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By H. F. Walther

Basic electric-are furnace steel production mainly involves the use of two separate types of slags. The first, known as the "melt down" or oxidizing slag, which is in most cases removed from the furnace mechanically, and the heat finished under the second or deoxidizing slag, which is commonly known as the "finishing slag.'' The melt down slag is formed by the addition of lime or limestone to the charge, which combines with the oxides formed during the melting period and the product of any bottom erosion that may take place.

Jan 1, 1935

amounted to about 2000 metric tons. The total output is increasing from year to year. Marine salt is now produced in Haiti in quantity sufficient to supply nearly all the requirements of this Republic, so production tax is now collected. Central America Guatemala-The major production of salt in Guatemala is solar salt derived from sea water, but the Indian population prefers salt derived by boiling coastal marine earth. Salt is taxed by the Government. The industry has been beset by controversies in recent years, especially following the revolution of October 1944. The Government issued a decree in August 1940 designed to control production and price of salt. The creation of a salt consortium was provided for and marketing was to be governed by production quotas. It is understood that the Government pool was later dissolved and the industry is now under older laws whereby production and sales have no limits. South America Panama-Output of salt in Panama in a very recent year was 11,000 net tons of solar-evaporated sea salt. A Government bank is in charge of output and distribution of the product. Colombia-Rock-salt deposits are known in five places-Zipaquira, Nemocon, and Sesquile, in the Department of Cundinamarca, the Cumural y Upin near Restrepo, and San Miguel y Barital, near Medina in Meta Intendency. The latter deposit never has been worked on account of its inaccessibility. Saline springs are worked in four locations. The largest producer among marine salinas is Manare but it is now planned to make Bahia Honda the largest. Some evaporated salt is made in vacuum pans. The deposits at Zipaquira, Nemocon, and Sesquile are believed to occur in the domal type of deposit. All the salt resources are under Government control. Venezuela-The salt industry in Venezuela is under Government control and is taxed. Taxes in recent years, however, have been reduced for salt used in curing hides and salting meats, fish and fish products. Production has approximated 25,000 metric tons yearly but may now be considerably above that figure. The basin on the peninsula of Araya, State of Sucre, which at present is the only important source of salt, could produce at least 175,000 metric tons if more ground were provided-a larger supply than the entire country could consume. This unique landlocked basin of nearly 1000 acres lies 12 ft below sea level. Ecuador-Salt is a Government monopoly in Ecuador and is produced chiefly by solar evaporation close to the shore. The main producing center is on the Santa Elena peninsula, which supplies about 90 pct of the salt. Small fields are at Punta Arenas, Payana, and Chara-

Jan 1, 1949

By William E. Horst, John H. Bassarear

A technique is described which simplifies the standard procedure for measuring the Bond work index of a specific ore and illustrates how to overcome the strict requirements regarding feed size distribution normally encountered in operating plants. Actual results obtained from various process streams in a copper concentrator are presented and the grindability data are discussed in relation to the observed plant performance. This type of information can be used to gain a better understanding of plant behavior and to assist in the evaluation of plant modifications and process control studies.

Jan 1, 1977

By Stewart K. Griffiths

A general method-of-lines numerical approach for modeling gas driven fractures has been developed and tested. The numerical solutions agree very well with known similarity solutions for laminar and turbulent flow. Acceptable accuracy is obtained with a very few numerical grid points and with modest execution times. The model has also been checked against the results of several field tests, in which air was used to drive axisymmetric fractures into permeable tunnel-bed tuff.

