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By A. R. Calawa, T. C. Harman, M. Finn, P. Youtz

A study has been made of the growing, annealing, and diffusion parameters in PbSe, Pb1-ySnySe, and Pb1-xSnxTe. Single crystals of these materials have been grown using the Bridgman technique. For all of the above materials the as-grown crystals are p type with high carrier densities. To reduce the carrier concentration and increase the carrier mobility, the samples are annealed either isothermally or by a two-zone method. From isothermal anneals, the liquidus-solidus boundary on the metal-rich side of the stoichiometric composition has been obtained for some alloys of Pb1-xSnxTe and on both the metal- and seleniunz-rich sides for PbSe and alloys of Pbl-ySnySe. In Pbo.935 Sno.065 Se carrier concentrations as low as 5 x1016 Cm-3 and mobilities as high as 44,000 sq cm v-1 sec-1 at 77°K have been obtained. Inter diffusion parameters mere also studied. The ddiffusion experiments mere identical to the isothermal or two-zone annealing experiments except that the samples were removed prior to complete equilibration. The resulting p-n junction depths were determined by sectioning and thermal probing. Inter diffusion coefficients for various temperatures were calculated for both PbSe and Pb0.93Sn0.0,Se. RECENTLY, there has been considerable interest in the PbTe-SnTe and PbSe-SnSe alloys with the rock salt crystal structure. The unusual feature of these systems is the variation of energy gap EG with composition. Several investigations1-3 have shown that EG for the lead chalcogenides decreases as the tin content increases, goes through zero, and then increases again with further increase in tin content. The possibility of obtaining an arbitrary energy gap by selecting the composition is an especially attractive feature of these alloys for applications involving long-wavelength infrared detectors and lasers. In addition, some unusual magneto-optical, galvanomagnetic, and thermomag-netic effects should occur for alloys with low band gaps. If uncompensated low carrier density crystals can be obtained, then a small carrier effective mass, a large dielectric constant, and the resultant high carrier mobility should yield enormous effects at low temperature in a magnetic field. The relative variation of the energy gap with pressure should also be very large for these low gap materials. The primary purpose of this paper is to provide some information concerning the preparation of low carrier concentra- tion, high carrier mobility, and homogeneous single crystals with a predetermined alloy composition. I) DETERMINATION OF ALLOY COMPOSITIONS In all of the work described in this paper, the composition of lead and tin chalcogenides in the alloys was determined by electron microprobe analysis. Separate X-ray spectrometers are used to make simultaneous intensity measurements of the Pb La1 and Sn La1 lines emitted by the sample under excitation by a beam of 25 kev electrons focused to a spot about 2 µm in diam. These intensities are compared to the intensities of the same lines emitted by standards under the same conditions. The standards used are the terminal compounds of each pseudobinary system, i.e., PbTe and SnTe for Pbl-xSnxTe alloys, PbSe and SnSe for Pbl-ySnySe alloys. The composition of the sample is then obtained from theoretical calibration curves which relate the weight fractions of lead and tin in the alloy to the measured ratios of X-ray intensities for the sample and the standards. The lead and tin calibration curves for each alloy system were calculated by using corrections for backscattered electrons,4 ionization,5 and absorption,6 and assuming that the atom fraction of tellurium or selenium in the sample and standards is exactly +. Results obtained by using the microprobe are in good agreement with those obtained by wet chemical analysis. II) CRYSTAL GROWTH FROM THE VAPOR Early work on the vapor growth of PbSe was carried out by Prior.7 He used small chips of Bridgman-grown single crystals as the source material and frequently converted the whole charge of a few grams into one crystal. In the present work, vapor growth occurred using a metal-rich or chalcogenide-rich two-phased alloy powder as the source material. Small, nearly stoichiometric crystals are formed on the walls of the quartz tube. The procedure will now be described in detail. Initially, a 100-g charge containing (metal)o.51(chalco-genide)o 49 proportions or (metal)o.49(chalcogenide)o. 51 proportions of the as-received elements in chunk form are placed in a fused silica ampoule. After the ampoule is loaded, it is evacuated with a diffusion pump and sealed. The sealed ampoule is placed in the center of a vertical resistance furnace. The region containing the ampoule is heated to about 50°C above the liquidus temper-ature for the particular composition used. After about one-half hour at temperature, the elements are reacted and the molten material homogenized. The ampoule is quenched in water. The quenched ingot is crushed to a coarse powder for vapor growth experiments and to a fine powder for the isothermal annealing experiments which are discussed in a later section. Vapor growth experiments were carried out using the powdered, metal-rich or chalcogenide-rich alloys

