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By H. W. Hockin, D. r. Brandt, R. H. Walsh, P. L. Dietz, P. R. Girardot

New Jersey, Florida, and Canadian ilmenites were reduced with hydrogen or coke under various experimental conditions and the phase changes occurring in the ilmenite upon reduction have been studied by microscopic examination of polished sections and by X-ray diffraction. The products formed were dependent upon the type of ilmenite, temperature, time and reducing agent. Of the reducing agents, hydrogen was the more effective at lower temperatures. 1 HE possible utilization of ilmenite as a source of both iron and titanium has resulted in the development of a number of methods for the separation of the iron and titanium content. Slagging processes as currently used in Canada are typical of such methods. Somewhat less attention has been given industrially to the reduction of the iron content at less than the slagging temperature. Although references maybe found to such work, in general only one type of ilmenite, either natural or synthetic, has been studied by each author. We have attempted to draw some relationship between the results of experimental reduction and the type of deposit from which the ilmenite was derived, as evidenced by phases occurring in the ores and in the reduction products. Ilmenite ores having from 27 to 61 pct titanium dioxide were included in this study and in each case reduction was carried out at such temperatures that only limited coalescence of the particulate iron product occurred within the ilmenite grains. The history of the individual ilmenite samples and the temperature of reduction were found to determine the occurrence of various phases and the mode of distribution of the iron. REVIEW OF EARLIER WORK ON REDUCTION One of the earliest references to the reduction of ilmenite at less than the slagging temperature was made in 1917.' The metallic iron produced was_____ leached out by the action of dilute sulfuric or hydrochloric acid, to leave a product high in titanium dioxide. Subsequent to this, numerous patents2-'? and other references13"21 have appeared concerning reduction of ilmenite by carbon, hydrogen, carbon monoxide, methane, coal gas, water gas, or the like in the absence of fluxing agents. Mineragraphic examinations were not reported, and in the main, the only examinations made were chemical analyses. However, in two cases3,13, titanium suboxides were reported in the products and in one case2' rutile was reported, in addition to metallic iron. Both were identified by X-ray diffraction. While reductions in the absence of fluxing agents were generally followed by either a wet or dry chemical process for removal of the metallic iron, a Canadian source17 reported removal of the metallic iron by magnetic separation. By the addition of fluxing agents during reduction, the metallic iron has been coalesced into "pearls." Each reference to such a process23-28 has shown that the coalesced iron could be removed by magnetic or gravity means after the product was crushed. In the absence of fluxes, the coalescence did not generally occur. The major part of the present study has been limited to reductions without fluxing agents in order to determine the primary reactions of naturally occurring ilmenites. Titaniferous iron ores have also been studied,29-33 17, l9 their reduction having been used as the basis of a commercial process for beneficiation of such ores in Norway29 and more recently considered in the United States34,35. The ease of reduction of titaniferous iron ores relative to that of hematite or magnetite has been referred to,33 with the conclusion that the more

Jan 1, 1961

By F. W. Gibson

A detailed description of the smelting and refining operations of the Amax-Homestake Lead Toller's smelter at Buick, Missouri. This is one of two completely new lead smelting and refining operations to go into operation in the United States in over forty years. Incorporated into the operation are the new methods and equipment which have been developed and lend themselves to the particular metallurgy of this plant. The text, as well as the statistical data presented, represent actual current practice after 22 months of operation, and although the metallurgy is considered to be relatively simple, several metallurgical problems unique to Missouri concentrates are discussed.

Jan 1, 1970

By C. D. Dolman

Since the outbreak of the war we have discovered in the united States minerals of which there was no general knowledge, and which compared very favorably with anything that could be found in any foreign country. One of these was magnesite, or the carbonate of magnesium as it occurs in nature. This mineral crystallizes in the rhombohedra1 form, has a specific gravity of 3.00, molecular weight of 84.4, molecular volume of 28.1, and a hardness of 3.5 to 4.5.1 Had it not been for the development of the California deposits of this mineral and the discovery of immense new deposits in Stevens County, Wash., the production of steel during the war would have been more seriously handicapped than it was. Now that the war is over, we face the possibility of competition with the cheap Austro-Hungarian magnesite; and while that may not be so cheap as it was before the war, adequate protection should be given the producers in this country to insure the full development of our own resources. The consumption of magnesite in the United States in 1913, the year preceding the war, was 172,591 tons of calcined and 22,872 tons of crude magnesite. Less than 3 per cent. of this amount was produced at home. At the present time, practically all of the magnesite used in the United States is produced at home. Expensive plants have been constructed, extensive exploration work done, and production pushed to the utmost to supply the necessary requirements of the war. Thus a considerable industry has been built up within our borders. Some magnesite has been imported from Canada and Mexico, but the Canadian ore was of an inferior grade and could not be used satisfactorily. During the year 1918, production decreased in both the United States and Canada; the production in the United States was 225,000 tons in 1918 as against 315,000 in 1917, and in Canada 39,365 tons in 1918 as against 58,090 in 1917. This decrease was mainly due to over-production during 1917, the domestic demand being only 300,000 tons. The material produced and sold in the United States must contain, in the crude form, not more than 3.5 per cent. silica and 2 per cent. lime;