Jan 1, 1984

By Tell Ertl, Ernest E. Burgh

The Bureau of Mines is operating an oil-shale mine 10 miles west of Rifle, Colo., as part of its Synthetic Liquid Fuels program. The purpose of operating this mine is twofold: First, to supply oil shale to an experimental Processing plant; and second, to develop practices and select methods for mining oil shale on a commercial scale at the lowest practicable cost. The second purpose—that of finding out how to mine oil shale most cheaply—entails considerable mining research. Since the drilling of oil shale probably will be one of the major items of the mining cost, fattors that influence drilling speeds were investigated. One phase of the drilling program was the development of a successful hard-surfaced rock-drill bit1 that can be used for drilling long holes in oil shale without changing bits. During that phase, drilling speeds were measured and drill cuttings were collected for assay and for screen sizing, when the cuttings from the individual tests were compared, a definite relationship was shown to exist between the drilling speed and the coarseness of the drill cuttings. Procedure Measurement of Drilling Speeds All drilling in the tests was done with a Model UMB-D-99W Gardner-Denver wagon drill. Round-lugged drill steel, 141 in. in diameter was used in 6, 12, and 18 ft lengths with 1/8-in. Timken H-type bits hard-faced with acetylene tube borium. The tests were made in the lower adit of the Bureau of Mines oil-shale mine; the grade of the oil shale drilled ranged from 18.6 to 42.7 gal per ton, During the experiments air pressure varied between 75 and go psi while water pressure remained fairly constant at 75 psi. All holes were drilled almost horizontally. Each drill hole was thoroughly cleaned of cuttings after being collared. The advance of the drill along the carriage was measured and recorded as the drilling speed in inches per minute. Method of Collecting Cuttings TO facilitate the collection of cuttings, each drill hole was collared in a smooth, vertical portion of the oil-shale breast (Fig 1). A galvanized-stee1 sheet was fastened to the breast below the area in which the hole was to be drilled. The cuttings washed out of the drill hole by the drilling water were guided by the steel sheet into a wooden box. The cuttings that remained in the drill hole after the drill was withdrawn were scraped out and placed in the same box as the cuttings washed out of the hole. After the cuttings from a I-min. drilling interval were collected, they were placed in flat metal pans. The fines were allowed to settle and the clear water was decanted. The cuttings then were dried in the sun.

Jan 1, 1949

By D. S. Eppelsheimer, D. N. Williams

The cold rolled textures of iodide titanium and of three samples of commercial titanium were examined using the Schulz-Decker Geiger counter technique. The iodide titanium and two of the three samples of commercial titanium showed a (0001) [1010] texture rotated 30' toward the transverse direction about an axis in the rolling direction. The third sample of commercial titanium showed a double texture. THE metals of the hexagonal system tend to deform similarly if the c/a ratios are similar. Thus titanium, zirconium, and beryllium, with c/a ratios of 1.601, 1.590, and 1.570, respectively,l should have similar cold rolled textures. The cold rolled texture of high purity iodide titanium has been described as (0001) [1010] rotated 30" toward the transverse direction about an axis in the rolling direction.' The texture of zirconium has also been reported as (0001) [1010] with a transverse rotation from the ideal position of approximately 30" about an axis in the rolling direction." This texture differs from that reported for titanium however since a continuous spread of (0001) poles toward the transverse direction was reported rather than distinct (0001) maxima 30" from the rolling plane normal. Beryllium has a texture similar to that of zirconium although the angle of transverse rotation of the (0001) poles is much less.' These three metals thus show a common type of cold rolled texture, as yet unexplained, which can be described as (0001) [1010] with various degrees of rotation toward the transverse direction about an axis in the rolling direction. Since titanium showed the greatest degree of rotation from the (0001) [1010] position, the cold rolled texture of titanium was re-examined using a semiquantitative Geiger counter X-ray technique to obtain more accurate experimental data from which a theoretical interpretation of this new type of hex- agonal rolling texture could be developed. The cold rolled textures of iodide titanium and of three samples of commercial titanium were determined. Table 1 gives the analyses of the titanium samples. Experimental Procedure Preparation of Samples: Prior to the final rolling operation each of the samples was given an initial reduction of approximately 50 pct and annealed to remove the gross effects of any previous treatments. Samples were annealed in vacuum, high purity helium, and air to determine whether annealing atmosphere had any effect on the cold rolled textures developed. All samples were annealed 1 hr at 800°C. Grain size determinations were made using the formula, 1.075 in which n is the number of grains counted in an area A (in sq mm) and M is the magnification of the area counted.' This formula gives the diameter between opposite flats assuming hexagonal grains. At least three areas containing more than sixty grains each were counted in each grain size determination. Rockwell B hardness readings were made on the annealed samples. The results of the measurements of

