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By NORMA D. MACFADDEN

WHILE the library work of the Woman's Auxiliary to the A. I. M. E. was founded three years after the formation of the Auxiliary, its present policy of establishing permanent libraries in mining camps throughout the United States dates only from 1924. Since then sixteen libraries have been established and thousands of books have found their way to homes of far-away miners, bringing pleasure and knowledge to a multitude of Americans and future citizens. Library work was initiated under the presidency of Mrs. H. W. Hardinge in 1922 and firmly established with her aid as one of the main activities of the Auxiliary. The first chairman served but a short time and Mrs. A. O. Ihlseng then took over the work of chairman of the Library Committee. To place the surplus books of Auxiliary members and their friends in use in mining camps was the immediate work of the committee. This was accomplished by placing a traveling library in the Bureau of Mines' cars and also by sending books for distribution to section chair- men in our larger mining camps.

Jan 1, 1929

By P. K. Weimer

Coinpletely integrated thin-film circuits inco?,porating more than 1000 active and passive elements have been fabricated reproducibly in the laboratory by evaporation of- all components. A 180-stage modified shift register comprising 540 CdSe TFT's, 360 resistovs, and 180 capacitors was deposited upon a glass substrate during one pump-down of the vacuum systeitl. Experimental units have been operated for more than 5000 hr at temperatures uP to 85°C without failure of any slages. The present pupper reviews the charvactevistics of evaporated thin-film transistors (TFT's) and discusses their application to integrnted circuils. INTEGRATED circuits most widely used today are based upon silicon technology, with the circuits formed on the surface of a block of single-crystal silicon1 or on a block of sapphire 2,3 upon which a thin layer of silicon has been deposited. Transistor patterns and interconnections are defined by photographic procedures using photoresist masking. Large groups of transistors are produced in batches which undergo many processing steps, some of which are carried out at elevated temperatures. Passive elements are formed by treatment of the semiconductor surface or are deposited by evaporation alongside the active elements. The size and complexity of the circuits are limited by defects in the devices and by the size of the available single-crystal chips. Capacitative coupling to the semiconducting substrate may also limit useful size and frequency response of the circuits. An alternative approach to integrated circuits is based upon the deposition by evaporation of all circuit components upon a noncrystalline, insulating substrate such as glass.4 Thin-film field-effect transistors,1'6 known as TFT's, can be deposited in large arrays on glass or plastic substrates at the same time the associated passive elements are being deposited. Although still in the research stage the all-evaporated approach is expected to offer certain advantages for many applications. In particular, the use of thin films upon a noncrystalline substrate offers the prospect of producing complex, large-area circuits not now feasible with single-crystal silicon. Important applications of this type include memory arrays for computers and imaging devices for television. The ease with which the evaporated TFT's can be deposited may permit continuous, automated production methods not possible with high-temperature batch processing. Recent advances7'8 in the fabrication of thin-film transistors have led to greatly improved reproduci-bility and life of the TFT's. Experimental circuits having over 1000 active and passive elements deposited upon a common glass substrate are currently being produced in the laboratory. The present paper reviews recent progress in the development of the TFT and in its application to integrated circuits. I) DESCRIPTION OF THE THIN-FILM FIELD-EFFECT TRANSISTOR The TFT is a field-effect transistor of the type having the control gate separated from the semiconductor by a thin insulating spacer. Although its operation resembles that of the silicon MOS transistorg its construction is based entirely on thin-film techniques. Fig. 1 shows a cross-sectional view of an evaporated TFT deposited upon a glass substrate compared with a silicon MOS transistor deposited upon single-crystal sapphire.3 The semiconductor in the TFT is a poly crystal line layer, of a material which can be readily evaporated, such as cadmium sulfide, cadmium selenide,l0 or tellurium." Silicon monoxide layers have usually served as the gate insulator, but other oxides, sulfides, and fluorides may be used. Film thicknesses range from a few hundred to a few thousand angstroms. The source, drain, and gate electrodes in the TFT are of metal. Qpical source-drain gap dimensions are 0.0003 x 0.030 in., with a gate strip whose width slightly overlaps the source and drain. The source and drain electrodes should make low impedance contacts to the semiconductor. With cadmium sulfide films, gold is a satisfactory material for underlying electrodes, while aluminum is preferable for overlying electrodes.12 Considerable variation in design of the TFT is permissible, with the electrodes being

Jan 1, 1967

By B. N. Whittaker, C. J. Bonsall

The paper gives an account of the factors influencing the stability of coal mining tunnels and goes on to examine various bases of support and lining design of such tunnels in relation to geological and mining conditions. The different types of coal mining tunnels are compared and comments made regarding the factors influencing their choice and basic design features. Foremost amongst design considerations is the design method and special thought has been given to the validity of different formulae as related particularly to UK Carboniferous geological conditions. Emphasis is placed on the role of the stress field in relation to tunnel stability. Shape of mining tunnel has been investigated and conclusions drawn regarding the merits of different commonly excavated geometries from a stability point of view. Detailed design aspects pertaining to determination of tunnel lining strength and resulting stability are critically examined and current design methods are compared. Data from UK mining tunnels are included as the basis for comparison of these design methods.