Jan 1, 1920

By Ernest L. Ohle

The newly opened Hayden Creek lead mine represents a variation from the usual Southeast Missouri type. Galena mineralization occurs in sandy dolomite cementing a conglomerate of granite boulders and in cracks in the boulders. The conglomerate occurs at the base of the Bonneterre formation on the slopes of two buried pre-Cambrian knobs. IN 1943 diamond drilling from the surface in an area 2 miles southwest of Leadwood, Mo., discovered a lead deposit of a markedly different character from the usual southeast Missouri type. Subsequent drilling of about 500 holes indicated several million tons of ore, and in 1950 a 701-ft vertical shaft was sunk into the orebody. This paper describes the geology of this interesting occurrence insofar as it is known from the drilling and the small underground exposure at the bottom of the shaft. Geology The location of the Southeast Missouri Lead Belt and of the Hayden Creek property are shown in Fig. 1. As shown here, there are two separate producing areas, one from which the larger tonnage has come, located near Bonne Terre, Flat River, Desloge, and Leadwood, and the other to the south around Fred-ericktown and including famous old Mine LaMotte. The best published description of Lead Belt geology is by Tarr.* In pre-Cambrian time in this area, an assemblage of granites and rhyolitic flow rocks was eroded to a mature topography. Sedimentation, beginning in the Upper Cambrian, filled in the valleys and gradually covered even the highest hills. The first formation deposited was the La-motte sandstone; it is successively overlain by the Bonneterre dolomite, the principal lead-prodbcing formation, then the Davis shale. the Derby-Doerun limestone, and a succession of Cambro-Ordovician cherty dolomites. Several of these formations may be found in direct contact with the pre-Cambrian as their deposition progressively overlapped the older rocks on the flanks of the igneous knobs and ridges. Immediately overlying the pre-Cambrian there is, not uncommonly, a thin basal conglomerate of granite or porphyry boulders, which is incorporated into the overlying sediments. Deposition of the lower part of the rock section was fairly continuous, and the Lamotte sometimes grades almost imperceptibly into the lower sandy Bonneterre. Since the sediments were deposited on an uneven floor, they tend to reflect the irregularities in that floor. Most of the steep dips found in the district, that is, dips in excess of 10°, are original dips and not caused by deformation. Such domelike structures in the sedimentary rocks around the igneous knobs have localized a considerable number of the orebodies in the district and particularly those in the Frederick-town area. Many of the larger orebodies, however, have no close relation to the pre-Cambrian topography. Most of the lead production has come from the lower 150 ft of the Bonneterre formation, where disseminated ore spreads laterally parallel to the bedding for great distances. Average stoping height is about 20 ft, but in a few places there are stopes over 175 ft high.

Jan 1, 1953

By Ernest L. Ohle

The newly opened Hayden Creek lead mine represents a variation from the usual Southeast Missouri type. Galena mineralization occurs in sandy dolomite cementing a conglomerate of granite boulders and in cracks in the boulders. The conglomerate occurs at the base of the Bonneterre formation on the slopes of two buried pre-Cambrian knobs. IN 1943 diamond drilling from the surface in an area 2 miles southwest of Leadwood, Mo., discovered a lead deposit of a markedly different character from the usual southeast Missouri type. Subsequent drilling of about 500 holes indicated several million tons of ore, and in 1950 a 701-ft vertical shaft was sunk into the orebody. This paper describes the geology of this interesting occurrence insofar as it is known from the drilling and the small underground exposure at the bottom of the shaft. Geology The location of the Southeast Missouri Lead Belt and of the Hayden Creek property are shown in Fig. 1. As shown here, there are two separate producing areas, one from which the larger tonnage has come, located near Bonne Terre, Flat River, Desloge, and Leadwood, and the other to the south around Fred-ericktown and including famous old Mine LaMotte. The best published description of Lead Belt geology is by Tarr.* In pre-Cambrian time in this area, an assemblage of granites and rhyolitic flow rocks was eroded to a mature topography. Sedimentation, beginning in the Upper Cambrian, filled in the valleys and gradually covered even the highest hills. The first formation deposited was the La-motte sandstone; it is successively overlain by the Bonneterre dolomite, the principal lead-prodbcing formation, then the Davis shale. the Derby-Doerun limestone, and a succession of Cambro-Ordovician cherty dolomites. Several of these formations may be found in direct contact with the pre-Cambrian as their deposition progressively overlapped the older rocks on the flanks of the igneous knobs and ridges. Immediately overlying the pre-Cambrian there is, not uncommonly, a thin basal conglomerate of granite or porphyry boulders, which is incorporated into the overlying sediments. Deposition of the lower part of the rock section was fairly continuous, and the Lamotte sometimes grades almost imperceptibly into the lower sandy Bonneterre. Since the sediments were deposited on an uneven floor, they tend to reflect the irregularities in that floor. Most of the steep dips found in the district, that is, dips in excess of 10°, are original dips and not caused by deformation. Such domelike structures in the sedimentary rocks around the igneous knobs have localized a considerable number of the orebodies in the district and particularly those in the Frederick-town area. Many of the larger orebodies, however, have no close relation to the pre-Cambrian topography. Most of the lead production has come from the lower 150 ft of the Bonneterre formation, where disseminated ore spreads laterally parallel to the bedding for great distances. Average stoping height is about 20 ft, but in a few places there are stopes over 175 ft high.