Jan 1, 1954

By Jan Law

Problems of oil recovery are attacked from the approaches dictated by the two strikingly dissimilar complexes that comprise an oil reservoir—the fluid complex and the interstitial complex. Knowledge of the fluid complex, due to labors in the fields of fluid mechanics and physical chemistry, has far outdistanced knowledge of the interstitial characteristics of the sand complex. This paper is concerned with the latter and applies the technique of statistics to petrographic facts—namely, porosity and permeability—dealing with what might be called petrometry. Statisticians have long worked within the problem of reconstruction of a universe oi variables by means of samples that comprise a small percentage of the universe from which the samples were drawn. Core-analysis data comply with the requisite of random sampling as stipulated by theoretical statistics. A basic concept of statistics employs t.he following substitution: 1. The results of sampling are arranged as a frequency distribution. 2. The observed frequency distribution is compared with a mathematically precise distribution. 3. If a sufficiently good agreement is found between the two, the precise distribution is substituted in all subsequent operations involving characteristics of the sampled material. This mathematically precise distribution is also known as the normal curve, curve of error, the probability, the Gaussian, and the bell-shaped curve and is describable with but two figures. Further, these two figures, the arithmetic average and the standard deviation, are subject to mathematical manipulation. This paper demonstrates that, in some cases in the Dominguez field of Southern California, if sufficient core-analysis samples are taken over not too great a thickness of sediments, the resultant permeability and porosity assemblages give satisfactory agreement with ilormal curves. It is shown that the indications are strong that oil wells wherein a satisfactory agreement is found are predictable as to productivity. Since the predictions are made by employing the laws of chance that are operative within sedimentation, it follows that the mechanism by which the predictions were made is a basic concept of reservoir mechanics. Therefore, tentative examples are given of the application of normal curves to the solution of problems of primary and secondary recovery. Nature of Permeability Frequency Distributions Core-analysis data are made available as a tabulated depth vs. permeability profile. The nature of the distribution of permeability values within a given strati-graphic interval may be approximated from an array constructed with samples plotted in the order of their appearance with depth (accession number) against their permeability value in millidarcys. A wide variation in the nature of the distribution of K (permeability) values for

Jan 1, 1944

By Jan Law

Problems of oil recovery are attacked from the approaches dictated by the two strikingly dissimilar complexes that comprise an oil reservoir—the fluid complex and the interstitial complex. Knowledge of the fluid complex, due to labors in the fields of fluid mechanics and physical chemistry, has far outdistanced knowledge of the interstitial characteristics of the sand complex. This paper is concerned with the latter and applies the technique of statistics to petrographic facts—namely, porosity and permeability—dealing with what might be called petrometry. Statisticians have long worked within the problem of reconstruction of a universe oi variables by means of samples that comprise a small percentage of the universe from which the samples were drawn. Core-analysis data comply with the requisite of random sampling as stipulated by theoretical statistics. A basic concept of statistics employs t.he following substitution: 1. The results of sampling are arranged as a frequency distribution. 2. The observed frequency distribution is compared with a mathematically precise distribution. 3. If a sufficiently good agreement is found between the two, the precise distribution is substituted in all subsequent operations involving characteristics of the sampled material. This mathematically precise distribution is also known as the normal curve, curve of error, the probability, the Gaussian, and the bell-shaped curve and is describable with but two figures. Further, these two figures, the arithmetic average and the standard deviation, are subject to mathematical manipulation. This paper demonstrates that, in some cases in the Dominguez field of Southern California, if sufficient core-analysis samples are taken over not too great a thickness of sediments, the resultant permeability and porosity assemblages give satisfactory agreement with ilormal curves. It is shown that the indications are strong that oil wells wherein a satisfactory agreement is found are predictable as to productivity. Since the predictions are made by employing the laws of chance that are operative within sedimentation, it follows that the mechanism by which the predictions were made is a basic concept of reservoir mechanics. Therefore, tentative examples are given of the application of normal curves to the solution of problems of primary and secondary recovery. Nature of Permeability Frequency Distributions Core-analysis data are made available as a tabulated depth vs. permeability profile. The nature of the distribution of permeability values within a given strati-graphic interval may be approximated from an array constructed with samples plotted in the order of their appearance with depth (accession number) against their permeability value in millidarcys. A wide variation in the nature of the distribution of K (permeability) values for

Jan 1, 1944

By A. B. Parsons

When the Seeley W. Mudd Memorial Fund was established in. 1929 the donors mentioned certain types of projects to which preference might be given in selecting those to he financed by the income from the Fund. One suggestion. was that the projects "be of particular benefit to young engineers." This modest little book meets this specification most aptly. It seeks to guide the engineer-particularly the young one-with the least loss of time and effort to the most convenient source of authentic information regarding any topic in which he may at the moment be interested. Knowing the best place to find the literature on a subject is almost as valuable-and far more practicable-than maintaining a library of one's own large enough to provide the information.

