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By AIME AIME

THE time of the Section delegates was economized this year by providing the section reports in mimeo- graphed form, together with the reports of the officers and committees of the Institute, for their consideration on arrival. The meeting was called for Thursday forenoon and despite a certain amount of oratory managed to get through before all the luncheon was gone. In all, nine section delegates and one from the Iron and Steel Division attended and took part. One delegate, who had come many miles, got lost in the complication of the program and failed to attend. Six appointed dele- gates failed to attend and two sections neglected to make appointments.

Jan 1, 1929

By W. F. Sullivan, J. R. Coleman

The use of radioisotopes in obtaining basic information on large scale industrial processing is illustrated with two examples. The first is concerned with the operating characteristics of a kiln scrubbing tower and the second with those of a Hardinge ore mill. The examples show the advantages associated with the industrial use of tracers as well as the limitations. The Atomic Energy Commission regulations governing the use of radioisotopes in this manner are also discussed. The nuclear properties of radioactive isotopes have provided a new technique for obtaining basic information on large scale industrial processing. A small portion of the process stream is made radioactive by mixing with a suitable radioisotope or by irradiation in a nuclear reactor. The "tagged" portion is then part of the normal process stream and can be followed by detection and measurement of the associated radioactivity. The advantages of radioactive tracing over other forms of tracers are well known, and include such factors as chemical similarity, capability of precise determination of very small quantities due to the high sensitivity of detection apparatus, and the absence of foreign element contamination of the final product. This report will illustrate two applications of the use of radioactive tracers in large scale industrial processing which have provided information that would have been hard to obtain by other means. The first is concerned with the operating characteristics of a kiln scrubbing tower and the second with those of a Hardinge ore mill. ATOMIC ENERGY COMMISSION REGULATIONS Atomic Energy Commission approval can be obtained by qualified personnel if the proposed quantity of radioactivity does not exceed AEC's standards for

Jan 1, 1965

By John T. Galey

Oil and gas development in southern Pennsylvania during 1937 was marked by considerably increased activity in deep-sand drilling. Nine tests were completed to the Oriskany sand: one in Independence and three in South Beaver townships, Beaver County; one in Franklin township, Butler County, two in Slippery Rock township, Lawrence County; one in Mt. Pleasant township, Washington County, which is drilling below the Oriskany, and one in Fairfield township, Westmoreland County. Two of these wells, both of which were in the Blackhawk pool, South Beaver township, Beaver County, obtained wet gas with open-flow volumes of 1.5 million cu. ft. and 3.1 million cu. ft. and closed-in pressures of 1900 Ib. The remaining seven were unproductive in the Oriskany. Two wells, one in Hampton township, Allegheny County, which is shut down temporarily as a result of a gas pocket, and one in South Beaver township, Beaver County, are drilling to the Oriskany. One deep test on the Chestnut Ridge anticline, South Union township, Fayette County, was completed after considerable difficulty as a dry gas well in the Onondaga limestone. At this locality the cherty limestone is porous as a result of fracturing. Three additional tests are under way in the area, one in South Union township, a second in North Union township, and a third in Wharton township. Completions Oil.—Despite price cuts and production curtailment of Pennsylvania Grade crude, caused largely by a decreasing demand from export markets, operation in the shallow oil areas continued at a fairly high rate and a number of good wells were completed. Some of these were new wells in close proximity to old production and others were old wells drilled into deeper pays. One new well of a number of producers drilled to the Nineveh Thirty-foot sand in the Harvey pool, Center township, Green County, made 400 bbl. of oil and 500 million cu ft. of gas the first 24 hr. The Chambers dam pool of Amwell and South Franklin townships, Washington County, yielded a number of Fifth Sand producers with initials as high as 200 bbl. Several wells in the old Mars-Butler field