Jan 1, 1983

By Strathmore R. B. Cooke, Thomas E. Ban

MUCH experimental work has been performed on the mechanism of agglomeration and pelletizing of moist ore and concentrates and on the process of firing agglomerates, but except for the work of Tigerschiöld and Ilmoni1 much of the published information is empirical, and the literature contains no information concerning the structure of fired pellets. Results of a preliminary study of the microstructures occurring in pellets produced both in the laboratory and on a pilot-plant scale are presented in this paper. Most of the results were obtained from pellets prepared from Mesabi magnetic taconite, but through the courtesy of the staffs of the Minnesota Mines Experiment Station and the Bethlehem Steel Co., fired pellets produced from limonite and hematite ores and from Lebanon magnetite have also been examined. The work has been restricted almost entirely to pellets produced without additives, the exceptions being those in which coal was. added to the filter cake before rolling. Schwartz has described the microstructures occurring in ore sinters produced under reducing conditions.2 Many of the structures and constituents he describes are common to fired pellets, but the constituents normally occur in markedly different proportions. His statement that "in all satisfactory sinter the amount of hematite is small, perhaps not over 2 or 3 per cent" is inapplicable to pellets produced by pilot plant operation or by any process in which air is not deliberately excluded. Pilot plant pellets contain over 90 pct by weight of hematite, and those produced in the smaller furnaces of the Minnesota Mines Experiment Station contain more than 80 pct of that constituent. Preparation of Specimens It is difficult to examine unfired pellets microscopically because of their insufficient coherency to withstand sectioning and polishing. Fired pellets sometimes lack coherency and frequently contain holes which are troublesome during polishing. Impregnation of both air-dried and fired pellets is readily accomplished by the use of methyl methacrylate monomer.3 The dry pellets are covered in a test tube with excess monomer, to which a small amount of accelerator has been added. When the test tube is placed in a cooling bath and evacuated with an aspirator, most of the entrapped air is removed, and disruption of weak pellets by boiling of the monomer is reduced to a minimum. Polymerization is then effected by immersion of the test tube in a water-bath at about 45°C, this temperature being held for 4 or 5 days. The test tube may then be broken away from the solidified mass and the pellets sectioned by a carborundum wheel or a diamond saw. Where time is important, impregnation is carried out at a higher temperature by Meyer's method.4 Air-dried pellets must be impregnated with especial care; otherwise swelling occurs and the solids are displaced. It is more important to be certain that the monomer forms a reasonably complete network throughout the specimen than that all entrained air is removed, and for this reason the vacuum technique may be omitted. Impregnated agglomerated products and pellets are extremely coherent, section well, and may be polished either by hand or by machine. Hand polishing is not satisfactory for the examination of conditions existing at the boundaries of grains, and for this machine polishing must be used. The Graton-Vanderwilt machine gives excellent results, provided that pressure on the specimen is considerably in excess of that recommended by the manufacturer. Mineralogy of Fired Pellets Only two opaque iron minerals, magnetite and hematite, have been recognized in pellets. The complete identity of these artificial minerals with their corresponding natural counterparts is shown by their mineralographic characteristics and their X-ray structures. Wüstite has not been found. Slag is the most common transparent constituent of fired pellets. Occasionally conditions have been appropriate for the crystallization of fayalite from the slag, and at other times another crystalline sil-