Jan 1, 1933

In accordance with the provision of the Constitution, notice is here given to all Members, Associates and Junior Members, that the dues of the year 1917 will be payable on Jan. 1, 1917, at the office of the Secretary. The dues for Members and Associates are $12 per year and the sum of $3 additional is asked of those Members and Associates who desire to have the three volumes bound in the Institute's standard half morocco binding. The dues of Junior Members are $5 per year. Volume 54 of the Transactions is now printed, and will he sent in January to all members whose dues for the year 1917 are paid.

Jan 12, 1916

By H. D. Kessler, R. J. Van Thyne

Phase diagrams of the titanium-rich portion of the ternary systems from 0 to 10 wt pct Al and 0 to 1 wt pct 0, N, and C were determined. Micrographic analysis of annealed high purity arc melted alloys was the principal method of investigation and was supplemented by X-ray diffraction. TITANIUM-ALUMINUM alloys exhibit excellent properties, particularly for elevated temperature use. For this reason, the Materials Laboratory, Wright Air Development Center, sponsored an investigation of the effect of the interstitially soluble contaminants, oxygen! nitrogen, and carbon, on the Ti-A1 system. Using high purity arc melted alloys and micrographic analysis of annealed samples as the chief method of investigation, titanium-rich partial phase diagrams were determined for the ternary systems. Experimental Procedure Materials: The titanium used in the preparation of the alloys was iodide crystal bar (99.9+ pct pure) produced by the New Jersey Zinc Co. and Foote Mineral Co. The aluminum was obtained from the Aluminum Co. of America in the form of sheet. The given analysis was: Si, 0.0006 pct; Fe, 0.0005; Cu, 0.0022; Mg, 0.0003; Ca, <0.0006; Na, <0.0005; and Al, 99.99. High purity titanium dioxide purchased from the National Lead Co. was used in the preparation of the oxygen-bearing alloys. The spectrographic analysis of this material was as follows: SiO,, 0.07 pct; Fe,O,,, 0.002; A1,0,, <0.001; Sb,O,, <0.002; SnO,,, <0.001; Mg, <::0.001; Cb, <0.01; Cu, 0.0004; Pb, 0.002; Mn, <0.00005; W, <0.01; V, <0.002; Cr, <0.002; Ni, <0.001; and Mo, <0.002. Special spectroscopic graphite rod purchased from the National Carbon Co. was used in the preparation of the Ti-A1-C alloys. Alloy Preparation: Alloy ingots weighing 10 grams were melted in a nonconsumable tungsten electrode arc melting furnace using water-cooled copper hearths and a helium atmosphere. The arc was struck on a tungsten stud in the copper block to minimize contamination from the electrode. Details of the techniques have been reported.&apos;, &apos; Each ingot was inverted and remelted a minimum of four times to insure homogeneity, without opening the furnace. Remelting small control ingots of iodide titanium under similar conditions resulted in no measurable hardness increase, indicating contamination-free melting conditions were used. The alloy charges and resultant ingots were weighed to the nearest milligram. Only small weight losses were obtained upon melting, indicating that the actual compositions were very close to the nominal compositions. Check analyses substantiated this. Oxygen and nitrogen were added during ingot preparation as master alloys. An oxygen master alloy containing 25 wt pct 0 was prepared by melting iodide titanium and pressed titanium dioxide (40 pct 0) powder. The Ti-25 pct 0 alloy is more easily handled during weighing and charging than the pressed TiO, powder. Chemical analysis indicated that titanium-nitride received from an outside source contained large amounts of impurities (2.7 pct Ca). Therefore, a master alloy containing approximately 12 pct N was prepared by melting nitrided sponge titanium. As the sponge melted with difficulty, the alloy was diluted by addition of titanium to lower the melting point. The chemical analysis of the final alloy was 6.69 pct N. Both master alloys are friable and were used as —8 +16 mesh lumps resulting from crushing the ingots. NIelting the Ti-A1-0 and Ti-A1-N compositions five times produced homogeneous ingots. The preparation of homogeneous carbon-bearing alloys caused considerable difficulty. Alloys containing less than 1 pct C were prepared using spectrographic graphite rod, 1/8 in. diameter by 1/8 in. long. However, the graphite did not dissolve even with long melting times and many remelts. The ?/s in. pieces of graphite were used rather than powder because the low density powder is troublesome in arc melting.