Jan 1, 1969

By R. K. Dann, L. W. Roberts, R. B. Benson

The mechanical properties of 300-series stainless steels were investigated in both high-pressure hydrogen and helium environments at ambient temperatures. An auslenitic steel which is unstable with respect to formation of strain-induced a (bee) and € (hcp) mar-tensile is embrittled when plastically strained in a hydrogen environment. A stable austenitic steel is not embriltled when tested under the same conditions. The presence of hydrogen causes embrittlement at the mar-lensitic structure and a definite change in the general fracture mode from a ductile to a quasicleavage type. The embrittled martensitic facets are surrounded by a more ductile type fracture which suggests that the presence of hydrogen initiates microcracks at the martensitic structure. If a steel is unstable with respecl to fortnation of strain induced martensile, plastic deformation in a hydrogen environment will produce rapid embrittlement of a notched specimen in comparison to an unnotched one. FERRITIC and martensitic steels can be embrittled by hydrogen that has been introduced into the alloys, either by thermal or cathodic charging prior to testing.1-5 However, conflicting reports exist as to whether austenitic steels that are stable or unstable with respect to formation of strain-induced martensite can be embrittled by hydrogen.8-12 A recent investigation has shown that cathodically-charged thin foils of a stable austenitic steel can be embrittled.13 An earlier investigation of a thermally charged 18-10 stainless steel revealed a significant decrease in the ductility only at the lowest test temperature of -78°C, although strain-induced bee martensite was shown to be present in one specimen tested at ambient temperatures.' When martensitic steels are tested in a hydrogen atmosphere, they are embrittled.'4-'7 It has been observed in this Laboratory that 304L steel, which is unstable with respect to formation of strain induced martensite, forms surface cracks when plastically strained in a high-pressure hydrogen environment. Work in progress elsewhere concurrent with this investigation has also established that 304L is embrittled when tested in a high-pressure hydrogen atmosphere." The objective of this investigation was to study the effect of a high-pressure hydrogen environment on the tensile properties of a stainless steel that contained strain-induced martensite (304L) and one that did not (310). EXPERIMENTAL TECHNIQUES Notched and unnotched cylindrical specimens were machined from 304L* and 310 rods that were heat- treated at 1000°C in argon for 1 hr followed by a water quench. The chemical analyses of these steels are given in Table I. The unnotched specimens had a reduced section diameter of 0.184 & 0.001 in., a gage length of 0.7 in., and were threaded with a 0.5-in.-diam. thread on each end. The notched specimens had a reduced section diameter of 0.260 * 0.001 in. and a 0.75-in. gage length, with a 30 pct 60 deg v-notch at the center. The notch had a maximum root radius of 0.002 in. The tensile bars were fractured in a hydrogen or helium atmosphere of 104 psi at ambient temperatures. The system used for mechanically testing the specimens is to be described in detail elsewhere.19 Several specimens of each type were tested in air using an Instron testing machine. The same yield strength and ultimate tensile strength were obtained in 104 psi helium with the above system as with the conventional testing machine. Magnetic analysis was employed to determine that there was a (bee) martensite in plastically deformed 304L and that it was not present in plastically deformed 310. The magnetic technique depended on allowing the material being studied to serve as the core between a primary and secondary coil. Thus, any change in the amount of magnetic material present between the annealed and plastically deformed steels will be indicated by corresponding changes in the induced voltage in the secondary circuit." The ratio of the output signal of a nonmagnetic stainless steel to a completely magnetic maraging steel was 2000 to I. Several unnotched 304L bars tested in hydrogen were analyzed for hydrogen by vacuum fusion analysis. There was an increase in the hydrogen content to approximately 2 ppm for the specimens tested in hydrogen, as compared to less than 1 ppm for the as-received material. Several thin sections cut from notched areas of 304L specimens tested in hydrogen and containing the fracture surface contained approximately 1.5 ppm H. The accuracy of these determinations was estimated to be ± 50 pct.