Jan 1, 1952

By Norman F. Schulz, Emert W. Lindroos, Strathmore R. B. Cooke

DURING the course of an investigation of the effects of various starch products on hematite and quartz in regard to their separation by flotation, it was found that whereas most starches flocculated suspensions of hematite in water, they did not flocculate similar suspensions of quartz. However, a derivative of whole corn starch containing approximately one tenth aminoethyl group (-—CH,CH2NH2) per glucose unit proved to be an exception. This aminoethyl starch was a very good flocculant for both hematite and quartz, and also possessed the property of depressing both minerals in cationic flotation tests. In view of the widespread use of starch as a flocculating agent of solids in tailing water, pulps, and for coal slimes, ore and various other purposes in sulphide and nonsulphide flotation, attention is called to the effective surface activity of aminoethyl starch in flocculating suspensions of the two minerals investigated. Test Materials The starch products employed included Globe Pearl starch No. 144 and fresh aminoethyl starch, both supplied by the Corn Products Refining Co. Dr. A. L. Elder" has kindly furnished a description The minerals used in the various tests are listed in Table I. Their specific surfaces were determined by the air permeability method, which gave results reproducible to within plus or minus 3 pct. Surface areas obtained by krypton adsorption were greater than the air permeability values by a factor of 2.0 for quartz and 62.4 for hematite. Starch Adsorption on Mineral Surfaces Starch adsorption data were obtained by agitating for 1 hr measured volumes of neutral starch solutions of known concentrations with weighed quantities of finely divided mineral of measured specific surface. The mineral then was separated from the pulp liquor by centrifugation and the residual starch content determined by chemical analysis. The analytical procedure consisted of oxidizing the starch with an excess of dichromate in acid medium at elevated temperature and titrating the excess dichromate by the ferrous ammonium sulphate—potassium permanganate method. Analytical results were reproducible to within less than 1 pct. Adsorption data obtained in unbuffered solutions near the neutral point are plotted in Fig. 1. The adsorption on either mineral was far greater for the aminoethyl starch than for the Pearl starch. Flocculation The degree of flocculation was determined for a given pulp by measuring the time required for the supernatant liquid to reach a certain degree of clarity. This was accomplished by passing a standard light beam through the pulp, contained in a glass settling tube, and measuring the time required after agitation ceased for the intensity of the transmitted beam to reach a predetermined value. Starch reagent was added to each pulp in small uniform increments, and the settling time was determined after each such addition. Increase in pulp liquor volume due to the added starch reagent was ignored in these tests. Pulps were maintained at or near neutrality. of the preparation of the aminoethyl starch: "Three hundred and sixty grams of powdered unmodified corn starch was slurried in 3 liters of water and stirred during gelatinization. Eighty-six grams of ethylenimine was added slowly during reflux which was continued for 4 hr. The yellow solution set to a gel upon cooling. This was broken up and neutralized with HC1. The thick paste was dried on hot rolls. Adsorbed polyethylenimine and salts were removed from the yellowish products by washing first with acidified aqueous '60 per cent' alcohol. The white product contained nitrogen corresponding to about one aminoethoxy group per ten glucose residues." Only laboratory samples of this starch derivative have been prepared. The starch reagents for use in flocculation, flotation, and adsorption tests were made up by dispersing the appropriate quantities of air-dry starch in cold water, adding boiling water, and heating for 30 min at 120°C under pressure. When used ip adsorption tests, the starch solutions first were cleared of insoluble matter by centrifugation.

Jan 1, 1953

By Strathmore R. B. Cooke, Emert W. Lindroos, Norman F. Schulz

DURING the course of an investigation of the effects of various starch products on hematite and quartz in regard to their separation by flotation, it was found that whereas most starches flocculated suspensions of hematite in water, they did not flocculate similar suspensions of quartz. However, a derivative of whole corn starch containing approximately one tenth aminoethyl group (-—CH,CH2NH2) per glucose unit proved to be an exception. This aminoethyl starch was a very good flocculant for both hematite and quartz, and also possessed the property of depressing both minerals in cationic flotation tests. In view of the widespread use of starch as a flocculating agent of solids in tailing water, pulps, and for coal slimes, ore and various other purposes in sulphide and nonsulphide flotation, attention is called to the effective surface activity of aminoethyl starch in flocculating suspensions of the two minerals investigated. Test Materials The starch products employed included Globe Pearl starch No. 144 and fresh aminoethyl starch, both supplied by the Corn Products Refining Co. Dr. A. L. Elder" has kindly furnished a description The minerals used in the various tests are listed in Table I. Their specific surfaces were determined by the air permeability method, which gave results reproducible to within plus or minus 3 pct. Surface areas obtained by krypton adsorption were greater than the air permeability values by a factor of 2.0 for quartz and 62.4 for hematite. Starch Adsorption on Mineral Surfaces Starch adsorption data were obtained by agitating for 1 hr measured volumes of neutral starch solutions of known concentrations with weighed quantities of finely divided mineral of measured specific surface. The mineral then was separated from the pulp liquor by centrifugation and the residual starch content determined by chemical analysis. The analytical procedure consisted of oxidizing the starch with an excess of dichromate in acid medium at elevated temperature and titrating the excess dichromate by the ferrous ammonium sulphate—potassium permanganate method. Analytical results were reproducible to within less than 1 pct. Adsorption data obtained in unbuffered solutions near the neutral point are plotted in Fig. 1. The adsorption on either mineral was far greater for the aminoethyl starch than for the Pearl starch. Flocculation The degree of flocculation was determined for a given pulp by measuring the time required for the supernatant liquid to reach a certain degree of clarity. This was accomplished by passing a standard light beam through the pulp, contained in a glass settling tube, and measuring the time required after agitation ceased for the intensity of the transmitted beam to reach a predetermined value. Starch reagent was added to each pulp in small uniform increments, and the settling time was determined after each such addition. Increase in pulp liquor volume due to the added starch reagent was ignored in these tests. Pulps were maintained at or near neutrality. of the preparation of the aminoethyl starch: "Three hundred and sixty grams of powdered unmodified corn starch was slurried in 3 liters of water and stirred during gelatinization. Eighty-six grams of ethylenimine was added slowly during reflux which was continued for 4 hr. The yellow solution set to a gel upon cooling. This was broken up and neutralized with HC1. The thick paste was dried on hot rolls. Adsorbed polyethylenimine and salts were removed from the yellowish products by washing first with acidified aqueous '60 per cent' alcohol. The white product contained nitrogen corresponding to about one aminoethoxy group per ten glucose residues." Only laboratory samples of this starch derivative have been prepared. The starch reagents for use in flocculation, flotation, and adsorption tests were made up by dispersing the appropriate quantities of air-dry starch in cold water, adding boiling water, and heating for 30 min at 120°C under pressure. When used ip adsorption tests, the starch solutions first were cleared of insoluble matter by centrifugation.