Jan 1, 1955

By James J. Bean

Although determining and controlling specific gravity of operating medium in a heavy-media plant manually presents no problem, there are advantages to automatic recording and control. The two installations discussed employ the usual method of measurement. Pneumatic control with band control and reset features is used to regulate dilution water and hence specific gravity. Difficulties have been mechanical in nature and associated with obtaining a proper sample and maintaining tight air connections in bubble-tube piping.

Jan 3, 1950

By Howard B. Bradley, Charles F. Weinaug

The phase behavior of a naturally occurring hydrocarbon system whose critical temperature is near the reservoir temperature has been described. The same volume per cent liquid was observed for the firkt time at three different pressures for isotherms immediately below the critical temperature. The shapes of the isothermal equilibrium constant curves necessary to predict this phenomena are discussed and illustrated. INTRODUCTION The phase behavior of a number of hydrocarbon systems has been reported; however, very little data are available on natural occurring hydrocarbon systems whose critical temperature is near the reservoir temperature. This appeared to be the case for the fluid studied here; therefore the pressure-volume-temperature data for this system were determined for preqentation. METHOD The PVT data were obtained with equipment similar to hat described by Weinaug and Katz,1 consisting principally of a two-section, double-windowed gauge mounted in a conktant temperature air bath. The procedure followed was essentially that used by Katz and Kurata5 except that a cathetom-eter, reading direct to 0.01 cm, was used to determine the height of each extreme phase limit. The system studied was formed by recombining -.vapor and liquid samples from the first stage separator of the well. Portions of these samples were displaced with mercury into the cell which had previously been filled with mercury. A predetermined amount of the liquid sample was introduced, while an excess of vapor was admitted. The resulting mixture was brought to equilibrium at the condition of the separator during sampling. By adding mercury to maintain the pressure, enough vapor was displaced to give a gas/oil ratio within the cell equal to that produced by the separator at the time of sampling. The remaining material was then considered to be equivalent to the reservoir fluid. An analysis of material in the cell, computed from analysis of vapor and liquid samples and the separator gas/oil ratio. is given in Table I. Table I — Composition of Hydrocarbon System Component Mole Per Cent Carbon Dioxide 0.13 Nitrogen 0.76 Methane 53.91 Ethane 14.20 Propane 9.64 Iso Butane 1.25 Normal Butane 4.29 Iso Pentane 1.12 Normal Pentane 1.87 Hexane 2.72 Heptanes + 10.11 hloleculal. Weight of Heptanes + 178.50

Jan 1, 1951

By Howard B. Bradley, Charles F. Weinaug

The phase behavior of a naturally occurring hydrocarbon system whose critical temperature is near the reservoir temperature has been described. The same volume per cent liquid was observed for the firkt time at three different pressures for isotherms immediately below the critical temperature. The shapes of the isothermal equilibrium constant curves necessary to predict this phenomena are discussed and illustrated. INTRODUCTION The phase behavior of a number of hydrocarbon systems has been reported; however, very little data are available on natural occurring hydrocarbon systems whose critical temperature is near the reservoir temperature. This appeared to be the case for the fluid studied here; therefore the pressure-volume-temperature data for this system were determined for preqentation. METHOD The PVT data were obtained with equipment similar to hat described by Weinaug and Katz,1 consisting principally of a two-section, double-windowed gauge mounted in a conktant temperature air bath. The procedure followed was essentially that used by Katz and Kurata5 except that a cathetom-eter, reading direct to 0.01 cm, was used to determine the height of each extreme phase limit. The system studied was formed by recombining -.vapor and liquid samples from the first stage separator of the well. Portions of these samples were displaced with mercury into the cell which had previously been filled with mercury. A predetermined amount of the liquid sample was introduced, while an excess of vapor was admitted. The resulting mixture was brought to equilibrium at the condition of the separator during sampling. By adding mercury to maintain the pressure, enough vapor was displaced to give a gas/oil ratio within the cell equal to that produced by the separator at the time of sampling. The remaining material was then considered to be equivalent to the reservoir fluid. An analysis of material in the cell, computed from analysis of vapor and liquid samples and the separator gas/oil ratio. is given in Table I. Table I — Composition of Hydrocarbon System Component Mole Per Cent Carbon Dioxide 0.13 Nitrogen 0.76 Methane 53.91 Ethane 14.20 Propane 9.64 Iso Butane 1.25 Normal Butane 4.29 Iso Pentane 1.12 Normal Pentane 1.87 Hexane 2.72 Heptanes + 10.11 hloleculal. Weight of Heptanes + 178.50

