation was made by Cook,' who studied the directional properties of 70-30 brass strip for which the final and penultimate, or next to the last, anneals and the final reductions were varied. He found that, for any given combination of penultimate anneal and final reduction, the tendency toward the development of directional properties was reduced as the temperature of the final anneal was decreased. In addition to drawing cups and making tensile tests of the finished material at various angles to the rolling direction, he measured the frequency and the angles of twins in grains for several specimens. Plots of his twin counts showed directionality for the materials that produced eared cups. Test Materials and Equipment For this investigation, one commercial heat of 68-32 brass was cast in the form of bars for cold-rolling, I31/2 in wide and I1/2 in. thick. The analysis was as follows: 68.83 per cent copper, 0.04 per cent lead, 0.01 per cent iron, 31.12 per cent zinc (by difference). The bars were so processed to the final thickness, 0.020 in., as to obtain on this thickness all possible combinations of the variables listed below except those involving the sequence of 84 per cent penultimate reduction and 84 per cent final reduction: I. Penultimate reductions of 37 per cent, 50 per cent and 84 per cent; 2. Penultimate anneals at 800°, 900°, 1050° and 1200°F.; 3. Final reductions of 37 per cent, 50 per cent, 69 per cent and 84 per cent;

Jan 1, 1942

By E. C. Bohlen, H. l. Burghoff

The work reported in this paper was carried out to supplement the existing information concerning directional properties and recrystallization textures of annealed brass sheet and strip. These characteristics are of direct interest when the forming and drawing properties of such material are being considered. Among those who have made contributions in this field are Bass and G1ocker;l Bauer, Göler and Sachs;2 Phillips and Samans;3 Pratt;4 Price;5 Cook;6 Richards;7 Brick;8 and Brick and Williamson.9 These investigators have found, in general, that in brass strip that shows directional variations in properties, tensile strength has a minimum value and elongation has a maximum value at 45' to the rolling direction. The most pronounced directional properties have been found in material given the greatest reductions in rolling followed by high annealing temperatures. Recrystallization texture of brass has been variously reported as (II3)[II2], (ooi)[ioo], and a combination of (II0)[II5] and traces of the primary rolling texture, (110)[112]. The directional studies have been very informative, but actual tests appear to have been confined to material in its final condition. Tests at intermediate stages have received little attention although previous history of some materials has been partly considered. Perhaps the most comprehensive investigation was made by Cook,' who studied the directional properties of 70-30 brass strip for which the final and penultimate, or next to the last, anneals and the final reductions were varied. He found that, for any given combination of penultimate anneal and final reduction, the tendency toward the development of directional properties was reduced as the temperature of the final anneal was decreased. In addition to drawing cups and making tensile tests of the finished material at various angles to the rolling direction, he measured the frequency and the angles of twins in grains for several specimens. Plots of his twin counts showed directionality for the materials that produced eared cups. Test Materials and Equipment For this investigation, one commercial heat of 68-32 brass was cast in the form of bars for cold-rolling, I31/2 in wide and I1/2 in. thick. The analysis was as follows: 68.83 per cent copper, 0.04 per cent lead, 0.01 per cent iron, 31.12 per cent zinc (by difference). The bars were so processed to the final thickness, 0.020 in., as to obtain on this thickness all possible combinations of the variables listed below except those involving the sequence of 84 per cent penultimate reduction and 84 per cent final reduction: I. Penultimate reductions of 37 per cent, 50 per cent and 84 per cent; 2. Penultimate anneals at 800°, 900°, 1050° and 1200°F.; 3. Final reductions of 37 per cent, 50 per cent, 69 per cent and 84 per cent;