Jan 1, 1953

By R. E. Somers

Discussion of the paper of R. E. SOMERS, presented at the San Francisco meeting, September, 1915, and printed in Bulletin No. 101, May, 1915, pp. 957 to 996. A. C. LAWSON, Berkeley, Cal.-One point to which Mr. Graton (in summarizing the paper for us) called attention is that the author had not explained why some copper was fixed in the zone of oxidation. I recollect very well puzzling over that question at Ely, Nev., some years ago. Mr. Sales, in his paper on Butte,1 suggests the explanation. It is clue according to him to the paucity of pyrite in the primary ore. Where there is abundant pyrite sufficient sulphuric acid is formed by oxidation to take all the copper into solution and carry it to lower levels; but where the pyrite is scant so that insufficient sulphuric acid is formed, some of the copper is carbonated and so fixed in the gossan. The hypothesis, or some modification of it, as for example the combination of the sulphuric acid with lime, would appear to explain satisfactorily the fixation of the copper in the gossan as carbonate. I have, however, had no occasion in recent years to study the phenomenon. L. C. GRATON, Cambridge, Mass.-As I remember, the rocks in which the chrysocolla occurs in the Burro Mountains are both silicified and kaolinized. It seems probable that in surroundings deficient in carbon dioxide, complete oxidation of chalcocite may yield chrysocolla up to a maximum of half the copper in the chalcocite; while in rocks, like garnet contact zones and certain easily decomposable porphyries, surface decomposition appears often to yield silica in the necessary form to convert the copper of primary sulphides into chrysocolla immediately and directly upon oxidation.

Jan 12, 1915

By M. S. NORTH

IT may be a far cry from the days of the old horse whim, and it is relatively a long way back to hand production in factories. Modern machinery has made possible deep shaft-sinking, newer methods have increased the recovery of mineral. Technically, excavating and ore dressing have advanced as has mass production and its many ramifications in the manufacture of commercial product. To those of the mining industry who would have us believe that mining and manufacturing are totally different enterprises, it can be said that certain differences do exist. These differences rather than being fundamental are the result of adhering to past practices which were possibly sound years ago but do not measure up today. Differences in managerial control, sales, and distribution, cost finding, etc., are often so pronounced that efforts to compare or contrast are almost futile.

Jan 1, 1930

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

August 10 to 14, 1914, inclusive Headquarters will be at the Hotel Utah. The following program of the meeting has been arranged y the Local Committees: Monday, August 10.-Members and guests will register at the Secretary's desk in Room C-38, Hotel Utah, and receive the official badges, booklets and programs of the meeting. At 2:30 P. M., there will be an organ recital at the Mormon Tabernacle, after which members and guests will be taken for a trip around Salt Lake City in sight-seeing motor cars. At 8:30 P. M., the ladies will assemble in the lobby of the Hotel Utah, where they will be met by the members of the Ladies' Entertainment Committee, and will be taken for an automobile drive about the city. At 8:30 P. M., a technical session will be held in the ballroom of the Hotel Utah. The following papers will be presented: F. W. BACORN: An Amendment to Sales's Theory of Ore Deposition. C. W. GOODALE: Drumlummon Mine, Marysville, Mont. I. B. JORALEMON: The Ajo Copper-Mining District. STUART CROASDALE: Leaching Experiments on the Ajo Ore. FRANK R. VAN HORN: The Occurrence of Bournonite, Jamesonite, and Calamine at Park City. HOWLAND BANCROFT: Dip Chart. M. N. ALLING: Ancient Auriferous Gravel Channels of Sierra County, California. B. S. BUTLER AND H. D. MCCASKEY: Copper Ores of the New London Mine. GEORGE A. PACKARD: Rope Idlers in the Raven Shaft. ARTHUR CROWFOOT: Development of the Round Table at Great Falls. FREDERICK LAIST AND A. E. WIGGIN: The Slime-Concentrating Plant at Anaconda. W, L, AUSTIN: The Treatment of Copper Ore by Leaching Methods. W. L. AUSTIN: Leaching Copper Products at the Steptoe Works.