Jan 1, 1953

By W. D. Mayercheck

Beginning in 1974, the Bureau of Mines, US Department of Interior, sponsored research and development efforts related to further development and use of continuous face haulage in underground coal mines (Cowan, 1975). The Department of Energy continued this effort as of Oct. 1977. This paper represents an update of an article previously published in Mining Engineering magazine (Mayercheck, 1979). Development progress is summarized for a variety of prototype systems for components now being built, surface tested, or tried underground.

Jan 1, 1984

By Daniel R. Stewart, Ralph R. Sacrison

The function of the geological engineer is to assist in mine planning and operations by collecting, interpreting, and applying geologic data to the solution of engineering problems. The geologist supports this effort by collecting additional geologic information specifically useful to the engineer. This use of geologic information reinforces the value of mine geology to the mining process beyond the traditional role of orebody definition. Work discussed includes: evaluation of caving strategies at the Climax and Henderson mines, support definition and slope stability at the Climax mine, and some uses of geology in cavability estimation for the Mount Emmons project.

Jan 1, 1984

By S. G. Malghan, A. L. Mular

Size distribution and surface area measurements play an important role in the characterization of crushed and ground granular materials properties. This paper outlines sampling methods of granular materials followed by a detailed treatment of principles of size and surface area measurements of a wide range of sizes from crushers feed to ball-mill ground sub-micron particles. Currently available equipment for size distribution and surface area analysis is described and critically examined with respect to advantages, range of application and precautions in their use. Equipment for on- stream size analysis is also evaluated. Finally, a list of criteria are given for selection of particles size and surface area measuring devices for a particular application.

Jan 1, 1982

By S. F. Reiter, W. R. Hibbard

A survey of the effect of heat treatment on the room temperature hardness of Fe-Mo alloys has been made. Constant strain rate tensile tests were performed between room temperature and 1800°F. These data were analyzed to determine the effect of temperature and composition on the strain hardening coefficient and strain rate sensitivity. Constant load creep-rupture tests were made on these alloys and the results related to composition and structure. A relation between the high temperature strength of the precipitation hardened alloys and the volume of precipitate has been observed. IN view of the extensive use of ferritic materials at elevated temperatures, it is surprising to note the limited amount of information relating the variables of plastic deformation, i.e., composition, structure, temperature, stress, strain, and strain rate. Hollomon and Lubahn' showed how the several variables of plastic flow might be treated analytically. No data were available on carbon-free iron and its alloys in a form suitable for this analysis. Several German investigations2-" constitute most of the experimental work relating high temperature properties to the constitution of these types of materials. In order to obtain new data, the iron-rich alloys of the Fe-Mo system were selected for detailed investigation for the following reasons: 1—Some of the important effects of molybdenum on the mechanical properties of iron have already been studied.' , 821 2—By suitable heat treatment of selected alloys, it is possible to study strengthening effects of four types: AT -a transformation, B—substitutional, C—precipitation, and D—dispersion of hard inter-metallic compound. Materials and Treatment Four-pound ingots were vacuum cast, employing the same melting schedule previously used.? The raw materials were electrolytic iron and lamp-grade molybdenum. The ingots were forged to l/z in. sq. rod and one portion swaged to 0.350 in. diam rod for the production of 1 15/16 in. long button-head specimens. The button-head specimen blanks were solution treated for 16 hr at 2100°F in hydrogen of —70°C dewpoint and then water quenched. They were subsequently plunge ground to the standard 0.160 in. diam test bar. Micrographs of the solution treated alloys are given in Figs. la through Id. The higher molybdenum alloys contained large equiaxed ferrite crystals similar to those in Fig. Id. A portion of the % in. rod was hot rolled to 0.100 in., sandblasted, and cold rolled to 0.020 in. Strip tensile specimens having a 0.020x0.200 in. cross-section and a 2.25 in. gage length were machined from the sheet. The alloys containing molybdenum were subsequently annealed 1 hr at 1560°F. The iron strip was annealed 4 hr at 1300°F in wet hydrogen. The resultant structures are shown in Fig. 2a through h. The ASTM grain sizes were 1 to 3 as solution heat treated or 3 to 4 as annealed. The chemical analyses of the alloys are given in Table I. Carbon contents were obtained after the heat treatments in hydrogen. Alloy 15.9 pct Mo was tested as a cast alloy.'