Jan 1, 1942

By J. Kent Smith

The object of this investigation was to ascertain the effect of varying percentages of beryllium upon pure copper and the properties of the resultant alloys in their softest condition, the effect of heat hardening on them, and the extents to which these properties could be augmented by different combinations of heat hardening and cold rolling. The data compiled in this paper represent partial results of continuing work done by the writer during the years 1930 and 1931, which was a continuation of the unpublished ground work incepted in the laboratory of the Beryllium Corporation of America by H. B. Pulsifer in the year 1926. A short bibliography on beryllium alloys is appended to this paper. It has, of course, long been known that copper subjected to cold work is hardened and strengthened to a considerable extent; furthermore it had been qualitatively noted in previous experiments that copper-beryllium alloys seemed to take on hardness and strength as the result of cold work at a greater rate even than does plain copper. It was decided therefore to endeavor quantitatively to determine such rate of increase, as also the relative increases by combinations of cold working and heat hardening. The results are summarized in Tables 3, 4 and 5. A preliminary series of experiments had indicated that by an exposure to the heat of 575" F. for 2 1/2 hr. age-hardening of a 2.50 per cent beryllium-copper alloy took place. Slab ingots of nine different beryllium-copper alloys were prepared under identical conditions by means of the addition of a previously prepared 12.5 per cent beryllium-copper alloy to well melted and deoxidized pure copper. The ingots were then reduced by hot rolling to 12 gage (about 0.080 in.). These strips were heated to 1450" F. and quenched in cold water, and thus brought to their softest condition. (See Table 1.) Strips were next "precipitation-hardened" by reheating to a definite temperature. Similar strips to those itemized in Table 1 (which had been quenched from 1450" F.) were reheated for varying periods of time at 575" F. The hardness figures show that a metastable condition, of which the range of stability is dependent entirely upon time at the given temperature, begins to be noted in copper samples containing as little as 0.85 per cent beryllium. It is extremely noticeable in samples containing

Jan 1, 1932

By J. Kent Smith

THE object of this investigation was to ascertain the effect of varying percentages of beryllium upon pure copper and the properties of the resultant alloys in their softest condition, the effect of heat hardening on them, and the extents to which these properties could be augmented by different combinations of heat hardening and cold rolling. The data compiled in this paper represent partial results of continuing work done by the writer during the years 1930 and 1931, which was a continuation of the unpublished ground work incepted in the laboratory of the Beryllium Corporation of America by H. B. Pulsifer in the year 1926. A short bibliography on beryllium alloys is appended to this paper. It has, of course, long been known that copper subjected to cold work is hardened and strengthened to a considerable extent, furthermore it had been qualitatively noted in previous experiments that copper-beryllium alloys seemed to take on hardness and strength as the result of cold work at a greater rate even than does plain copper. It was decided therefore to endeavor quantitatively to determine such rate of increase, as also the relative increases by combinations of cold working and heat hardening. The results are summarized in Tables 3, 4 and 5. A preliminary series of experiments had indicated that by an exposure to the heat of 575° F. for 2 1/2 hr. age-hardening of a 2.50 per cent beryllium-copper alloy took place. Slab ingots of nine different beryllium-copper alloys were prepared under identical conditions by means of the addition of a previously prepared 12.5 per cent beryllium-copper alloy to well melted and deoxidized pure copper. The ingots were then reduced by hot rolling to 12 gage (about 0.080 in.). These strips were heated to 1450° F. and quenched in cold water, and thus brought to their softest condition. (See Table 1.) Strips were next "precipitation-hardened" by reheating to a definite temperature. Similar strips to those itemized in Table 1 (which had been quenched from 1450° F.) were reheated for varying periods of time at 575° F. The hardness figures show that a metastable condition, of which the range of stability is dependent entirely upon time at the given temperature, begins to be noted in copper samples containing as little as 0.85 per cent beryllium. It is extremely noticeable in samples containing

Jan 1, 1932

By FREDERICK C. BROWN

THE practice of fine-grinding is now being so successfully - carried on in some fields, notably in West Australia, and its advisability has been so frequently pointed out' that the matter in this paper is not put forward as being new ; its chief object being to call attention to the importance of fine-grinding in the treatment of comparatively low-grade ores. I have been engaged during the last five years in the cyanide-treatment of ores in the Ohinemuri district (North Island), New Zealand, and I consider that, in the near future, extremely fine-grinding (almost sliming) will become a very important feature of the milling-methods in this field, since it seems absolutely necessary to reduce the most of ores to a very fine state of division if a high extraction is to be obtained; and, in most cases, the extra percentage of saving will leave a good margin above the increased cost of treatment due both to the fine-grinding and to the interest on the capital spent for the grinding-machinery. The average ore of the Ohinemuri field is composed of a quartz-gangue with some calcite, carrying the gold-value in the form of an alloy of gold and silver in about equal proportions, and the silver-value in the form of mixed sulphides of silver, usually associated with a considerable amount of iron pyrites. In the upper levels, the ores are decomposed and carry large quantities of black manganese oxide and some iron oxide, but, as. depth is reached, the decomposed ore gives place to sulphides and, in some mines, rhodonite, manganese silicate, is present in fairly large quantities. The average value of the