Jan 1, 1951

By Lawrence H. Van Vlack, Otto K. Riegger, Gerald I. Madden

The microstructural variations of periclase (MgO) in the presence of oxide liquids are examined under the steelmaking variables of: 1) temperature, 2) liquid composition, and 3) FeO additions under different oxidation levels. Attention is given to the distribution of the phases, both liquid and solid, and to the growth of individual crystalline grains. Silicate liquids penetrate more extensively between individual periclase grains than do liquids containing high percentages of Fe2O3 Higher MgO solubilities in the liquid and lower MgO contents of the solid favor more rapid grain growth. The presence of a second solid phase reduces the periclase grain growth rate and increases the amount of the solid-to-solid contact within the oxide microstructures at high temperatures. The service suitability of a refractory depends on many factors. Two are of major importance and include 1) the thermal resistance to melting, and 2) the mechanical resistance to loads at service temperatures. Neither is a simple consequence of the service temperatures because service conditions will alter compositions, produce partial melting, and induee phase changes. Consequently, the equilibrium phase relationships have been rather thoroughly studied and give a knowledge of the thermal resistance to melting, but do not give full information about the mechanical properties because two refractories with the same types and quantities of phase may have different microstructures. Although variations of microstructures with time, temperature, and composition have been subjects for extensive investigation in metals, only a limited amount of comparable microstructural work has been performed for refractory materials.&apos; This study was an attempt to evaluate some of the consequences of service parameters upon the microstructures of refractories so that bases may be established for the analyzing of high temperature mechanical properties. Periclase (MgO) was chosen as the refractory oxide; variables included those which are encountered under steelmaking conditions such as 1) temperature, 2) liquid composition, and 3) FeO additions under various oxidation levels. Specific attention was given to the distribution of the phases, both liquid and solid, and to the growth of individual crystalline grains. The most closely related work on microstructures of polyphase materials is that of Van Vlack and Rieg-ger2 on the microstructure of magnesiowüstite [(Mg,Fe)O] in the presence of silica. In that work which pertained to solid solutions with less than 40 pct MgO, most of the quantitative work was performed on FeO microstructures. The chief conclusions concerning these relatively low-melting oxide solids were as follows: 1) the rate of crystalline grain growth is inversely proportional to the grain diameter, 2) grain growth proceeds more rapidly at higher temperatures but is slightly retarded by additional liquid content, and 3) a Silicate-containing liquid penetrates as a film between the individual magnesiowüstite grains independent of time, temperature, amount of liquid, or the MgO/ FeO ratio. The above observations are in contrast to prior work3 on the microstructure of silica in the presence of iron oxide-containing liquids where the liquid does not penetrate as a complete film between solid grains. The phase relationships for the compositions of the present work are shown in Fig. 1 which is a summary of the work of several investigators.4 Of importance is the fact that CaO forms a more stable structure with SiO2 and Al2O3 than do either MgO or FeO. The oxygen potential has little effect on periclase unless iron oxide is also present. The iron oxide is ferrous at moderately low oxygen levels, changing to ferric as the Oxygen potential is increased so the spinels, magnetite, and magesioferrite are formed.5 These two phases are relatively stable in air at steelmaking temperatures. I) EXPERIMENTAL PROCEDURE ractory were made with reagent grade Oxides. The magnesium oxide used was 99 pct MgO after ignition, and the iron oxide raw material had a minimum content of 99 pet Fe2O3. The CaO, SiO2, and A12O3 were also reagent grade raw materials. After mixing, the required compositions were pressed into pellets at a minimum pressure of 5000 psi to insure compaction of the raw materials and prevent excess void content. A silicon carbide element tube furnace was used with thermocouple control for sin-

Jan 1, 1963

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,&apos; 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 Dr. T