Jan 1, 1969

By R. E. Cech, J. H. Hollomon

KURDJUMOV and Maksimova reported experiments with manganese steels and high carbon steels' and with an Fe-Ni-Mn alloy' in which mar-tensite was formed isothermally over a range of temperatures. They found in some cases that mar-tensite formation could be suppressed by rapid quenching to liquid nitrogen temperature. From their microstructural observations of martensite formed isothermally, they concluded that the rate controlling step is nucleation rather than growth. Kulin and Cohen,3 in an attempt to reproduce these experiments, found that with a steel having the same composition as that reported by Kurd-jumov and Maksimova, the transformation to martensite was essentially complete above the temperature range of Kurdjumov and Maksimova's isotherms. The possible reasons for this disagreement were not considered. Recent papers by Das Gupta and Lement4 and Kulin and Speich5 report the formation of isothermal martensite in a high chromium steel and in an Fe-Cr-Ni alloy, but neither paper can be considered a verification of the original Kurdjumov and Maksimova results. Further, in neither case were the authors able to suppress the formation of martensite entirely. Because of the important bearing the Kurdjumov and Maksimova results have to an understanding of the mechanism of martensite reactions it was felt that an experimental investigation directly concerned with checking the validity of their results was in order. This paper describes the results obtained on the isothermal transformation over the temperature range from —79" to —196°C of an alloy of iron, nickel, and manganese. Experimental Apparatus A 15 lb heat of an alloy containing 73.3 pct Fe, 23.0 pct Ni, and 3.7 pct Mn was melted by induction and cast under argon. The ingot was forged to 1-in. bar and a portion rolled to 1/16x1 1/2-in. strip. This strip was pack-homogenized 300 hr at 1100" in a helium-filled sealed iron tube. The composition after homogenization was 73.2 pct Fe, 22.94 pct Ni, 3.73 pct Mn, 0.05 pct C, and 0.015 pct N. The strips were cut to 1/2-in. width for dilatometer and metal-lographic specimens. Only the center portion of the 11/2-in. strip was used in the present investigation. The dilatometer employed was similar in design to one described by Flinn, Cook, and Fellows." A concentric fused auartz rod and tube assembly with hooks for holding the specimen was mounted so as to transmit the specimen dilation to a 1/10,000 in., 1/10 in. travel dial gage. The dilatometer proper was mounted by means of extension arms to a counterweighted sliding member on a vertical standard. This method of mounting permitted rapid transfer of the dilatometer from the austenitizing furnace to the quenching bath and low temperature chamber. A small electrical vibrator on the dilatometer kept frictional effects of the quartz members at a minimum. The austenitizing unit was a vertical, molybdenum-wound, hydrogen atmosphere furnace maintained at a constant temperature ±3°C by means of constant power input. A 12-in. stainless steel jacketed copper liner having 1/2-in wall thickness acted to equalize the temperature in the hot zone of the furnace. This liner, closed at the bottom end and open at the top to permit entrance of the dilatometer and specimen, was kept filled with dry nitrogen gas. A chromel-alumel thermocouple was placed inside the tube to determine the temperature. The 4-in. dilatometer specimens in the chamber varied less than 1/2° across the specimen length except for a 1 1/20 drop at the end nearest the open end of the furnace. The low temperature isothermal holding bath was a double Dewar arrangement similar to one described by Turnbull7. The outer bath was filled with a refrigerant at a temperature lower than the desired holding temperature. The inner bath was filled with Freon "11" or "12" or a mixture of both, depending upon the holding temperature. This inner bath which tended to be cooled by the outer bath was kept at a constant temperature by introducing a small amount of heat with a manually controlled electric heater. Stirring was accomplished by bubbling dry air through the bath. A Leeds and North-rup type K potentiometer was used to measure the inner bath temperature as indicated by a five element copper-constantan thermopile. The bath temperature was maintained within ±0.2°C of the desired temperature by occasionally adjusting the heater current so as to keep the Leeds and Northrup galvanometer at zero deflection with a constant setting of the potentiometer. Isothermal tests were usually continued for 300 to 400 min and another reading made at approximately 1000 min if the bath, unattended overnight, had not deviated in temperature more than 5°C. Transformation curves are drawn dashed (Fig. 1) through the time region where temperature was not controlled precisely. Experimental Procedure Dilatometer specimens of 1/2x1/16-in. strip were cut to 41/2-in. length and holes were drilled for the quartz hooks with proper spacing to give a 4-in. measured length. A thermocouple consisting of 0.012-in. diameter chrome1 and alumel wires was spot welded to the specimen and threaded between the dilatometer rods to binding posts near the dial