Jan 1, 1956

By Thomas T. Read

Mining, which is at least twenty cen-turies old, was at first, and long, wholly a practical art. Little more than two centuries have elapsed since the inception of the idea that general education and a knowledge of natural science would be of advantage to those engaged in the mining industry. Though schools of mining began to develop in Europe early in the eighteenth century the concept of educational preparation, for technical conduct of the industry was slow in winning general acceptance in the industry itself. John Hays Hammond, in his autobiography, recalls that when he sought employment with a mining company after he had graduated from Yale and Freiberg he had to assure its executive, before being even considered for employment, that he did not consider that he had learned anything about mining. This was as late as 1880. Existence in the industry of a prejudice against education of the academic type is perhaps an explanation why inadequate provision has been made by the mining industry for the continuing education of technical employees after they enter employment, although engineering education prior to engaging in industry has now won general acceptance. I am familiar with the existence of 'loop" courses for engineering graduates in metallurgical plants, of schemes for giving mining graduates "practical experience," and of the interest in vocational courses for workmen which sprang up in the period of labor shortage during and immediately following World War I (but which quickly died when the depression of 1921 again made experienced workmen available in sufficient supply), having been chairman of a committee appointed by the Mineral Industry Education Division to make a survey of existing provisions for post-employment training for engineers in our industry. The results of that survey, reported elsewhere, clearly indicate that it is inadequate as to amount; the aim of this paper is to present evidence for belief that it is also inadequate in quality. To avoid becoming too involved, no reference will be made here to post-employment vocational training for workmen, which is a subject differing so much from post-employment education for engineers as to require separate treatment. Neither will postgraduate education for metallurgical engineers be discussed, becadse a distinction must then be made between training for research work and for plant operation, whereas mining engineers engage almost exclusively in operations. Since the situation in the coal-mining industry has been discussed at several recent meetings, that also will be passed over, and what follows should be taken as a discussion applying exclusively to the metal-mining industry. Professional Development In the operations field (both in mining and metallurgy) the work to which a beginner is assigned is seldom closely related to previous academic education. The contrast is almost as great as between

Jan 1, 1943

By Thomas T. Read

Mining, which is at least twenty cen-turies old, was at first, and long, wholly a practical art. Little more than two centuries have elapsed since the inception of the idea that general education and a knowledge of natural science would be of advantage to those engaged in the mining industry. Though schools of mining began to develop in Europe early in the eighteenth century the concept of educational preparation, for technical conduct of the industry was slow in winning general acceptance in the industry itself. John Hays Hammond, in his autobiography, recalls that when he sought employment with a mining company after he had graduated from Yale and Freiberg he had to assure its executive, before being even considered for employment, that he did not consider that he had learned anything about mining. This was as late as 1880. Existence in the industry of a prejudice against education of the academic type is perhaps an explanation why inadequate provision has been made by the mining industry for the continuing education of technical employees after they enter employment, although engineering education prior to engaging in industry has now won general acceptance. I am familiar with the existence of 'loop" courses for engineering graduates in metallurgical plants, of schemes for giving mining graduates "practical experience," and of the interest in vocational courses for workmen which sprang up in the period of labor shortage during and immediately following World War I (but which quickly died when the depression of 1921 again made experienced workmen available in sufficient supply), having been chairman of a committee appointed by the Mineral Industry Education Division to make a survey of existing provisions for post-employment training for engineers in our industry. The results of that survey, reported elsewhere, clearly indicate that it is inadequate as to amount; the aim of this paper is to present evidence for belief that it is also inadequate in quality. To avoid becoming too involved, no reference will be made here to post-employment vocational training for workmen, which is a subject differing so much from post-employment education for engineers as to require separate treatment. Neither will postgraduate education for metallurgical engineers be discussed, becadse a distinction must then be made between training for research work and for plant operation, whereas mining engineers engage almost exclusively in operations. Since the situation in the coal-mining industry has been discussed at several recent meetings, that also will be passed over, and what follows should be taken as a discussion applying exclusively to the metal-mining industry. Professional Development In the operations field (both in mining and metallurgy) the work to which a beginner is assigned is seldom closely related to previous academic education. The contrast is almost as great as between