THE application of electricity in the extraction of metals has hithcrto been chiefly confined to the electrolysis of dissolved or fused compounds of these by varios methods. The power of electric currents to generate intense heat in their passage through a resisting medium has, however, long been known, and the late W. Siemens thereby succeeded in fusing considerable quantities of steel. But it was reserved to Messrs. Eugene 11. and Alfred H. CoWles, of Cleveland, Ohio, to take a new step in the metallurgic art by maKing the heat thus produced a means of reducing in the presence of carbon the oxides not only of the alkaline metals, but of calcium, magnesium, manganese, aluminium, silicon, and boron, with an ease that permits the production of these elements and their alloys with copper and other metals 011 a commercial scale. In the apparatus devised and now employed by the Messrs. Cowles, a column of fragments of well-calcined charcoal, so prepared and arranged as to present the requisite electrical resistance, is imbedded horizontally in finely pulverized charcoal, and covered by a layer of the same material coarsely broken, the whole being arranged in a box of fire-brick, covered with perforated tiles and opened at the ends to admit two carbon electrodes an inch and a half in diameter.

Jan 1, 1886

Before hostilities between the colonies and Great Britain began in 1775, most of the coal used in the northern colonies undoubtedly came from England, with some supplies for New England coming from Nova Scotia; in New York and Philadelphia the supply came from England with some from the Virginia mines. Table 4 shows data obtained from the Public Records Office, London, for the years 1768-1772. This table supplements Table 3, which records only a few shipments from Richmond in 1768 and 1769; as there was no coal shown in imports coastwise in 1769 in Table 4, and only two small shipments in 1769 in Table 3, there may have been a cessation of shipments then, for some reason not now known. In Table 5 are incorporated all the data in the first two, with a few earlier years, and an attempt is made to estimate the amount used during the period by allowing for coal exported. With the small total tonnages a carryover from one year to another makes a large difference in the annual figures, but over the period the result may be fairly indicative of the amount of coal used before the Revolution. According to present day ideas the quantity of coal used during that war was very small, but apparently it was badly needed for the manufacture of the small amount of munitions made in those troublous days. As Philadelphia was the leading city along the Atlantic coast, and as the southeastern part of Pennsylvania was the leader in making iron, as well as making rifles, it is natural that the first call for coal came from there. At first, procuring supplies such as coal, powder and sulphur was handled by a Committee of Safety, which later became a Council of Safety and later this committee&apos;s functions were turned over to a Board of War, functioning with the military organization of the colony. . The organizations of the several colonies were slightly different, but Pennsylvania, Maryland and Virginia followed this scheme generally. Later in the war the Congress began to make arms for the troops, and it is difficult now, with the few records available, to tell when the state functions ceased and those of Congress began. On December 5th, 1775, the Committee of Safety