Jan 1, 1906

JESSE L. JONES,* Pittsburgh, Pa.-I would like to ask Miss Erskine if down-draft has been used in any of the foundries where heavy fumes have to be removed, instead of the overhead draft.? L. -ERSKINE.-The system of overhead draft to remove heavy fumes has been very much more successful. The entire efforts of the New Jersey Department of Labor in regard to stabilizing conditions in the foundry are the result of the physical examination of the foundryman himself on first-hand information as to the prevalence of the minor ailments and the bad timekeeping that naturally accompanies them. These ailments are a factor in not only increasing the labor turnover but in increasing the percentage of bad work as well. The physical exertion of the foundryman himself is of course an important factor. In certain standard shops the amount of energy expended runs from 11 to 13 tons of foot-pounds of energy a day. In certain shops on piece work, I found a record of the energy expended per day to run as high as 22 tons. In one shop, during the war period, the management established a bonus system, and the men increased their output from 60 to 100 molds a day. The result was an increase of some 60 per cent. in output, and an increase of 400 per cent. in defective castings. The question of the physical exertion in the unsanitary foundries, of course, is very much complicated by other factors, for which reason the department has devoted a good deal of attention to estimating what is a reasonable exertion in a sanitary, well ventilated foundry. We have met certain physical difficulties in the brass foundries that the iron foundries did not have. All that information is available through our Bureau of Industrial Information. The question of the physical energy exerted by the molder is found to have a very distinct bearing on the question of contracts, for the possibility of increasing production is balanced by the extra overhead involved. JESSE L. JONES.-I would like to ask if any evidence has been noticed of carbon-monoxid poisoning among the employees of the foundries.

Jan 4, 1919

By E. Stansfield

IT. has long been known that coal is unstable and oxidizes in air, even at ordinary atmospheric temperatures; also, that such oxidation affects the analysis of coal. Nevertheless little or no precaution is taken to prevent oxidation in the ordinary methods of analysis, and the possibility of error due to oxidation is sometimes ignored even in researches on coal. Although the general nature of coal oxidation is well known, and many workers have made careful studies of the rate of oxidation of different types of coal exposed to oxygen at different temperatures, yet the amount of oxidation coals undergo in the ordinary process of analysis, and its influence on the determined analysis, is not well known, and the published data are widely scattered through the literature. This paper is a collec-tion, from this laboratory, of data that bear on the subject, together with a brief summary of three methods employed here to evaluate the oxidizabil-ity of coal. The post-Carboniferous coals of Alberta range all the way from anthracite down to lignite. As some of them are notably susceptible to oxidation, the necessity for care was early forced upon our attention, and oxidation has been reduced either by the removal of air with a vacuum pump or by the displacement of air with natural gas (methane). The two routine analytical operations most liable to involve oxidation are the preliminary, partial drying of the crushed coal (called air-drying) and the determination of moisture. The first is a prolonged operation on coarse coal at ordinary temperatures, and the second a short treatment on powdered coal at higher temperatures. Oxidation also occurs in coal samples stored in ordinary sample bottles. In order to gain information for this study, determinations were recently carried out on the same samples in air, in natural gas, and in vacuo. Sixteen coals were tested; three would be classed in the United States as coking bituminous coals, two as noncoking, nonslacking, bituminous coals, and the rest as subbituminous. Table 1 gives typical analyses of these coals as mined.

Jan 1, 1934

By R. S. Archer

In the microscopic examination of aircraft-engine parts made of heat-treated alloy steels, the writer has been forcibly impressed by the failure of the usual etching processes to disclose any but gross defects in heat treatment. It seemed particularly desirable to bring out the grain size of the steel, which is indicated in the ordinary etching processes chiefly by the change in orientation of structure from grain to grain. After various attempts, a fairly successful method has been found, which is here presented in the hope that it may be of use to those who have occasion to examine these steels in the hcat-treated condition. The specimens worked with have been mostly chrome-nickel steels heat treated (that is, hardened and tempered) to a Brinell hardness of around 300. A few experiments with other specimens will be referred to later. Briefly, the method employed consists in etching the steel about 10 min. in a fresh solution of picric acid in ethyl alcohol, and then rubbing off the smudge of carbonaceous matter on moist broadcloth. Different samples of almost identical analysis, heat treatment, and physical properties (including resistance to impact) respond quite differently to this treatment. In some, the grain boundaries are developed quite readily, while in others, especially in those whose grain is unusually fine or in which the final hardening heat has not quite obliterated the previous crystallization, the results are more obscure. The exact time of etching to secure the best results also differs for various samples, and the greatest success is usually attained by a process of "tinkering." Such a process is illustrated in a series of micrographs, the first six of which were taken at a magnification of 300 diameters. The properties of the steel are as follows: Carbon, per cent............... 0.42 Brinell hardness.............. 293 Nickel, per cent................ 1.35 Yield point, pounds per square Chromium, per cent............. 0.90 inch........................ 131,000 Copper, per cent................ 0.025 Maximum strength, pounds per Manganese, per cent............ 0.74 square inch................. 144,500 Phosphorus, per cent............ 0.024 Elongation in 1 in., per cent... 28 Sulfur, per cent................ 0.036 Lod impact, foot-pounds...... 51 Reduction of area, per cent...... 57.3