Jan 1, 1938

By Basil B. Zavoico

The developments in the Russian oil industry during 1935 marked a very definite turning point from the time when the industry was being educated to the modern methods of oil-field finding and development, refining, transportation and marketing, to the time when the industry has thoroughly assimilated the modern technique and is now firmly standing on its own feet, as is shown by the remarkable qualitative, if not quantitative, progress in 1935. The oil industry promises that 1936 will be a record year in every respect with both quantity and quality approaching the desired high levels and standards. More particularly the Soviet Government is beginning to be successful in the development of new fields and such new production in geographically strategical points of the country will be in the coming years a factor of great importance in the industrial life of the country. The most notable achievements of the last year have been: the very successful development of the Ishimbaevo oil field in the Lower Oural-Permian Basin; the discovery and development of several promising oil fields in the Puta district of Azerbaijan, while large flush production of Baku area was extended 50 miles due southwest into the Saliani-Aliat district, where a 3000-bbl. well was completed early in 1936 at Pirsagat. Also, an apparently important discovery was made at Zikh, on the Apsheron Peninsula proper. These discoveries, as well as several important strikes in the deeper producing sands in the older fields of the Apsheron Peninsula, have greatly augmented the proven reserves of Russia and made them available either at the points where transportation facilities were already present or at points not too far distant from major industrial centers of the country. Of course, not all objectives were achieved during the past year, and several major difficulties remain to be solved in the coming years, the more important of which are: (1) supply of equipment and of parts; (2) the unavailability of competent technical men in sufficient numbers, which more particularly affects the distant fields; and (3) the problem of distribution of oil products throughout the country, especially the question of handling the needs of small consuming areas, which, while individually unimportant, in the aggregate require huge distribution.

Jan 1, 1936

By Basil B. Zavoico

The developments in the Russian oil industry during 1935 marked a very definite turning point from the time when the industry was being educated to the modern methods of oil-field finding and development, refining, transportation and marketing, to the time when the industry has thoroughly assimilated the modern technique and is now firmly standing on its own feet, as is shown by the remarkable qualitative, if not quantitative, progress in 1935. The oil industry promises that 1936 will be a record year in every respect with both quantity and quality approaching the desired high levels and standards. More particularly the Soviet Government is beginning to be successful in the development of new fields and such new production in geographically strategical points of the country will be in the coming years a factor of great importance in the industrial life of the country. The most notable achievements of the last year have been: the very successful development of the Ishimbaevo oil field in the Lower Oural-Permian Basin; the discovery and development of several promising oil fields in the Puta district of Azerbaijan, while large flush production of Baku area was extended 50 miles due southwest into the Saliani-Aliat district, where a 3000-bbl. well was completed early in 1936 at Pirsagat. Also, an apparently important discovery was made at Zikh, on the Apsheron Peninsula proper. These discoveries, as well as several important strikes in the deeper producing sands in the older fields of the Apsheron Peninsula, have greatly augmented the proven reserves of Russia and made them available either at the points where transportation facilities were already present or at points not too far distant from major industrial centers of the country. Of course, not all objectives were achieved during the past year, and several major difficulties remain to be solved in the coming years, the more important of which are: (1) supply of equipment and of parts; (2) the unavailability of competent technical men in sufficient numbers, which more particularly affects the distant fields; and (3) the problem of distribution of oil products throughout the country, especially the question of handling the needs of small consuming areas, which, while individually unimportant, in the aggregate require huge distribution.

Jan 1, 1936

The paragraphs quoted, regarding Mr. Hoover's appointment as chairman of the newly organized food board of the United States, are taken from the editorial page, of the New York Times for April 13: ?The country is fortunate in commanding the services of Herbert C. Hoover as Chairman of the newly established Food Board. This is n, problem of first importance. Few realize the extent to which American food stuffs will enter into the decision of the war, and it is doubtful if it has occurred to many minds as yet that we shall have to deny ourselves what we have regarded as necessaries in order to keep our European allies supplied. " Mr. Hoover is one of the leading mining engineers of the country. At the outbreak of the war he put his private affairs aside to become the head of the American Commission for Relief in Belgium. He has had an experience that perhaps no other man has ever had, covering the raising of money and the purchase and distribution of supplies on a large scale; He has been brought into close relations with the neutrals and the belligerents on both sides. By them all he is recognized is one of the best executives brought to the fore by the mar. Mr. Hoover is in a position now to place abilities and experience at the service of his country. He will come back with comparative data that will enable him to measure resources and deficiencies accurately. This appointment gives renewed assurance of our Government's grasp of the problems of war and its resolve to apply, business principles to their solution."