Jan 1, 1943

By L. C. Glenn

In the preparation of this paper the writer has drawn freely upon the writings of Orton, Munn, Shaw, Mather, Miller, Hoeing, St. Clair, Jillson, and others, as well as upon his own personal knowledge of the fields of both states. It is to be regretted that certain data gathered by him and his assistants last fall are not available for publication. Oil in Tennessee A few wells drilled for brine for salt making in Tennessee between 1820 and 1840 obtained oil, but no definite search was made for oil until just after the close of the Civil War. Active drilling was then begun in Overton and counties southwest of it on the eastern half of the Highland Rim. A number of strikes were made at shallow depths in the basal part of the Mississippian but the wells were soon exhausted and abandoned. Drilling was revived, about 1892, when the Spurrier district in Pickett County was developed and was followed by the Riverton district in the same county in 1896. A pipe line was laid from the Wayne County, Ky., fields and about 60,000 bbl. of oil were run before a very heavy slump in the production, a failure to find an extension of the field, and excessive local taxation caused the removal of the pipe line in 1906. There was then no production in Tennessee until the discovery, in 1915, of oil near Oneida, Scott Co., at about 950 ft. (289 m.) in fissures in the Newman or St. Louis limestone. This field, however, soon failed and was abandoned. In 1916, oil was found at Glen Mary, Scott Co., in the Newman limestone at a depth of 1232 ft. (375 m.) A number of wells have since been drilled there, some of which were dry while others, close by, were produccrs. The largest one yielded, at first, about 340 bbl. per day and produced for several months, when it suddenly went dry. Several of the first wells began at 6 or 8 bbl. per day and are still maintaining that output. Production is from a fissured part of the limestone and varies greatly in accordance with the size and extent of the ramification of the

Jan 1, 1921

By Earl S. Greiner, Eric R. Jette

The constitution of the iron-silicon alloys containing from 14 to 33.4 weight per cent silicon has been studied by a number of investigators, whose results have been reviewed in a monograph published by the Engineering Foundation1. In these previous researches, the solubility of silicon in iron was determined by thermal, microscopic or magnetic methods and the compound Fe3Si2 was reported to be stable at temperatures from 0 to approximately 1030' C. This paper describes the results of an X-ray investigation of the solubility of silicon in iron and gives data which prove that the Fe3Si2 phase is unstable below 825" C. In order to obtain the present results on the solubility of silicon in iron, the authors have utilized the lattice constants of the alpha-phase iron-silicon alloys given in a previous publication2, and also some additional data which will subsequently be described. Materials and Methods The alloys used in this investigation are listed in Table 1. They were prepared in 30 or 50-gram ingots by melting specially purified silicon and electrolytic or carbonyl iron in alundum crucibles under a pressure of less than 1 mm. of mercury. The purity of the silicon, electrolytic and carbonyl irons has been given by the authors in previous publications2, 5. The ingots were homogenized in vacuo at approximately 1000" C. for at least 96 hr. and then slowly cooled. The homogenized specimens were ground to powder in a hardened steel mortar. This powder was passed through a 150 or 200-mesh screen and sealed in evacuated quartz, Jena or Pyrex glass tubes and heat-treated as noted in the various tables. Specimens 23A, 24B, 33 and 35 and the specimens heated for one month at 700" C. were quenched by quickly removing the tubes from a horizontal tubular furnace and dropping them into water. The other specimens were quenched by means of a drop-quenching device, which has been described previously3.

Jan 1, 1937

By Gerald Sherman

Mine fires are always dangerous and are frequently accompanied by loss of life during the period of confusion which is apt to follow their discovery. In metal mines, fires may result from the accidental ignition of combustible material, or they may be of spontaneous origin resulting from the rapid decomposition of sulphide. They occur frequently enough to demonstrate the need of some special equipment and a general plan for controlling them, in addition to measures for their prevention. Nearly all the large copper mines have had fires, and the methods of fighting them have been well described in recent papers, notably by C. L. Berrien,1 R. E. Tally,2 and others in discussion. The Copper Queen mine has many shafts, which are connected by underground workings. The deeper parts are ventilated by fans, but in the shallower portions natural ventilation through numerous connecting raises or shafts is sufficient. There have been several fires in the past few years, of which all are extinguished but one, which is under control. These notes cover particularly the preparations that are being made to check a new fire, partially or temporarily, and to facilitate the escape of workmen in the interval before a definite plan of fighting it can be established. A fire may occur in a shaft or station, or in some working farther away. In case of fire in an upcast shaft, the gas would escape to the surface and the immediate result would probably not be dangerous to workmen, as they could escape by other shafts. In a downcast shaft, however, the gas would be distributed very rapidly throughout a large portion of the mine, and men might easily be trapped and asphyxiated. A fire in mine workings, drift, raise, or stope, would be dangerous in a degree, but the draft there is likely to be less strong than in a shaft and probably a smaller area would be invaded by the fire gases. At the Copper Queen mine, in all drifts connecting with individual