Jan 1, 1920

By W. A. Lang, K. C. Gilbart, E. Stansfield

It has long been known that coal is unstable and oxidizes in air, even at ordinary atmospheric temperatures; also, that such oxidation affects the analysis of coal. Nevertheless little or no precaution is taken to prevent oxidation in the ordinary methods of analysis, and the possibility of error due to oxidation is sometimes ignored even in researches on coal. Although the general nature of coal oxidation is well known, and many workers have made careful studies of the rate of oxidation of different types of coal exposed to oxygen at different temperatures, yet the amount of oxidation coals undergo in the ordinary process of analysis, and its influence on the determined analysis, is not well known, and the published data are widely scattered through the literature. This paper is a collection, from this laboratory, of data that bear on the subject, together with a brief summary of three methods employed here to evaluate the oxidizabil-ity of coal. The post-Carboniferous coals of Alberta range all the way from anthracite down to lignite. As some of them are notably susceptible to oxidation, the necessity for care was early forced upon our attention, and oxidation has been reduced either by the removal of air with a vacuum pump or by the displacement of air with natural gas (methane). The two routine analytical operations most liable to involve oxidation are the preliminary, partial drying of the crushed coal (called air-drying) and the determination of moisture. The first is a prolonged operation on coarse coal at ordinary temperatures, and the second a short treatment on powdered coal at higher temperatures. Oxidation also occurs in coal samples stored in ordinary sample bottles. In order to gain information for this study, determinations were recently carried out on the same samples in air, in natural gas, and in vacuo. Sixteen coals were tested; three would be classed in the United States as coking bituminous coals, two as noncoking, nonslacking, bituminous coals, and the rest as subbituminous. Table 1 gives typical analyses of these coals as mined.

Jan 1, 1934

By W. P. Heineken, A. T. Child

This paper presents the results of a series of experiments made in the metallurgical laboratory of Columbia University, New Pork City. The object of the investigation was to determine, as far as possible, the changes in micro-structure and physical properties caused by short periods of heat-treatment and the longer malleable cast-iron process. It was proposed to do this by means of micro-photographs, heating- and cooling-curves, and tensile tests after the various heat-treatments. I. Micro-Constituents of Iron and Steel. The list of the micro-constituents of iron and steel has grown till now it includes seven different substances, called ferrite, cementite, pearlite,* martensite, austenite, sorbite and troosite. Only the first five of these are mentioned in this paper, to facilitate the understanding of which, the following brief definitions are given: 1. Ferrite (named by Prof. Howe) is, chemically, iron free from carbon. It is the softest of the constituents, and is not colored by etching, except when long-continued. Under the microscope it is easily determined by its regular polygonal etructure; or, if structureless, as in malleable cast-iron, by the ease with which it is scratched. Ferrite appears in mild steel in small amount, in grey cast-iron, and in malleable cast-iron. 2. Cementite (also named by Prof. Howe) is now generally conceded to have the formula Fe3C. It is the hardest of the micro-constituents, having the hardness indicated by 7 of the mineralogical scale; and hence it is always left in relief after

Jan 1, 1901

By B. S. Norris, Charles R. Austin

IN a recent paper the authors1 discussed the reactions to tempering of hypereutectoid steels quenched from 1000° C., as revealed by studies on changes in hardness, electrical resistivity, coercive force and metallographic characteristics. The data, which related specifically to tempering temperatures of 550°, 650° and 710° C., for varying periods up to 125 hr., permitted the following important conclusions: 1. The rate of softening of the steels at the temperatures examined differed markedly although the steels were of "similar" general chemical composition. 2. The temperature of maximum softening spread over a range from about 650° C. to the eutectoid inversion. 3. The divergence in behavior was ascribed, at least in part, to a profound difference in tendency to graphitization on annealing at subeutectoid temperatures. 4. The node of spheroidization of the cementite, as revealed by metallographic studies, also varied considerably in the different steels. The purpose of the present investigation is to pursue further the study of the difference in behavior of the steels on tempering over a wider range of temperature. To this end the following features have received particular attention: 1. Comparison of temperatures of maximum softening of the various steels when the quenched samples were tempered for 5 hr. and for 75 hr. followed by furnace cooling and by quenching in water. 2. Determination of the effect of quenching temperature, prior to tempering, on the rate of softening. Quenching temperatures of 1000° and 850° C. were used in the investigations. 3. Examination of the microstructures obtained with the various heat-treatments employed.