Jan 5, 1917

By Henry A. Stiff

The classification and correlation of water analysis data presents many problems which can be solved by graphic methocis. The pattern system, a new type of graphic procedure described in this communication, is believed to have several advantages over older methods. Examples of the application, of the pattern system to the solution of problems encountered in petroleum production are given. INTRODUCTION Several graphic methods for presenting analytical water data have been developed and are now in use.1,2,3,4 It is believed, however, that a recently developed type of graph called the "pattern" offers several advantages over other methods. This system presents a better picture of the total salt concentration than is usual in such graphs. The effect of dilution or concentration has been reduced to a minimum, and at the same time distinction between various types of water has been improved. The system is extremely versatile, yet so simple it can be plotted on ordinary graph paper and adapted to almost any type of filing system. DISCUSSION The essential feature of the pattern system is the graph shown in Fig. 1. Horizontal lines extending right and left from a vertical line at zero form the graph. Positive ions are plotted to the left while negative ions are plotted to the right. The figure immediately beneath each ion gives the scale. Most oil field waters can be plotted on a scale where 100 milli-equivalents of sodium and chloride and 10 milliequivalents of each of the other ions are represented by one scale unit. For highly concentrated brines, 1,000 milliequivalents of sodium and chloride and 100 milliequivalents of each of the

Jan 1, 1951

By Henry A. Stiff

The classification and correlation of water analysis data presents many problems which can be solved by graphic methocis. The pattern system, a new type of graphic procedure described in this communication, is believed to have several advantages over older methods. Examples of the application, of the pattern system to the solution of problems encountered in petroleum production are given. INTRODUCTION Several graphic methods for presenting analytical water data have been developed and are now in use.1,2,3,4 It is believed, however, that a recently developed type of graph called the "pattern" offers several advantages over other methods. This system presents a better picture of the total salt concentration than is usual in such graphs. The effect of dilution or concentration has been reduced to a minimum, and at the same time distinction between various types of water has been improved. The system is extremely versatile, yet so simple it can be plotted on ordinary graph paper and adapted to almost any type of filing system. DISCUSSION The essential feature of the pattern system is the graph shown in Fig. 1. Horizontal lines extending right and left from a vertical line at zero form the graph. Positive ions are plotted to the left while negative ions are plotted to the right. The figure immediately beneath each ion gives the scale. Most oil field waters can be plotted on a scale where 100 milli-equivalents of sodium and chloride and 10 milliequivalents of each of the other ions are represented by one scale unit. For highly concentrated brines, 1,000 milliequivalents of sodium and chloride and 100 milliequivalents of each of the

Jan 1, 1951

By W. J. McKenna

THE International Smelting Co. concentrator at Tooele, Utah, first operated on a custom basis for the treatment of lead-zinc-iron ores on Nov.' 1, 1924, with a capacity of 500 tons per day. On May 1, 1925, the capacity was increased to 1000 tons per day by the addition of another 500-ton section. The concentrator has since operated on the two-section basis, each treating 500 tons per day entirely by flotation. LABORATORY AND TEST MILL In connection with the concentrator, a well-equipped laboratory and small continuous testing plant are maintained. The flotation equipment in the test plant is of both the Callow and Mineral Separations Sub-"A" types, so that actual concentrator conditions may be duplicated as closely as possible. PURCHASING OF ORE A new shipper usually sends to the plant a 25 to 50-lb. sample, representative of the ore to be shipped. Batch flotation tests are made on this sample to determine its amenability to the concentrator treatment flowsheet and reagent combinations. The results of these tests, which are accurately correlated with those obtained at the concentrator, both as to grades of products and recoveries, determine the actual value of the ore as submitted in the ore purchasing department's treatment schedule. Hearty cooperation has existed at all times between the ore purchasing and operating departments in the selection of ores as concentrator feed. ORE TREATED The basic tonnages for mixtures on the two sections come from the Park City and Bingham mining districts. The Park City tonnages are received by rail and consist of crude ores and gravity mill products. Those from the Bingham district are received by rail and aerial tramway,