Jan 1, 1942

By E. A. Gulbransen, K. F. Andrew

The gas-metal reactions of zirconium are very interesting. The metal is extremely stable at room temperature to reactions with the several gases present in air and the metal will stay bright indefinitely. However, at temperatures of several hundred degrees higher the metal reacts readily with oxygen, nitrogen and hydrogen. This behavior, in addition to the fact that zirconium is one of the higher melting point metals which might have high temperature applications under the proper conditions, resulted in the work reported in this communication. There are several factors which indicate that zirconium might have good oxidation resistance at elevated temperatures. These are: (1) the high melting point of approximately 1860°C, (2) the high melting point of the oxide of approximately 2675°C, (3) the high degree of thermodynamic stability of the oxide to chemical reaction and the low decomposition pressure of the oxide and (4) the possible formation of a continuous oxide film since the volume ratio of oxide to metal is greater than unity. The unfavorable factors are: (1) the metal reacts to form nitrides, hydrides and carbides, (2) the oxide is soluble at elevated temperatures in the metal and (3) the oxide ZrO2 undergoes crystal structure transformations at high temperature. The oxidation resistance of this metal is not only a question of the rate of film formation but is complicated by the fact that the oxide and other reaction products dissolve in the metal which in turn will affect the physical and mechanical properties of the metal. The protection of the metal to nitride formation must be considered separately from the oxide problem. One unfavorable factor is that the volume ratio of the nitride to the metal is about unity. This indicates that a discontinuous film might be formed. This paper will present measurements on the rates of reaction of the metal with O2, H2 and N2 over a wide temperature and pressure range. The reaction in high vacuum and the stability of the several compounds formed will be presented. The results are correlated with fundamental rate theory and with the physical and chemical structure of the metal and film. Literature Although many papers have been published on the chemical reactions of zirconium with various gases, comparatively few are concerned with the protective nature of the metal and its reactions at normal pressures. The studies in the pressure range below 0.01 mm of Hg gas pressure are largely of interest in the nature of the adsorption of gases by hot filaments in high vacuum apparatus. The reactions of zirconium in this pressure range have been reviewed by Fast8 and by RaynOr.27 In spite of certain differences of opinion as to the maximum adsorption temperatures for various gases, the low pressure range is qualitatively understood. Some of these papers will be mentioned briefly here. 1. LOW PRESSURE Ehrke and Slack&apos; find that oxygen reacts above 885°C and hydrogen above 760°C. Nitrogen does not react up to a temperature of 1527°C. Fast9 on the other hand observes that oxygen is absorbed above 700°C and nitrogen at temperatures exceeding 1000°C. Hydrogen is absorbed from 300" to 400°C and liberated between 500" and 800°C. It is readsorbed at 862°C and released above 862°C. Hukagawa and Nambo22 find a rather complicated picture for the absorption of oxygen. A rapid initial absorption is found between 180" to 230°C. Further oxygen is not taken up until a temperature of 450°C is reached. The optimum temperature for complete absorption is 650" to 700°C. Nitrogen is found to be completely adsorbed at 600°C. However some of the gas is evolved at higher temperatures. Their data on the absorption of hydrogen indicate some of the gas is removed at 550°C. Guldner and Wooten17 in a study of the low pressure reactions of zirconium with various gases observed that the reaction with oxygen occurs at temperatures above 400°C and that the oxide is formed. The reactions with carbon monoxide and carbon dioxide occur rapidly at temperatures of about 800°C with the oxide and carbide being formed. Zirconium reacts at temperatures of 400°C slowly and at 800°C rapidly to form the nitride and with hydrogen and water at 300°C to form the hydride and a mixture of the oxide and hydride respectively. 2. NORMAL PRESSURE DeBoer and Fast3 in a study of the electrolysis of oxygen in zirconium find that the metal absorbs up to 40 at. pct of oxygen without forming a new phase. The solubility of nitrogen in the lattice has been studied by de Boer and Fast4 and Fast10 and is found to be considerable. At higher temperatures the oxide dissolves in the lattice at an appreciable rate according to Fast10 and the zirconium surface becomes active. De Boer and Fast4 and Hägg18 have studied the solubility of hydrogen and find that at room temperature the solubility corresponds to ZrH1.95 Desorption occurs on lowering the pressure. Hydrogen is stated to be more soluble in the ß-form and the

Jan 1, 1950

By J. E. Howard

On Aug. 25, 1911, a rail failed on the Lehigh Valley Railroad, causing a disastrous wreck. The surface of the fracture was in a plane at right angles to the length of the rail. There was a dark-colored, oval spot on this surface, located on the gage side of the head, representing the part of the rail which was the first to fracture. The nucleus of this spot showed that the fracture had an interior origin. Other fractures of this kind, the peripheries of which had not reached the surface of the rail, presented surfaces having a (silvery luster. The darkened surface of the present fracture was caused, doubtless, by the air having had access to it. This fracture was recognized as a fatigue fracture, of a modified type, its interior origin having been due to a component in the rail which is not usually present in cases of fatigue fractures. The metal next the running surface of the head of the rail was in a state of internal compression, this being the component not commonly met with in other cases, and which caused the fracture to have its interior origin. For the purpose of giving this modified type of fatigue fracture a specific name, for identification, the term "transverse fissure" was applied. No mystery was thought to attach to its formation, or to its development. The explanation of its occurrence seemed obvious in the light of common knowledge upon the behavior of steel under repeated alternate stresses.&apos; By reason of the state of internal compression at the running surface, the maximum tensile stresses in the head, ander bending loads, were along an interior element. Here the tensile strains were higher than in the fibers more remote from the neutral axis. Under such conditions the fracture of the rail would be expected to have an interior origin. A discussion of the subject of transverse fissures essentially becomes a discussion of fatigue fractures, since they are believed to be identical. The descriptive term employed, merely for the identification of this type of fatigue fracture, had the appearance of creating alarm. Apprehensions arose that a new phenomenon in the physical properties of steel had presented itself, the explanation of which was sought in every

Jan 1, 1918