Jan 1, 1954

By R. B. Burt, James A. Barr, I. S. Tillotson

THE pumping of solids in water suspension is an important part of many metallurgical and mining operations. In most cases, it is still in the rule of thumb category for which no universal formula has been developed, and much research is needed. Because of the limited and incomplete data available, this article may be classed as an experience paper, which is presented with the hope that some contribution will be made toward the development of the so-called universal formula. This formula, if and when developed, may be evolved from several factors, many of which are not now available for general application. The designing engineer is interested in obtaining accurate forecasts on: 1-the minimum velocities needed to prevent choke-ups in the pipeline, which in turn dictates pipe sizes, 2-power required for pumping, 3-pump selection. The basic factors for a given problem will include: 1-weight per unit of time of solids to be handled, 2-specific gravity of solids, for calculation of volume, friction and power, 3-screen analysis of solids with the colloidal acting, i.e., the slime fraction, a very important factor, 4-shape of particle or some means of determining a friction constant, 5-effects of percentage of solids, 6-development of a viscosity factor to be used in the overall calculations, 7-calculation of the lower limits of pipeline velocities permissible, 8-calculation of total head, pump horsepower, and 9-setting up of pump specifications. In certain limited cases horsepower and total heads and minimum velocities may be computed and a suitable pump selected from basic data, but in many cases, as in mining of Florida pebble, phosphate, experience rather than a hydraulic formula still should be used as a basis of selection. Pumping Florida Pebble Matrix Pumping at the Noralyn mine of International Minerals and Chemical Corp. will be used as an example. Other areas will vary as to the characteristics of the matrix, especially the slime content. A typical screen analysis of this matrix is: +14 mesh, pebble size,* 2.1 pct; -14 +35 mesh, 11.4 pct; -35 +150 mesh, 60.5 pct; -150 mesh, 25.0; total, 100 pct; moisture in bank, 20.0 pct; weight per cu ft in bank, 120 lb. The -150 mesh fraction may increase to as much as 35 pct in adjacent areas. When thoroughly elutriated, the matrix has a relatively slow settling rate, which is an important factor in permitting lower pipeline velocities without choke-ups. Exact data is not available to evaluate settling rates. For a factor of 100 a suspension of clean building sand in water is suggested. When pumping long distances, a quick settling matrix allows the coarser solids to settle out along the bottom of the pipeline, causing drag, turbulence, and increased friction. With a slow settling matrix as at Noralyn, turbulence acts to keep the solids in suspension at a lower friction head, regardless of the pumping distance. When the pebble, content of the matrix, i.e., the +14 mesh fraction, is in excess of 10 pct of the total solids, trouble may be expected from settling out even in normal pumping distances. To prevent choke-ups and maintain tonnage, an additional pump must be added in the long runs, where one pump would otherwise be satisfactory. A typical pulp handled is: total volume, 7800 gpm; water, 4500; solids pumped per hr, 4200 lb; sp gr pulp, 1.4; percent solids in pulp, 46.; pipe size, 16-in. ID; pulp velocity, 12.85 fps; probable critical velocity, 10 fps, as below this minimum -velocity choke-ups would be numerous. In calculating friction heads the Armco handbook is used where a roughness factor based on 15-year-old pipe is set up. Because the pipe used in pumping matrix is, smooth and- polished because of the scouring, action of the phosphate and its silica content, the head losses in the Armco table for water are practically the same as in pumping the Noralyn matrix through smooth pipe, plus the fact that conditions vary widely over short periods, making accurate determinations difficult to obtain. New pumps and pump, changes are being tested continuously and a wealth of data built up. This has resulted in a substantial improvement and lower relative costs in pumping matrix. The Florida phosphate industry is constantly seeking to offset higher wage and material costs with improved technique. Until a few years ago a 12-in. discharge pump was commonly used, with heads as low as 80 ft. Sizes have gradually increased and heads more than doubled. For example, the following pump was placed under test at the Noralyn mine: make, Georgia Iron Works; size, suction 16 in., discharge 14 in.; impeller, 39-in. diam; motor, 600 hp, slip ring; full load speed, 514 rpm. The results were increased head, higher capacity than the older design, with fewer pumps in the line from mine to washer.