Jan 8, 1914

By J. W. Rutter, K. T. Aust

THE object of the experiments to be described in this report was to determine, first, which grains, out of a large number introduced into a sample in which their growth could proceed, were able to grow most successfully; and, second, the factors which control their growth selection. In an earlier study of grain boundary migration in high-purity lead,' it was found that, under some conditions, the most successful grain in an experiment of this type bears a special orientation relationship to the grain into which it is growing. The present work represents an extension of the previous study, directed at the determination of the orientation relationships which appear under a wider variety of conditions. Experiments of this general type have been done using commercial aluminum2 with somewhat conflicting results. In the present experiments, in contrast to the above,' the sample composition was a principal controlled variable, resulting in a considerable clarification of the phenomena observed. EXPERIMENTAL TECHNIQUE The experimental technique used in this investigation was essentially that employed previously in studies of grain boundary migration kinetics.1'3 The material used was zone-refined lead with various small amounts of tin or silver added to study the effect of varying the sample composition. The specimens were in the form of single crystals, about 1/4 in. 1/4 in cross section by 3 to 4 in. in length, grown from the melt in a horizontal graphite boat. A crystal grown in this way generally contained a lineage or "striation" substructure of the type shown in Fig. 1 of Ref. 1. This substructure consists of an array of low-angle boundaries which partition the crystal into regions misoriented from each other by a few degrees. The substructure constitutes a source of driving energy, estimated to be about 4000 ergs per cc, for the migration of a large-angle grain boundary into the striated crystal. New grains were introduced by plastic deformation in compression of a localized reglon at one end of the sample. Re-crystallization occurs at room temperature in the deformed region, introducing a large number of new, striation-free grains into the specimen. These grains are able to grow into the melt-grown crystal on annealing at a suitable temperature. The stria-tions are removed by passage of the grain boundary, as the substructure energy is utilized to produce the boundary migration. Usually, only one or two of the recrystallized grains persist after growth has occurred for about 1 cm out of the deformed region. Laue back-reflection X-ray photographs were obtained to determine the orientation relationship between the melt-grown crystal and the recrystallized grain or grains which grew most successfully in each specimen. EXPERIMENTAL OBSERVATIONS Fig. 1 shows the results obtained for a series of specimens to which had been added tin in the range from 0 to 5 ppm by weight. In this figure is plotted, in the standard stereographic triangle, the single axis about which the most successful recrystallized grain or grains are related to the starting, melt-grown crystal by the smallest rotation. The range of angular rotations observed about such axes is indicated beside each stereographic triangle. The results shown in the stereographic triangle on the left, Fig. l(a), were obtained by localized deformation at one end of each specimen at room temperature, followed by annealing in a furnace which had been preheated to 300°C. The furnace atmosphere was argon. It will be seen that the orientation relationships observed between the melt-grown and recrystallized grains are quite random. On the right, Fig. l(b), are shown results for samples in which the de-