Jan 1, 1918

Jan 1, 1923

By J. B. Wagstaff

The raceway in front of the tuyere of the blast furnace has been studied quantitatively and a correlation obtained for the penetrastudiedtion of the blast. Some evidence is presented for the height and width of the raceway which suggests that all the raceways of a ffurnace overlap. The size of the coke in this zone has been measfurnaceoverlap.ured photographically during normal operation and results are given for the various areas. IN an earlier paper,' it was shown that a raceway exists opposite each tuyere of a blast furnace. This raceway is formed by the jet effect of the air emerging from the tuyere and consists essentially of a turbulence in which coke particles are recir-culated at high speed. Its presence was deduced originally from observations on movies taken with a high-speed camera through the tuyeres of various furnaces and was confirmed by experiments made on a model. In the model described,' this raceway was shown as operating in a vertical plane only, although there was a suggestion in the motion-picture film exhibited at that time that the raceway was three dimensional, unless artificially restricted. There was also some doubt then about the factors influencing its size. This paper describes the next steps in the investigation. Since the size of the raceway is obviously of importance in the operation of the furnace, it seemed worth while to study the subject more carefully. It is probably in this region that about half the coke in the furnace is consumed, so that the movement of the stock column may well be controlled by raceway behavior. Furthermore, there is some evidence to suggest that the coke is packed densely in the center of the furnace to form the "dead man" and more loosely above the raceway. It is therefore probable that the bulk of the gases passing up the stack flow from the top surface of this raceway. Clearly then, a knowledge of this critical zone is of interest to the blast furnace operator, and the first half of this report is devoted to a quantitative discussion of the subject. A further topic of interest among operators is the degree of breakdown of coke in the furnace, with which is inseparably linked the importance of a strong coke. Indeed, the whole question of the optimum size and type of coke may be as dependent on the condition of the coke in the bottom of the blast furnace as at the top. Attempts have been made from time to time to obtain samples of coke from the tuyeres and other furnace openings but they all suffer from the fact that the coke is filled to a varying degree with metal and slag and is probably broken up by the very act of taking the sample. It has proved difficult to make any reliable studies of coke size by these methods. However, it did seem possible to use the highspeed movies mentioned earlier1 to estimate the size of the coke. These movies provide an accurate record of individual coke particles so that, in theory at least, it should be possible to measure the size of the particles one by one and to obtain, for the first time, information on the coke being blown around the raceway under actual operating conditions while the furnace is performing normally. Such a study has been made and is discussed in the second half of this paper. The results obtained enabled the blast furnace data to be correlated with the model results given in the first half. Raceway Size In order to make a quantitative study of the size of the raceway it was necessary to devise some apparatus of laboratory scale, which could be handled quickly and easily. This focused attention on models, which in turn means that the laws of similarity governing this particular process must be ascertained. Method of Procedure: Since the work was to be carried out on a smaller scale than the blast furnace, the linear dimensions of the model became unimportant provided that the scale was known; it is only important to insure that the container does not affect the raceway being observed. The studies therefore were carried out in a glass-sided box, 11 in. high x 7 in. wide x 3 in. deep, using air jets ranging

Jan 1, 1954

By R. Varbanov, D. Nikolov, I. Nishkov

An interesting new flotation technique which reportedly improves mineral recovery over an extended particle size range-from 3 mm to 5 microns and below-has been developed by the Institute of Physical Chemistry, Bulgarian Academy of Sciences. Designated the "static" flotation technique, it is suited for upgrading tin, molybdenum, tungsten, uranium, gold, copper, lead, zinc, and other metallic ores. Recoverable nonmetallics include feldspar, sulfur, and phosphorite. Characteristic of the static flotation process are: •longer contact period (up to 1000 times longer between particles and bubbles, •low collision velocity and inertial forces between the contact and aeration in a thin pulp layer, • aeration without the harmful hydrodynamic repulsion upon particles below 5 microns (the pulp layer is only a few millimeters thick and rising bubbles collide with the particles either directly or in the thin foam films formed), •option to conduct the process with or without froth by film flotation at equilibrium contact angles, and • the use of inexpensive frothers and/or unstable froth with separate regulations of froth stability by hydrodynamic, ultrasonic, or electrostatic means.