Jan 1, 1938

By N. E. Brown, F. L. Versnyder

THE apparent dependency of the electrical characteristics of hexagonal crystalline selenium on microstructure has aroused much interest in microscopical studies of selenium. Microscopic observations on the crystallization of selenium have been made by Escoffery and Halperin,' P. H. Keck,' and other investigators. It is the purpose of this paper to discuss the microstructural changes observed on polished cross-sections of single layers of selenium after various heat treatments. Observations were also made on crystallization of the free-surface layer of these deposits. In general, all of the transformations studied were either transformations of the vitreous selenium to hexagonal selenium or micro-structural transformation of the hexagonal selenium itself. Procedure The selenium used in this work was obtained from the American Smelting and Refining Co. and was approximately 99.96 pct pure. An intentional impurity of 1 part per 2,000 of bromine was added to the material prior to evaporation. A thickness of approximately 0.002 in. of this selenium was vapor deposited on an aluminum base plate. The maximum plate temperature during the vacuum vapor deposition was 140°C. Mounting of the cross-sectional specimens for metallographic study could not be done in plastic mounting media, as is customary, since temperatures in excess of 50°C would cause unwanted transformations. Consequently, a simple clamp-type device was used to mount the specimens for preparation. All grinding operations were then done carefully by hand in order that the specimen not become heated during this operation. Wet polishing was done on the conventional metallographic polishing laps, using successively finer grinding powders. An extremely careful polish is necessary, since observation and micrography of the specimens are done in the unetched condition under polarized light. The two observations of crystallization made on the free surface of vitreous selenium deposits (Figs. 4 and 5) were made on surfaces which were perpendicular to the cross-sections studied. These free-surface layers were examined directly, i.e., no pre- vious metallographic preparation, as obtained from the vacuum vapor deposition. Microscopic Observations A study was made of polished cross-sections of the vitreous selenium as-deposited. It was noted that in all cases there was columnar crystallization adjacent to the base plate, which appeared to occur during the vacuum deposition process. This observation has also been made by Keck? It also was observed that vagrant spherulitic crystallization occurred in the vitreous selenium. The term "vagrant" is used, since these spherulitic grains appear to crystallize at random throughout the vitreous selenium during the vacuum deposition process. Columnar crystallization at the A1-Se interface and a typical spherulite observed in a polished cross-section of "as-deposited" vitreous selenium may be seen in Fig. 1. Cross-sectional samples of vitreous selenium studied after heat treating individual samples for 20 min in 10" steps from 80" to 220°C revealed that crystallization—in this case, columnar crystal growth —proceeds from the aluminum base plate to the surface of the specimen (Fig. 2). Crystallization was microscopically observed to be complete after the 130°C heat treatment. Visual examination of the free surface of the specimen after the 130 °C heat treatment revealed the readily recognizable grey appearance of the completely crystallized selenium, in corroboration of the microstructural observations. No microstructural transformations then appeared to take place between 130" and 190°C. At 190°C the beginning of recrystallization appeared and proceeded until the columnar grain structure had been completely transformed to equiaxed grains between 210" and 220°C (Fig. 3). Naturally, the grain size of the recrystallized grains at the lower temperatures (190" to 210°C) was smaller than is illustrated in Fig. 3. In addition, polished cross-sections of deposits heat treated at 140°C for 10 min to cause complete crystallization and, subsequently, heat treated in 10" steps from 80" to 220°C for 20 min were studied. As expected, no microstructural transformations took place until the beginning of recrystallization was observed at 190°C. A comparison with the previously studied specimens revealed that recrystallization proceeded almost identically in the two experiments although in the first case the deposits were vitreous prior to the series of heat treatments and in the second case they had been crystallized by a previous heat treatment. By heat treating for longer times (180 min) at lower temperatures, the