Jan 1, 1928

By F. L. Sizer

The mining regulations of British Columbia and Mexico present some features which might well be copied in the United States, if we are to have a complete revision of the laws governing mining titles. 1. First and foremost is the "squarc" location, which would mean the abolition of extralateral rights. This is a condition in both of the countries above named which has seemed to work no hardship upon any one, and certainly the limitation of underground rights by vertical planes through all lines makes a locator's rights clear. In view of the long and costly litigation which has involved so seriously many of our most important mining districts, it would seem to be the part of wisdom to avoid a repetition of similar trouble on titles of lode mining claims, by the enactment' of a law similar to that in force in British Columbia. Objections have been raised by .representatives of English companies to the investment of large amounts of money in mining operations in the United States, because of the insecurity of title under the 'present apex law; and the statement has been made to me personally by one of the largest English operators, that he would .never again consent to the purchase of mines in the United States, preferring Mexico with all its revolutionary troubles to the danger of encroachment upon his underground rights by an unscrupulous neighbor. Without going into further argument as to the desirability of the I(square location," it should be sufficient to say to those who are inclined to "let well enough alone" and still stick to the "law of the apex" that there have never been any serious objections raised to this feature of the square location in either British Columbia or Mexico. There are well founded and logical reasons for abandoning the doctrine of extra-lateral rights since it is so difficult of interpretation; the most natural substitute being a law similar to that of British Columbia, giving to each locator an area 1,500 ft. square. I would advocate the right to locate adjoining claims of equal extent on either side of the discovery claim, on the strike of the lode, subject to a seasonable requirement in the matter of work upon them; and in the case of a vein dipping flatter than 45' from the horizon, or in case of a

Jan 1, 1915

By J. A. Faucher

The mining industry has undergone significant technological advances in metallurgical process methods in recent years. The 1000 tpd concentrator of St. Lawrence Colum-bium Metals Corp. portrays the continuing effort made by the industry to achieve economical concentration of new and difficult ores. During the active search for sources of uranium in the early fifties, radioactive minerals were found in the Oka district near Montreal. The compatatively small quantities of uranium which were found occurred in association with widespread columbium (niobium) mineralization which included perovskite, a calcium titanate containing roughly 40% Cb2O5; niocalite, a silicate containing some 20% Cb2O5; and pyrochlore, a calcium niobate containing 45 -70% Cb2O5 as well as fluorine and some water. An idealized formula for one type of pyrochlore is: A typical chemical analysis of pyrochlore is shown in Table I. An important feature of this analysis is the lack of tin, lead, sulphur and P2O5 which conforms with the requirements of most consumers. In general the cerium content varies with sodium content and any increase in Ta2O5 lowers the Cb2O5 content of the concentrate. However, Ta2O5 rarely exceeds 0.5%. The carbonatite host rock of the columbium mineralization has the average mineral composition shown in Table 11. In Table 11, the term "diopside" is used to cover all silicates except mica which is shown separately because of the problems involved with its separation during the concentration process. In some ore zones, small quantities of rare earth minerals, such as monazite are present.