Jan 1, 1961

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

By R. T. DeHoff

A general method for determining the geometric properties of structures composed of particles which are all the same shape and size is presented. The application of the method requires a knowledge of' the qualitative shape of the particles in the structure, ad a maximum of three simple counting measurenzents, which are made on a representative plane section taken through the structure. It is also shown that the number of different kinds of measurements necessary JOY the complete description of the structure can be decreased if some independent information about individual particles is available. The geometric properties that can be determined quantitatiz~ely from counting measurements for susch structures are size, shape, number, surface area, vlolume, ad such extensive properties as volume Mction and surface area per unit volume. THE simplest kinds of measurements that may be made on a metallographic section are counting measurements. There are three such simple counting measurements, which are determined by sampling the microstructure with a point, a line, and an area. The first of these, the point count, is probably the most familiar among metallographers. The second count, the number of intersections a test line makes with particle outline, is somewhat more recent in its origin and application. The third counting measurement, the number of particle sections observed in unit area of the plane of polish, has long been used in the estimation of grain sizes. The real utility of these three counting measurements lies in the fact that they are rigorously and unambiguously related to certain extensive geometric properties of the three-dimensional structure of which the metallographic section is a sample. These relationships will be reviewed briefly below. Of somewhat secondary importance to the fundamental relationships is the observation that, if some simplifying assumptions about the geometry of the three-dimensional structure are introduced, manipulation of the counting measurements gives a more complete description of the structure. Specifically, in addition to the extensive properties which these measurements rigorously estimate, the number of particles, their size, and their shape may be determined. The purpose of the present paper is to explore the consequences of introducing the assumption of constant size and shape. A later paper will deal with the estimation of geometric properties of structures which may be characterized by a two-parameter size distribution. It should be mentioned that the introduction of this simplest of assumptions, while clearly not generally justified in metallurgical structures, is not without precedent. For example, many estimates of the number of particles per unit volume of structure, based upon a single counting measurement, are scattered throughout the literature.13 Virtually all of these developments assume a constant particle shape, e.g., spherical or polyhydral, and constant size. That such an assumption is necessary is evident from the fact that, for more general structures, more than a single parameter is required to describe the three-dimensional structure, so that the determination of a single parameter on a section would be insufficient to specify the structure. Similar developments for the estimation of particle size from a single counting measurement, e.g., routine grain-size determinations, make the same very limiting assumption,435 but have nonetheless proven of practical value. The present paper embodies a generalized approach to the development of relationships among the two-dimensional counting measurements and the three-dimensional geometry of the structure, subject to the assumption of constant particle size and shape. It is the hope of the author that by presenting the relationships and the assumptions involved in dealing with this approximation, in a single, unified treatment, the reader may be impressed with the usefulness of the counting measurements, may be guided in their application to the estimation of details of the geometry in specific structures in which he may be interested, and may be moved to apply the results, with understanding, to new structural problems. Several authors6, 7 have demonstrated independently that it is possible to obtain unbiased estimates

Jan 1, 1964

By A. U. Seybol

Eight binary iron alloys were examined after ion nitriding experiments to determine the behavior of the following elements: Al, Mo, Mn, Si, Ti, V,Cr, and C. Only Al, Cr, Ti, and V additions caused hardening in binary iron alloys. A few steels were examined to see the effect of Cr, Cr + Al, Cr + Ti, and Cr + V. It is suggested that a useful new class of ni-triding grade steels might be those containing about I pct V. The nitriding of steel, first described by Fry1 about 45 years ago, rapidly attained commercial application with very little knowledge of the fundamentals involved. While Fry,' in describing the status of nitriding in 1932, apparently correctly postulated hardening by precipitated nitrides, the details of the nitriding process were not understood, nor has the situation changed much since that time. It is also interesting to note that the compositions of some typical nitriding steels given by Fry at that time have changed little in the intervening years. Currently used nitriding steels owe their surface hardening to either chromium (as in 4340 steel) or aluminum plus chromium as in the Nitralloy grades, where both CrN and AlN appear to contribute to harden ing. Titanium additions have been studied experimentally, but thus far titanium steels have not won wide commercial acceptance. This subject will be expanded later. The orthodox ammonia nitriding process has been reviewed very adequately many times as in Jenkins3 and Case and VanHorn,4 and their is no need to outline the process here. Ion nitriding is not as well-known, although there have been several descriptions5-9 of the process given, sometimes with comparisons with the ammonia process. Most of these papers are primarily concerned with a description of the equipment, or of the physics or electrical engineering aspects of ion nitriding, but Noren and Kindbom9 gave the results of a metallurgical investigation using both processes. In brief, ion nitriding is carried out in a vacuum chamber from which the air is exhausted and replaced by a N2-H2 mixture, typically containing 10 to 20 pct N2, at about 5 to 10 torr pressure. While ammonia gas has also been used in ion nitriding, there is no evidence that ammonia makes any improvement in the ion nitriding process. A few hundred volts dc is applied between the grounded container wall (positive) and an insulated center post supporting the work (negative) to be nitrided. A glow discharge is created in the ionized gas, accelerating positive nitrogen ions to the work. These ions contain enough energy to form the normally unstable Fe4N "white layer", thus establish- ing surface nitrogen solubility characteristic of the a Fe/Fe4N equilibrium. This creates a substantial concentration gradient, driving dissolved nitrogen into the steel. The temperature employed is in the same range (around 500" to 550°C) as in ammonia nitriding, but because of factors which are not understood at present the nitriding time is ordinarily considerably reduced in ion nitriding. Other advantages have been cited,9 but it is not the purpose of the present work to contrast the two processes. The present objective was to examine the behavior of binary iron alloys during ion nitriding with respect to the microstructure, hardness level, and depth, and to examine some of these factors in steels as well. In this way it was hoped to be able to find out something about the individual role of these elements in steels. While all the work was done by ion nitriding, there seems to be no reason why any conclusions reached would not equally apply to ammonia nitriding, excepting only the kinetic aspects of the process. Another objective was an exploration of the critical-ity of the ion nitriding variables: gas composition, pressure, temperature, and time. EQUIPMENT AND MATERIALS The equipment used was substantially as described by Jones and Martin.8 The vacuum tank was about 12 in. in diam by about 18 in. high, and consisted of water-cooled stainless steel, with a single small window at the top for viewing inside. This sat on a heavy mild steel base equipped with the main pumping port, pressure control port, and vacuum gaging. A series of variable resistances was interposed between the glow discharge and a large-capacity -40 amp variable primary transformer feeding a 1000-v transformer, but 600 v were about the maximum ordinarily used. With the small l-in.-round, 4-in.-thick discs used for nitriding, the electrical load was usually about 500 v at 0.8 amp. The specimen temperature was controlled by a stainless-steel sheathed chromel-alumel couple, whose junction was in the steel stool upon which the flat discs were placed. These were ground through 400 Sic paper. Cycling of the temperature controller caused -0.2 amp variation in ion current, providing an ample control band. The binary iron alloys were made from vacuum-melted hydrogen-deoxidized electrolytic iron and alloys of 99.9 pct purity. Cast ll-lb-square tapered ingots were forged and hot-rolled to about 11/4-in.-diam rounds. Discs of 1/4 in. thickness by about 1 in. diam were machined from the rods for nitriding specimens. The following alloys were prepared: 1 pct each of Mn, Mo, Cr, Ti, Al, V, Si, and an Fe-0.8 pct C alloy. EXPERIMENTAL VARIABLES Of the variables total gas pressure, nitrogen partial pressure, temperature, and time, only nitrogen partial pressure was found to be critical to the operation. A critical nitrogen partial pressure was found corre-