Jan 1, 1956

By AIME AIME

ON the afternoon of Feb. 20 of this year a new volcano was born in the center of the State of Michoacan, Mexico, about 100 miles inland from the Pacific Coast. Creation of this new mountain - forming crater began on an almost flat cultivated field at the south margin of a small basin about a mile in diameter and having an altitude of approximately 6800 ft. above sea level. This basin is connected to a gently inclined plain that forms the Parangaricutiro valley, the chief town of this municipality, bearing the same name as the valley, being situated three miles from the site of the new crater. The village of Paracutin, from which the new volcano received its name, is about one mile to the northwest of the crater. From the City of Mexico to the volcano is a distance of 330 miles. The paved highway running from Mexico City to Guadalajara, by way of Toluca and Morelia, is left at Carapan; from here another paved branch highway goes to Uruapan. The town of Paracutin is reached by a narrow dirt road 18 miles from Uruapan and connects with a road leading to Parangaricutiro where horses may be hired for a 40-minute trip to a place where visitors can enjoy a magnificent view of the volcano. It is possible to get within half a mile of the point of eruption in this manner.

Jan 1, 1943

By Arnulf Muan, R. W. Taylor

Activities of iron in Fe-Pt alloys have been dctermined by equilibrating mixtures of platinum metal and iron oxide at known oxygen Pressures in a thermobalance at 1300°C. Conzpositions and iron activities of the oxide phase at equilibrium are known from previous work, and compositions of the Fe-Pt alloy phase formed at equilibrium were detcvt?zined from the observed weight changes of the samples. The activity curve obtained shows a strow negative deviation from Raoult's law. THE present investigation was undertaken as part of a research program dealing with phase equilibrium relations existing among the oxides of iron and titanium at 1300°C. At low oxygen pressures of the gas phase in equilibrium with these oxides, the iron activity of the system is high, and considerable alloying of iron with the platinum used as a container material takes place. Thermodynamic data for Fe-Pt alloys at 1300°C are needed in order to evaluate quantitatively the extent of such reactions. Larson and chipmanlhave determined activities of iron in Fe-Pt alloys at 1550°C by equilibrating platinum metal with CaO-iron oxide-SiOzmelts in which the iron activities were known. Compositions of the resulting Fe-Pt alloys were determined by chemical analysis. Mundiath and Gerassimov2 have studied thermodynamic properties of Fe-Pt alloys by electromotive force measurements in the temperature range 550" to 1000°C. The experimental method used in the present investigation is a slight modification of that used by Grube and Ratsch3 in studies of NiCr-alloys. 1) EXPERIMENTAL METHOD 1) General. Mixtures of platinum metal and iron oxide were equilibrated at 1300°C in atmospheres of known oxygzn przssures, and the course of the reactions was followed by measuring the weight changes of the mixtures. The principles involved in the derivation of composition-activity relations from these measurements are illustrated by the composition triangle for the system Fe-FeZO3-Pt shown in Fig. 1. Take as an example a mixture of FeZO3 (hematite) and platinum such that the total composition is represented by point T. If this mixture is heated to 1300c in air (poz = 0.21 atm) and the oxygen pressure is then reduced gradually, the oxygen content of the oxide phase decreases and increasing amounts of iron enter the metal phase. As the oxide phase and the metal phase for all practical purposes are insoluble in each other, their compositions are represented by points moving toward Fe along the joins Fe-Fe,03 and Fe-Pt, respectively. The total composition of the mixture during this process also changes, but only with respect to oxygen content, because the vapor pressures of iron and platinum are negligible at 1300°C. Hence the change in total composition is described by a straight line (constant Fe/Pt ratio) radiating from the 0 apex of the composition triangle Fe-Pt-0, of which the triangle in Fig. 1 is a part. Only one such line ("oxygen reaction line", T-T",) is shown in Fig. 1. The total composition of the alloy-iron oxide mixture at any instant must, in addition, be located on the straight line (conjugation line) connecting the two points representing the compositions of the two coexisting phases. It therefore follows that the total composition of the mixture at any instant is represented by the point of intersection between the conjugation line and the oxygen reaction line. An example of the situation prevailing at a chosen oxygen pressure, po2, is shown in Fig. 1 by points a' (alloy composition), b' (oxide composition) and T' (total composition). Point b' is known from the work of Darken and Gurry,4 and point T' is experimentally determined by the observed weight change of the mixture (distance T-T). Hence, point a', the composition of the alloy, is determined from the above data as the intersection between the join Pt-Fe and the extension of the straight line bl-7'. The activity of iron in the alloy at equilibrium is identical to that of the iron oxide phase, if the same