Jan 1, 1964

By H. D. Newell

Jan 1, 1938

By H. D. Newell

Jan 1, 1938

By Thomas H. Clagett

ThE Pocahontas coal field comprises the area in Tazewell County, Va. and Mcrcer and McDowell counties, W. Va., in which Nos. 3 and 4, Pocahontas seams of bituminous coal are mined. It is a mountainous region with ridges rising 300 to 1000 ft. (91 to 305 111.) above the very narrow valleys and, except for some poorly kept farms along the tops of the ridges and the area occupied by the mining and coking plants and villages, is wooded throughout. First shipments were made from Pocahontas in 1883. There are now about 100 mines, 95 per cent. of which are drift mines. At the end of 1920, approximately 298,000,000 gross tons of coal had been produced and 35,000 acres of coal mined. No. 3 seam is from 4 to 10 ft. (1.2 to 3 m.) thick, but the change is gradual and the thickness fairly uniform in any particular locality. It has a streak of bone, about 2 in. (5 cm.) thick, to which the coal adheres on both sides. In parts of the field this bone is replaced by hard slate, usually from 2 to 4 in. thick. The seam has a slate or fireclay bottom and a draw-slate top. No. 4 seam is from 65 to 80 ft. (19.8 to 24 m.) above No. 3 seam, and of minable section only in the western part of the field. It is from 3 to 8 ft. thick and has two streaks of bone, cach from 1 to 2 in. thick. It has a fireclay or slate bottom and is overlaid by from 4 to 24 in. of a laminated coal and slate, locally termed "black rash," which is separated from the coal seam by about 3 in. of slate. This "black rash" averages about 2.5 per cent. ash, but contains some clean coal. The coal in both seams is quite soft. Cleavage sufficieiltly well defined to exert an influence on the mining is rare. Overlying strata arc slates, shales, and sandstones, the sandstones predominating, extending from 30 to 1000 ft. above No. 3 seam. The strata directly above the draw slate of No. 3 seam, or "black rash" of No. 4 seam, and up to the first sandstone are usually slates or shales, about 10 ft. thick over the.

Jan 1, 1923

By Thomas H. Clagett

ThE Pocahontas coal field comprises the area in Tazewell County, Va. and Mcrcer and McDowell counties, W. Va., in which Nos. 3 and 4, Pocahontas seams of bituminous coal are mined. It is a mountainous region with ridges rising 300 to 1000 ft. (91 to 305 111.) above the very narrow valleys and, except for some poorly kept farms along the tops of the ridges and the area occupied by the mining and coking plants and villages, is wooded throughout. First shipments were made from Pocahontas in 1883. There are now about 100 mines, 95 per cent. of which are drift mines. At the end of 1920, approximately 298,000,000 gross tons of coal had been produced and 35,000 acres of coal mined. No. 3 seam is from 4 to 10 ft. (1.2 to 3 m.) thick, but the change is gradual and the thickness fairly uniform in any particular locality. It has a streak of bone, about 2 in. (5 cm.) thick, to which the coal adheres on both sides. In parts of the field this bone is replaced by hard slate, usually from 2 to 4 in. thick. The seam has a slate or fireclay bottom and a draw-slate top. No. 4 seam is from 65 to 80 ft. (19.8 to 24 m.) above No. 3 seam, and of minable section only in the western part of the field. It is from 3 to 8 ft. thick and has two streaks of bone, cach from 1 to 2 in. thick. It has a fireclay or slate bottom and is overlaid by from 4 to 24 in. of a laminated coal and slate, locally termed "black rash," which is separated from the coal seam by about 3 in. of slate. This "black rash" averages about 2.5 per cent. ash, but contains some clean coal. The coal in both seams is quite soft. Cleavage sufficieiltly well defined to exert an influence on the mining is rare. Overlying strata arc slates, shales, and sandstones, the sandstones predominating, extending from 30 to 1000 ft. above No. 3 seam. The strata directly above the draw slate of No. 3 seam, or "black rash" of No. 4 seam, and up to the first sandstone are usually slates or shales, about 10 ft. thick over the.

Jan 1, 1923

By W. D. MOTTER

THE following brief description of the status of operations of the Chile Exploration Co. at Chuquicamata, Chile; and of the plant as it exists today, points out the-great progress that has been made since the initiation of prospect drilling in 1912. During the 11 years which have elapsed since then, a group of small mines, eking out a 'precarious existence, has been consolidated into one large operating property,, taking high rank among the world's producers of copper. After a drilling campaign followed by a construction period, the plant first started operations in 1915. Since then production has been gradually increased, as world conditions permitted, until the present status has been reached.