Jan 1, 1952

By J. E. Johnson

Discussion of the paper of Mark A. Amnion, presented at the Cleveland meeting October, 1913, and printed in Bulletin No. 70, October, 1913, pp. 1167 to 1 79. J. E. JOHNSON, JR., Ashland, Wis.:-Mr. Amnion's paper is of great value and it is not with any desire to reflect. on it that I wish to make some comments on the use of the scleroscope. We obtained one on trial some months ago and made very extensive tests with it, but without getting very satisfactory results. The readings on good car-wheels and bad ones were just about the same, but the factor in its use most likely to produce erroneous results is a variation in the thickness of the specimen being tested. In order to find out something on this subject we cut a thin disk, about -1,: in. thick, off a brass rod; then one 0.25 in. thick, and another about 1 in. thick, put the surfaces of all in about the same condition and tested them with the scleroscope. The readings varied widely; the resilience of the anvil evidently entered to a very high degree on thin pieces. By putting a soft cushion between such a thin specimen and the anvil, and forcing it up against the tube, the softness of the cushion cut off the resilience of the anvil and the results were more like those of the thick specimens. After a thickness of 1 in. was passed, the specimen seemed to have mass enough so that the resilience of the anvil no longer played an important part, and above that thickness results on different materials would be comparable, even though the thicknesses differed. But in order to get comparable results on thin specimens the thickness of those being tested should be the same. I should like to ask how the variations introduced in this way were overcome, so as to get strictly comparable results. Mr. AMMON :-.I have not had much experience in that, but the scleroscope is simply an indication of the surface harden-

Dec 1, 1912

By Thomas W. Dawson

The H. C. Frick Coke Co. has used belt conveyers for handling coal for the last eighteen years but, until recently, only for small tonnages and over short distances. The first installations were outside the mines for distributing coal to various parts of plants. A belt conveyer was put in service at Colonial No. 4 Mine in November, 1906, to carry coal from the main hoisting shaft to a storage bin serving two blocks of beehive ovens on the other side of the valley; it was in constant service until the Colonial No. 4 ovens were abandoned less than a year ago. This conveyor was in an overhead gallery that spanned our sidings and yard tracks and the main line of the Pennsylvania Railroad. It was a crude installation, from the viewpoint of present conveyor engineering practice. It had no mechanical feeding device, the coal simply ran through a gate in the side of a bin on to the belt; but one belt on this conveyor lasted eleven years. This conveyor is about 300 ft. long center to center of pulleys. It operated at a speed of 250 ft. 'per min-and carried about 400 tons per day. On this basis, the belt life of eleven years means that not over a million and a quarter tons was carried by the belt. whi1e: this is not a large tonnage, the cost per ton was much less than by any previous method in use for supplying coal to ovens located at a distance from the main shaft. The next belt conveyor was installed at Bridgeport Mine in 1907. It carried about the same daily tonnage as the first, delivering from the hoisting shaft to a coke-oven bin. Very few data were kept on this conveyor. It also operated until the coke ovens at the plant were put out of blast and the coal taken to the Clairton byproduct plant by river. In 1916, work was started to equip the Bridgeport, Palmer, Gates, and Ronco mines to load their entire output on the river for transportation to the Clairton byproduct plant, which was then being built. These mines were all operating at that time and had a large area of coal available for river shipment. The Monongahela Railroad was located between the hoisting shaft and the river at each of these plants and, therefore, had to be crossed at each location to deliver coal to the river. After careful study, it was decided to transport this coal from the hoisting shaft to the river at each of these plants by belt conveyors.