Jan 10, 1979

The negative charges on diaphragms of quartz, tungstic oxides, stannic acid, acid dyestuffs, soaps, and glass have for a number of years been explained on the basis of chemical equilibria-a hydrogen ion or light metal ion passes into solution leaving the solid complex ion negatively charged. While there are a number of observations which indicate a proportionality between the ( potential and the streaming potential it should be recognized that all the experimental evidence thus far presented shows that if hydrogen ion concentration is kept at a constant value, electrokinetic phenomena are influenced by salts. The multivalent ions exert the greatest effect on the reduction of osmotic flow. In the interpretation of all electrokinetic data the assumption is made that the potential of the solid remains constant. That this is not true is evidenced by the values of ( potential for quartz in contact with conductivity water as reported by the several investigators and by the authors of this paper.

Sep 1, 1956

By J. R. Szedon, T. L. Chu, G. A. Gruber

Amorphous adherent filnzs of silicon dioxide have been deposited on silicon substrates by the oxidation of silane at temperatures ranging from 650 to 1050C. Various diluents (argon, nitrogen, hydrogen) were used to suppress the formation of SiO2 in the gas phase. Deposition rates of the oxide were determined over the temperature range in question as functions of' re-actant flow rates. Etch rate studies were used for a cursory comparison of structural properties of deposited and thermally grown oxides. From electrical evaluation of metal-insulator-silicon capacitors it was determined that the interface charge density of deposited films is similar go that of dry-oxygen-grown films in the 850° to 1050 C temperature range. Deposited films exhibit several ionic instability effects which differ in detail from those reported for thermal oxides. Stable passivating films of silicon nitride over deposited oxides appear to be practical for use in silicon planar device fabrication. Such films can be prepared under temperature conditions which have less effect on substrate impurity distributions than in the case of grown oxides. AMORPHOUS silicon dioxide (silica) is compatible with silicon in electrical properties and is the most widely used dielectric in silicon devices at present. Silica films can be prepared by the oxidation of silicon or deposited on silicon or other substrate surfaces by chemical reactions or vacuum techniques. The ability of thermally grown silicon dioxide films to passivate silicon surfaces forms one of the practical bases of the planar device technology. Properly produced and treated films of grown SiO 2 can have low densities of interface charge (-1 X 10" charges per sq cm) and can be stable as regards fast migrating ionic sgecies. 1 To maintain these properties, even with an otherwise hermetically sealed ambient, the Sia layers must be at least l000 A thick. Such thicknesses require oxidation in dry oxygen for periods of 7.8 hr at 900°C or 2 hr at 1000°C. Although oxidation in steam or wet oxygen can reduce these times to 17 and 5 min, the resulting oxides must be annealed to produce acceptable levels of interface charge., Oxidation or annealing involving moderate to high temperatures for extended periods of time can be undesirable. Under some conditions, there can be changes in the distribution of impurities within the underlying substrate. A chemical deposition technique using gaseous am-bients is particularly attractive and flexible for preparing oxide films. With a wide range of deposition rates available, films can be produced under condi- tions of time and temperature less detrimental to impurity distributions in the silicon than in the case of thermal oxidation. The pyrolysis of alkoxysilanes, the hydrolysis of silicon halides, and various modifications of these reactions are most commonly used for the deposition of silica films.3 Silica films obtained in this manner are likely to be contaminated by the by-products of the reaction, organic impurities, or hydrogen halides. The use of the oxidation of silane for the deposition process has been reported recently.4 The deposition of silica films on single-crystal silicon substrates by the oxidation of silane in a gas flow system has been studied in this work. The deposition variables studied were the crystallographic orientation of the substrate surface, the substrate temperature, and the nature of the diluent gas. The electrical charge behavior of Si-SiO2-A1 structures prepared under various conditions was investigated by capacitance-voltage (C-V) measurements of metal-insulator-semiconductor (MIS) capacitors. The experimental approaches and results are discussed in this paper. 1) DEPOSITION OF SILICA FILMS The overall reaction for the oxidation of silane is: The equilibrium constants of this reaction in the temperature range 500° to 1500°K, calculated from the JANAF thermochemical data,= are shown in Fig. 1. In addition to the large equilibrium constants, the oxidation of silane is also kinetically feasible at room temperature and above. However, the strong reactivity of silane toward oxygen tends to promote the nucleation of silica in the gas phase through homogeneous reactions, and the deposition of this silica on the substrate would yield nonadherent material. The formation of silica in the gas phase can be reduced by using low partial pressures of the reactants. Argon, hydrogen, and nitrogen were used as diluents in this work. 1.1) Experimental. The deposition of silica films by the oxidation of silane was carried out in a gas flow system using an apparatus shown schematically in Fig. 2. Appropriate flow meters and valves were used to control the flow of various reactants, i.e., argon, hydrogen, nitrogen, oxygen, and silane. Semiconductor-grade silane, argon of 99.999 pct minimum purity, oxygen of 99.95 pct minimum purity, and nitrogen of 99.997 pct minimum purity, all purchased from the Matheson Co., were used without further purification. In several instances, a silicon nitride film was deposited over the silica film. This was achieved by the nitridation of silane with ammonia using anhydrous ammonia of better than 99.99 pct purity supplied by the Matheson CO.' The reactant mixture of the desired composition was passed through a Millipore filter into a horizontal water-cooled fused silica tube of 55 mm