Jan 1, 1924

By R. W. Fountain, John Chipman

The solubility of nitrogen in Fe-B alloys (0.001 to 0.91 pet B) is determined by the Sieverts' technique for temperatures of 950° to 1150°C. The activity coefficient of nitrogen is decreased by boron. The three-phase equilibrium between ? iron, BN, and gas is established and also the four-phase equilibrium between iron, BN, Fe2B, and gas. The above equilibria are calculated for a iron. The relation of these data to hardenability and strain aging of boron-treated steels is discussed. BORON additions are known to enhanbe the hardenability of heat-treatable steels and to assist in the control of strain aging in sheet steel for deep drawing. The increase in hardenability is explained by the theory that adsorption of boron on austenite grain boundaries reduces their free energy and thus retards ferrite and upper bainite nucleation.l,2 Digges and Reinhart3 have shown that the full effectiveness of boron in commercial steels is achieved only when strong nitride formers such as titanium and zirconium are also present. The influence of nitrogen on eliminating the boron contribution to hardenability was also demonstrated by Shyne and Morgan.4 These workers prepared Ni-Mo steels containing either nitrogen or boron or nitrogen plus boron. The nitrogen-plus-boron steels showed the lowest hardenability which was attributed to the presence of stable nucleating particles, presumably nitride. Morgan and Shyne5-7 have shown that boron in the amount of 0.007 pet will completely eliminate strain aging due to nitrogen in low-carbon, open-hearth steels. In addition, by proper control of the boron additions, a rimming steel can be produced. Since the effectiveness of boron on hardenability and eliminating strain aging is influenced by the amount and distribution of the nitrogen in the steel, the present study was. undertaken to determine the influence of boron on the solubility of nitrogen in iron. EXPERIMENTAL PROCEDURE The solubility of nitrogen in Fe-B alloys was measured by the method of Sieverts, which consists of determining the amount of gas dissolved by the metal in a constant volume system. The apparatus employed in this investigation and the experimental details have beendescribed previously.B AMcLeodgage was added to the apparatus to allow measurements at very low pressures. The alloys were melted at reduced pressure in a basic-lined induction furnace using electrolytic iron and ferroboron. Ferroboron was added after the primary deoxidation of the iron with carbon. Since it was difficult to attain a constant low level of oxygen by this procedure, silicon was added after the carbon deoxidation and prior to the ferr obor on addition. The alloys were castas 2-in. sq ingots, heated in argon at 1050loC, and forged to 1/4-in. plate. After forging, 1116 in. was machined from each side of the plate to remove any possible contamination, and it was then cold-rolled to 0.010-in. sheet. The sheet was cut into approximately 1/4-in. squares and pickled in an inhibited H2SO4 solution to ensure a clean surface. In the case of the boron alloys, a hydrogen treatment could not be used for surface cleaning because boron losses resulted. The composition of the alloys is given in Table I. For a solubility determination, a 75-g sample was inserted in a quartz tube and sealed in place in the apparatus. The entire system was evacuated at room temperature and leak tested for 24 hr. If no leaks were observed, the system was heated to the temperature of measurement and again leak tested for 24 hr. If no leaks were detected, the hot volume and solubility determinations were begun. The hot volume was determined at a constant temperature for each run by admitting successive amounts of argon and recording pressure vs volume, which, in all cases, resulted in a straightline relationship. The argon was then removed and the procedure repeated with nitrogen. Successive additions were made until the desired nitrogen content of the metal and equilibrium pressure of the system were obtained. The

Jan 1, 1962

By John F. Walker

WITH an estimated production of over 936,000,000 for the first six months, the gross value of mine production for 1937 in British Columbia should exceed $70,- 000,000. This figure, if attained, will establish an all-time record for the Province. Great changes have taken place in the different divisions of the mining industry since 1929, the previous peak year of mineral production. A brief review of the earlier history of mining in the Province will also be given.