Jan 1, 1962

By J. Groyecki, M. Markuszewicz, J. Lassota, A. Zawada

The ratio of stable to unstable inclusions was found to ploy an essential role in the process of sccorldar-y recrystatlizalion in Si-Fe. The analysis of the free energy of inclusions in the range of heat-treatment of individual inclusions to be predicted. The effects MnS. ns inslable inclusions. were investigated. TO secure a high induction, the secondary recryslulliztt-lion associated wilh the texture is necessary. To obtain a low core loss an additional refiuing in the solid state is required. It has been found that sulfur can be more easily removed in racunm than in hydrogen and thai this process was hindered by the prescrzce of INCLUSIONS play an essential role in the development of cube-on-edge texture in Si-Fe. Their function consists in restraining the growth of primary grains up to about 900°C and in passing subsequently into solution at higher temperatures. This process is accompanied by the selective growth of secondary grains with (110)[001] orientation. The general effect of inclusions depends on such factors as the type of impurities, their amount. dispersion and stability, the conditions of diffusion in the space of lattice of metal, and the reactions at the metal/gas interface. In recent years, some of these factors were the subject of a special investigation. A positive influence of Mns, siN,' and vN3 has been established. The quantity of impurities4 and their dispersion5 have been found to be of major importance. Attention was called to the vital importance of diffusion and the conditions under which the impurities are removed from metal., It has also been demonstrated that in Fe-Si alloys by the techniques of powder metallurgy a special opportunity exists to obtain the (110)[001] type texture. 6 The aim of this work was to conduct qualitative investigations on the influence of inclusion stability on the development of cube-on-edge texture in a metal containing approximately 3 pct Si. Experiments were carried out on cast alloys and on those manufactured by powder-metallurgy techniques. The results obtained from these experiments were utilized to explain the phenomena involved and to analyze the relationships between stable and unstable inclusions and the magnetic properties of alloys. EXPERIMENTS AND RESULTS The raw materials used in these experiments were the powder of carbonyl iron with the analysis (in pct) 0.044 C, 0.01 Mn, 0.005 Si, 0.009 P, 0.002 S, traces of Cu, 0.06 Ni, 0.0015 Al, 0.03 Cr, 0.02 Mo, 0.01 Ti, 0.002 Co, traces of Pb, and the powder of silicon containing 94.14 Si, 0.003 S, 0.048 C. The powders were ground and mechanically mixed in 100-g batches. and then pressed at 9 tons per sq cm into 74 by 24 by 8 mm blocks. Sintering was carried out at 1100°C for 12 hr in vacuum (2 x lo-' Tr) or in hydrogen. In this instance the material was heated slowly and subjected to prolonged soaking at 350°, 650°, and 750 2C, respectively, to secure reduction of ferro-oxides. This was checked by making measurements of the dew point, which was found to change from -15" to -35°C after reduction. The compacts after sintering were hot-rolled to 2.4 mm, annealed at 800 C, and finally cold-reduced to 0.35 mm with intermediate annealing at 800°C at a gage of about 0.8 mm. Impurities were added in the powdered form and mixed with iron and silicon powders. Sulfur in the elemental state, electrolytic manganese, and pure aluminum oxide were employed. Besides, to obtain a material with low contents of impurities, especially