Jan 1, 1969

By E. J. Ripling

A NY mechanism proposed to explain hydrogen embrittlement in titanium and its alloys must, of course, be consistent with the experimental data that characterize this embrittlement. Unfortunately, however, the mechanical behavior of hydrogen-bearing titanium, at least a-ß titanium, has not been unequivocally defined. Lenning, Craighead, and Jaffee have clearly shown that hydrogen cmbrittles a-titanium by elevating its transition temperature, probably as the result of the formation of titanium hydrides. Therefore, in these alloys, hydrogen acts like at least one other interstitial contaminant, namely, nitrogen.&apos; On the other hand, ß-titanium has been shown by these same investigators to tolerate very large amounts of hydrogen without suffering severe mechanical damage.2 Mixing these two phases, however, to form the most important class of commercial alloys, the a-ß alloys, again results in severe hydrogen embrittlement, although the mechanism by which the embrittlement is produced is not of the same type as that which causes brittleness in a alloys. Ductility damage due to hydrogen increases as the strain rate is reduced in a-ß alloys, while embrittlement in a alloys increases as the strain rate is increased, since the latter is a transition temperature behavior. Steel, like the a-ß alloys, becomes more hydrogen sensitive at slow strain rates, suggesting that the mechanism producing the embrittlement in these two metals is similar. Brown and Baldwin&apos; described the hydrogen-produced ductility depression in steel as a function of testing temperature and strain rate by defining the slope of the two surfaces that produced the depression in a three dimensional chart, Fig. 1. One of these surfaces was given by the equations (de/de)4 > 0 (de/dT) < 0 [1] while the other was defined by the pair of equations Surfaces of the type given by Eq. 1 are suggested in two ways. One is an embrittlement mechanism wherein the diffusion rate of hydrogen is competitive with the rate at which the material is being deformed, as suggested by the planar pressure theory of Zapffe and his co-workers.&apos; The other is the diffusion controlled extension of Orowan&apos;s theory on delayed fracture in glass by Petch and Stables.&apos;&apos; Surfaces of the type given by Eq. 2 are also compatible with a mechanism of pressure build up in voids, according to de Kazinczy,&apos; since the solubility of hydrogen in the metal increases with testing temperature so that as the temperature is raised, the pressure in the voids is reduced. Kotfila and Erbin recently presented some data on the dependence of ductility on testing temperature and strain rate for the a-ß 3 pet Mn complex alloy at four different hydrogen levels.H Although data were presented for only three testing temperatures at three different strain rates, their results indicated that surfaces of the types defined in Eqs. 1 and 2 are produced in the alloy when the hydrogen level is sufficiently high—200 and 300 ppm—Fig. 2. Jaffee and his co-workers presented data on a number of different a-ß alloys which indicated the existence of surfaces of the type described by Eq. 2, but the ductility recovery at low temperatures as given by Eq. 1 was not found." In an attempt to aid in crystallizing this description of the ductility dependence of hydrogen-bearing a-ß alloys, tests were conducted by the author on a-ß titanium 140A with three different hydrogen contents. The tensile properties of two as-received rods and one vacuum annealed rod* were obtained over a range of testing temperatures and strain rates as shown in Figs. 3 and 4. Hydrogen analyses were made by the Battelle Memorial Institute on four pieces of the rod whose properties are shown as solid circles in Fig. 4. The hydrogen content of these pieces, taken at widely spaced intervals within the rod, were 280, 270, 289, and 270 ppm, indicating that the hydrogen content within a single as-received rod was quite uniform. One of the broken test pieces whose properties are shown in Fig. 3 as solid circles was also analyzed, and found to have a hydrogen content of 310 ppm. The analyses obtained on two of the vacuum annealed specimens were 92 and 170 ppm.

Jan 1, 1957