Jan 1, 1937

By James E. Howard

At the request of the Council of the Institute, I have the honor to submit the following remarks upon the Program of Tests under which the current work of the Watertown Arsenal Testing Laboratory is carried on, which comprises, among other items, the tests of steel ingot metal and derivative shapes. The intended scope of the tests may be illustrated by extracts from the descriptive part of the program as submitted by the Laboratory under date of April 17,1907, and subsequently approved by the Chief of Ordnance, U. S. A. Under Item 1, Ingot Metal—Open hearth, acid and basic; Bessemer, acid and basic; crucible; fluid compressed and uncompreesed—descriptive remarks were made as follon-s: "A thorough, fundamental inquiry into the physical properties of steel necessarily begins with the ingot metal. Investigations, having for their object the improvement of steels, should also begin with the ingot. A knowledge of the ingot structure is essential for judging of the subsequent behavior or appearance of the metal. Under ordinary conditions, so little information is obtained from the ingot in individual cases that practically none of importance is acquired. These remarks have particular reference to the state of physical and structural

Jan 1, 1909

By W. C. Leslie, R. M. Fisher, K. G. Carroll

A nitride, believed to be Si3N, has been separated from three nitrided silicon steels. Germanium nitride, Ge3N4, has been prepared from pure germanium. Comparison of the diffraction patterns indicates that the two nitrides are isomorphous; on orthorhombic structure is suggested in place of the rhombohedral structure previously reported for Ge3N4. THE possibility that a nitride of silicon may, under appropriate conditions, precipitate in silicon steels or in steels killed with silicon makes it desirable to have some positive means of identifying such a compound. One such means is the X-ray or electron diffraction pattern of the nitride. A review of the meager data in the literature indicates that the nitride most likely to form is Si3N4, a conclusion supported by the results of a study of nitrided silicon steels to be published shortly by L. S. Darken and R. P. Smith, of this Laboratory. Unfortunately, there is available no diffraction pattern for this nitride. Data have been reported, however, for Ge3N4 which, judging from the similarity between germanium and silicon, might be expected to be isomorphous with Si3N4. An effort was made, therefore, to form such a silicon nitride, to determine its composition and diffraction pattern and, if possible, its structure. To this end a series of three silicon steels was nitrided under controlled conditions with the resultant formation of nitride particles which yielded an electron diffraction pattern in situ. The particles were then extracted from the steel and an attempt was made to determine their chemical composition. X-ray and electron diffraction patterns were also obtained from the extracted particles, which indicate that the nitride is isomorphous with Ge3N4, although a complete determination of the structure has not been possible. These results show that a silicon nitride with a well-defined diffraction pattern can form in silicon steels, and they suggest that this nitride is Si3N4. Materials and Procedures The sillicon steels investigated were In the form of thin sheet or strip and had the composition shown in Table I. The 0.58 and 1.21 pct Si steels were nitrided by holding them at 1110°F in an H2-NH3 atmosphere containing 3 pct ammonia for 48 hr. The nitride particle size was increased by subsequent heating at 1500°F for 13 1/2 hr in helium. The resulting microstructure is shown in Fig. 1. The steel containing 3.20 pct Si was nitrided at 1200°F for 16 1/2 hr after which it was held in helium at 1500°F for 4 hr. Its structure as seen under the electron microscope is illustrated by Fig. 2. As would be expected from the higher silicon content and the shorter holding time at 1500 °F, the nitride particles are smaller and more numerous than those in the 1.21 pct Si steel. The ammonia-hydrogen treatment reduced the carbon content of the steels to a very low level, so no interference was encountered from carbon or carbides. In the case of the 3.2 pct Si steel, the carbon was reduced to 0.003 pct before nitriding by heating in dry hydrogen. Attempts to obtain an X-ray diffraction pattern from polished and etched surfaces of the 1.21 and the 3.20 pct Si steels were unsuccessful. However, an electron diffraction pattern was obtained from the surface of the steels. The interplanar spacings obtained from these patterns arc shown in Table 11, col. 5. The nitride particles were then extracted from all three steels by dissolving the ferrite matrix in bromine-methyl acetate, the solution used in the Beeghly method for the extraction of aluminum nitride from steel. X-ray diffraction patterns of these residues, obtained by means of a spectrometer and by a 57 mm Debye-Scherrer powder camera using filtered cobalt or chromium radiation, are given in Table II along with the pattern obtained by

Jan 1, 1953