Jan 1, 1970

By A. D. Mutch

IT has long been known that there are wide variations in the thermo-electric potential of pyrite. In the last few years a study of this variation and other properties of pyrite was carried out at the University of Toronto by F. G. Smith on specimens of pyrite from many loyalities. As a result of these studies the pyrite geothermometer was developed by Professor Smith. The calibration of the pyrite geothermometer is based on the assumption that "crystals of any one electronically conducting mineral species deposited at a high temperature have a more positive thermoelectric potential than crystals deposited at a low temperature, and the thermo-electric potential varies continuously between any given limits of the temperature of deposition." The cause of the variation was postulated to be crystal discontinuities, such as lineage boundaries. As yet this postulated relationship has not been established as fact. On theoretical grounds it is indicated that the thermo-electric potential of pyrite or any other partial conductor is dependent upon a number of factors as well as the temperature of formation. For this and other reasons there is ground for doubt as to the validity of the relationship postulated above. To date a large number of readings have been made with the pyrite geothermometer which have been recorded in terms of the calibration of the instrument in degrees centigrade. So far most of the pyrite tested by this technique has been in association with gold ore. The values for the temperature of formation obtained in these tests appear to be reasonable and, in relation to geological problems, to vary in the right sense. Determinations on some specimens not in association with gold ore have given readings that appear to be much too high, taking into account the probable maximum temperature of the host rock. To sum up, although many determinations made with the pyrite geothermometer appear to give reasonable values for the temperature of formation of the pyrite, there are at the same time other readings which seem anomalous. On the basis of an examination of available results of work with the pyrite geothermometer, two problems must be considered: 1—the validity of the calibration of the pyrite geothermometer; and 2— the nature of the distribution of the thermo-electric potentials of pyrite in relation to the specific problems that have been examined. In this paper the academic problem relating to the validity of the calibration of the pyrite geothermometer will not be discussed. Instead, the variations of thermo-electric potential of pyrite in association with gold veins will be discussed with regard to specific examinations. The first of these two examinations deals with the distribution of thermo-electric potentials of pyrite in association with a gold vein and was carried out in the McIntyre Porcupine Mine, Schumacher, Ont., in the summer of 1949 as part of a study with this technique. The second problem deals with variations of thermo-electric potential of pyrite in gold ore specimens from all over the world. The specimens used in this study were part of the private collection of Frank Ebbutt, geologist for Howe Sound Exploration Co. Results of Detailed and Reconnaissance Studies In discussion of the results of determinations made in these two studies the values of thermo-electric potential in millivolts will be used. It will be noted that in some of the diagrams the determinations are recorded in terms of pyrite geothermometer temperatures. Fig. 1 is a calibration chart relating pyrite geothermometer temperatures and thermoelectric potentials. A full discussion of the technique is given in the original paper by F. G. Smith.' Briefly, the determinations are made by placing two stainless steel probes, one hot and the other cold, against the surface of the pyrite crystal being tested. The thermoelectric potential that is developed is read with a null-point potentiometer that is calibrated in what