Jan 1, 1967

By P. R. Gage, R. W. Bartlett

At high temperatues and reduced oxygen pressuves, molybdenum silicicles oxidize to form SiO(g) vathev than a passivating SiO2 film. This is a sevious problem for low-pressure applications of sili-cide-coated rejvactory tnetals. As oxiclalion pvoceeds, the higher oxidntion potential of silicon initially suppresses oxidation of molybdenum and silicon is depleted near the surface. Eventually, silicon depletion causes secondary passivation (SiO2) mid an active to passiue transition in oxidntion behavior at moderately low pressures. At very low pressures, silicon depletion continues until steady-state oxidation of both silicon and rnolyhdenum can proceed at rates propovtional to their initial stoicliiorrzetvies. Ohsel-vations of 'oxidatiou-rate belzcriliov at temperatures from 1101° to 1700°C and oxygen pressures from 10-7 to 1 at in were made using thermogravimetn'c, X-ray diffraction, and elect?*on-rtric?ro/,vobe techniqrres. The experimental results are in good agreement with calculated lirnits for the various types of behavior that were based on tlievtnochernicnl atzd dffusion rate data for the Mo-Si system. A protective oxide film normally forms during the oxidation of elemental silicon. However, at elevated temperatures and reduced pressures this film is not present and oxidation is rapid. wagnerl has shown that this behavior occurs because SiO(g) is more stable than SiO2. The behavior of the silicides at high temperatures is similar but more complicated. Molybdenum and several silicide compounds are involved and the chemical activity of silicon, or the equivalent silicon vapor pressure, can vary considerably in these phases. Also, diffusion in the silicides resulting from reactions in which a higher silicide is reduced to a lower silicide, or molybdenum containing dissolved silicon, must be considered. EXPERIMENTAL AND ANALYTICAL METHODS Isothermal oxidation experiments were conducted using hot-pressed MoSi2 and Mo5Si3 wafers. Each experiment was conducted at a fixed oxygen pressure by controlling the flow of oxygen in and out of the furnace chamber. Most of the experiments were conducted in a molybdenum-wound tube furnace. Special construction features, including use of a high-purity dense A12O3 refractory tube, permitted operation in high vacuum to 1500°C. Higher temperatures could be obtained at higher working pressures and with a sacrifice of tube lifetime. Temperature was measured with three Pt 6 pct Rh/Pt 30 pct Rh thermocouples and controlled with a proportional controller. Weight changes were monitored with a quartz spring balance. The few experiments, at higher temperatures and low pressures, were conducted in a cold wall vacuum chamber using induction heating with direct susceptance of the sample. Because of the variable levitation effect of the induction coil on the sample, weight changes could not be monitored continuously in these experiments. All samples representing both experimental methods were weighed before and after oxidiation and examined with a microscope and analyzed by X-ray diffraction. The analytical treatment assumes equilibrium at interfaces and uses existing thermodynamic data. For convenience, equilibria are expressed as chemical potentials or as vapor pressures of the gases involved. The resulting differences in equilibrium vapor pressure between adjacent interfaces and between the surface and external atmosphere drive diffusion processes in the solid and gas boundary film, respectively. These diffusion processes govern the rate of oxidation. A bibliography of the sources of thermochemical data for the reactions pertinent to the Mo-Si-O system is given in Table I. Reactions are listed with the sources of free-energy data referenced. Since all of these reactions involve one or more gas species, usually oxygen, a plot of the product-gas chemical potential, -RT In Pg, vs absolute temperature for each reaction is given in Fig. 1. These curves can be used to determine equilibrium vapor pressures or to compare the stability of different compounds in the various gases: O2, Si, SiO, and Moo3,. The data of Table I and Fig. 1 were used to determine the analytical results presented in this paper. EXPERIMENTAL RESULTS The weight changes for three MoSi, samples oxidized at 1500°C are plotted against time in Fig. 2. The treatments were identical except for the indicated variance of oxygen pressure and each curve represents one of three characteristic types of behavior that were observed. The upper curve is an example of passive oxidation, which is defined as

Jan 1, 1965

By A. S. Richardson

The design of mine airways receives, in general, very little engineering treatment. To a large extent this is, of course, due to the fact that information upon which to base calculations is seldom available in definite form. In many rnines the extent of the workable deposits may not be known at the time an air course is planned, and the length of service is indeterminable. Volume of air required for ventilation rnay also increase with extension of the life of a property, and natural obstacles, such as heavy ground, often place limitations upon the size of opening that can be maintained. Perhaps most of the shafts used in the ventilation of metal mines were originally intended as hoisting shafts, and many of the tunnels and crosscuts similarly used, were also designed as haulage ways or for other operating purposes. Even when a shaft is sunk solely for ventilation, custom usually dictates a size and shape consistent with the type commonly used for ordinary operations, because experience has demonstrated it can be excavated and maintained. In fact, most ventilation openings were never made with any consideration as to economic design for such use. When an air course is required to pass air between different parts of mine workings under a fixed pressure, the size of opening required for a given volume of flow, is, of course, determined by the resistance factor of the air course. It is then impossible to proportion the opening with reference to economics of power consumption, and this paper is limited to the design of openings where ventilation pressure or power consumption may he varied for economic advantage. As the size of an air course is increased, the expense involved in excavation and support is, of course, also increased, but the charge for power is decreased. In the case of a mine that has only a short assured operating life, it would not be ecouomical to provide large openings in order to reduce power bills; but when operations are likely to continue for a long time, the power charge becomes a very important economic factor. Although lack of definite information on such factors as service life and costs of excavation and support affects the design of an air course, it appears, from a mathematical analysis of the problem, that considerable variations may be made in estimating these factors, without greatly

Jan 1, 1927