Jan 1, 1953

By A. D. Mutch

IT has long been known that there are wide variations in the thermo-electric potential of pyrite. In the last few years a study of this variation and other properties of pyrite was carried out at the University of Toronto by F. G. Smith on specimens of pyrite from many loyalities. As a result of these studies the pyrite geothermometer was developed by Professor Smith. The calibration of the pyrite geothermometer is based on the assumption that "crystals of any one electronically conducting mineral species deposited at a high temperature have a more positive thermoelectric potential than crystals deposited at a low temperature, and the thermo-electric potential varies continuously between any given limits of the temperature of deposition." The cause of the variation was postulated to be crystal discontinuities, such as lineage boundaries. As yet this postulated relationship has not been established as fact. On theoretical grounds it is indicated that the thermo-electric potential of pyrite or any other partial conductor is dependent upon a number of factors as well as the temperature of formation. For this and other reasons there is ground for doubt as to the validity of the relationship postulated above. To date a large number of readings have been made with the pyrite geothermometer which have been recorded in terms of the calibration of the instrument in degrees centigrade. So far most of the pyrite tested by this technique has been in association with gold ore. The values for the temperature of formation obtained in these tests appear to be reasonable and, in relation to geological problems, to vary in the right sense. Determinations on some specimens not in association with gold ore have given readings that appear to be much too high, taking into account the probable maximum temperature of the host rock. To sum up, although many determinations made with the pyrite geothermometer appear to give reasonable values for the temperature of formation of the pyrite, there are at the same time other readings which seem anomalous. On the basis of an examination of available results of work with the pyrite geothermometer, two problems must be considered: 1—the validity of the calibration of the pyrite geothermometer; and 2— the nature of the distribution of the thermo-electric potentials of pyrite in relation to the specific problems that have been examined. In this paper the academic problem relating to the validity of the calibration of the pyrite geothermometer will not be discussed. Instead, the variations of thermo-electric potential of pyrite in association with gold veins will be discussed with regard to specific examinations. The first of these two examinations deals with the distribution of thermo-electric potentials of pyrite in association with a gold vein and was carried out in the McIntyre Porcupine Mine, Schumacher, Ont., in the summer of 1949 as part of a study with this technique. The second problem deals with variations of thermo-electric potential of pyrite in gold ore specimens from all over the world. The specimens used in this study were part of the private collection of Frank Ebbutt, geologist for Howe Sound Exploration Co. Results of Detailed and Reconnaissance Studies In discussion of the results of determinations made in these two studies the values of thermo-electric potential in millivolts will be used. It will be noted that in some of the diagrams the determinations are recorded in terms of pyrite geothermometer temperatures. Fig. 1 is a calibration chart relating pyrite geothermometer temperatures and thermoelectric potentials. A full discussion of the technique is given in the original paper by F. G. Smith.' Briefly, the determinations are made by placing two stainless steel probes, one hot and the other cold, against the surface of the pyrite crystal being tested. The thermoelectric potential that is developed is read with a null-point potentiometer that is calibrated in what

Jan 1, 1953

By Thomas Clagett

THE Pocahontas coal field comprises the area in Tazewell County, Va., and Mercer 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 305m.) 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, io 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 off bone, each 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 25 per cent. ash, but contains some clean coal. The coal in both seams is quite soft. Cleavage sufficiently well defined to exert an influence on the mining is rare. Overlying strata are 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 5, 1922

By J. L. SCHUELER

THE writer has reread Mr. Ingalls' interesting article in the July, 1923, issue of MINING AND METAL- LURGY on "The Use of Spelter in Galvanizing." It seems that most writers, in commenting upon coatings of spelter on sheets and wire, dwell upon the thin coatings which these materials carry, and rightly so. However, they seem to forget that until very recently, in the case of wire, the manufacturer did not know how to apply a heavy coating of spelter to the wire, especially if the wire was to be woven into fence or fabricated in some other manner, because heavy coatings of spelter are exceedingly brittle. This is even true in the case of high-grade spelter, but to a lesser degree than with Prime Western. Because of this brittleness, it has been necessary for wire manufacturers to smooth the coating by passing the wire through tightly compressed wiping means of some kind, usually asbestos. This removes all of the excess spelter and allows only a thin coating to remain. The latter, as a rule, is malleable and the wire can be fabricated without material injury to the coating.

Jan 1, 1924

By J. A. Herrick

Jan 1, 1879