Jan 1, 1925

By Russell Paul

THE Wisconsin zinc district, also known as the Upper Mississippi lead and zinc district, is an area of about 2500 sq. mi. in the southwestern portion of Wisconsin and adjacent parts of Illinois and Iowa. It includes Iowa, Grant and Lafayette counties in Wisconsin, Jo Davies County in Illinois, and an irregular strip of Clayton and Dubuque counties in Iowa, parallel to the Mississippi River. During periods of high metal prices mining has been quite active in this district, but recently the lower metal prices have caused many companies to suspend, so that at the present time there are only a small number of mines operating. The short life of these mines and the low mineral content of the zinc deposits limit the investment in development and equipment, and necessitates the operation of this equipment at maximum running time and maximum capacity. The tonnage of rock handled (locally termed dirt) is large in comparison with the tonnage of concentrate produced. Moreover, the zinc content of the concentrate is low, varying from 25 to 40 per cent zinc, and the value per ton is correspondingly low. The life of the mines varies greatly. An exception-ally good deposit may produce 2,000,000 tons of rock during a period of ten years, market value permitting, from which will be obtained 100,000 to 150,000 tons of concentrate. One property which might be con-sidered as fulfilling the requirements of a profitable operation was developed and equipped in 1925, oper-ated continuously for a period of two and a half years, produced 484,292 tons of rock, from which was obtained 37,659 tons of zinc concentrate, 34.4 per cent Zn, and 1155 tons of lead concentrate, 67 per cent Pb. During the war period prices of ore permitted the mining of lower grade ores than has been possible in the past few years. The maintaining of a higher grade mill-feed has resulted in reducing the size of stopes formerly carried in the old mines and confining the workings within narrower limits.

Jan 7, 1928

By Claudio Guarnaschelli

Alteration of the electronic distribution of mineral surfaces by light irradiation has been used to modify the adsorption characteristics of flotation reagents. Energy of a few electron volts is suficient to cause the necessary transitions that either enhance or retard the adsorption phenomenon. The adsorption characteristics of potassium ethyl xanthate on galena and marmatite are presented as functions of the energy of illumination, type of semiconductor, and surface oxidation. In dilute solutions, the adsorption differences are readily detected by controlled kinetic measurements. The correlation between the electronic distribution and the adsorption and desorption phenomena at the solid surface is gaining more attention and acceptance. These interrelations have found a practical application in mineral processing since all of the sulfide minerals display semiconducting properties. By varying the ratio of free electron to electron vacancies, the separation of ilmenite from rutilel and zircon from pyrochlore" has been executed successfully. Plaksin et al.' indicate three possible ways of utilizing the semiconductor properties of a mineral. The first one involves the control of the oxidation-reduction potential of the liquid phase, the second one consists of allowing selected additives to diffuse through the mineral surface, while the third one entails a change in the adsorption and chemical activity of minerals by irradiating their surface. The aim of the present work is to consider the effect of irradiation on the adsorption-desorption characteristics of natural minerals. Since the effect of irradiation is to change the electronic distribution at the surface:

Jan 1, 1971

By J. S. Hromatko, L. J. Gurevich

In the course of the examination, at the BureLu of Standards, of fusible tin boiler plugs for the Steamboat Inspection Service, it became evident that an investigation should be undcrtaken to determine the precautions necessary in the manufacture of acceptable plugs. The results of the tests of these plugs show that their manufacture has improved, though at present not all of the plugs tested are, satisfactory. Table 1 gives the result of tests of some 1500 plugs from about 100 makers. Records of the tests show that several of the makers were able to produce satisfactory plugs with every pouring. The Steamboat Inspection Service has the following specifications for fusible plugs: "Fusible plugs for use in boilers of steam vessels under the jurisdiction of the Steamboat Inspection Service shall be made of bronze casing with the bore tapering continuously and openly from end to end, and filled from end to end with tin not less than 99.7 per cent. pure and to contain not more than 0.1 per cent. of lead and not more than 0.1 per cent. of zinc. The small end of the bore may be countersunk not more than 1/32 in. in depth and width, but no recess, thread, or cavity other than this countersink shall be allowed." Table 1.—Thirty-"five-mdh Testing Record of Fusible Plugs Causes of Rejection Inspection Period June-November, 1916.................. 311 32.8 47.2 3.8 11.5 15. 1 10.9 1 1.9 4.5 December, 1916-May, 1917............. 318 71.4 28.6 2.2 4.4 12.8 5.9 i ... 2.8 June-November, 1917.................. 228 73.0 27.01 ... 9.6, 5.2 9.6' ... 0.8 December, 1917-May. 1918............. 214 72.028.0 0.9 0.4 11.6 7.0 ... 7.9 June-November, 1918...............250 70.7 29.3 ... 2.0 20.0 5.2 ....2.8 December, 1918-April. 1919............ 23378.121.9 7.2 1.2 1 4.7 3.0 ... 6.0 Total 35 months....................1544.69.7 30.3 2.3 4.8 11 0 6.9 0.3 4.1

Jan 1, 1921

By Erskine Ramsay

The following description of the Alabama coal-,fields is taken (with slight omissions) from the report " On the Warrior CoalField, by Henry McCalley, A.M., C. and M. E., Assistant State Geologist:" The coal lands of Alabama are of the great coal basin of the Ohio, or of the great Appalachian coal-field, and are estimated at 8660 square miles. They formed one connected field prior to the great Appalachian revolution, when there was pushed up through them long, narrow, anticlinal ridges which have been denuded into the present well-known anticlinal valleys, and thus this great field has been divided up into three more or less distinct parts. These parts were named by Prof. Tuomey, in 1849, the Warrior, the Cahaba and the Coosa coal-fields, respectively, from the names of the rivers which drain them. They are of very unequal size, the Warrior, with an area of 7810 square miles, being nearly ten times as large as the other two combined, and about two-thirds as large as the coal-area of Great Britain. This Warrior field is the most northwestern of the three coal-fields of Alabama, and comprises all of the coal-measnres in Alabama, northwest of the Alabama Great Southern railroad, or all of those drained by the Warrior and Tennessee rivers. The greater part of this field, almost all of it away from the present railroad lines, has never received more than a surface-examination. Still, we have in the Warrior coal-field one of the richest coal-basins of this or any other country. As a whole, the Warrior coal-field is a broad, shallow, tray-shaped depression, sloping towards the southwest, and with its southwest end covered by a newer formation and its southeast side, especially, complicated by folds and fractures. As is the case with all of our Coal Measures. it is composed of a series of sandstones. conglomerates, shales, slates and coal-seams, with some little limestone at several horizontal positions, but contains no thick bed of this last rock like the Measures of Pennsylvania and other States. The thickest conglomerates are near the bottom and top of the series, and hence these coals might be said to belong mainly to the

Jan 1, 1891

By Leo J. Vogel, E. D. Hummer

INTRODUCTION by E. D. HUMMER An efficient refuse-disposal system is a necessary part of the modem cleaning plant. The large-scale refuse system and disposal area, engineered for the lifetime of the plant, has become more important due to the greater tonnages of refuse produced from increased quantities of mechanically mined and prepared coal. Laws and increased government regulations have affected the design and operation of disposal systems. THE EFFECT OF MINE AND PLANT OPERATION Refuse disposal starts at the mining face. The mining system, the type of roof support, the machinery used, and the degree of discipline at the face contributes to the amount and type of refuse that must be removed through the disposal system. Economies gained through modification of the mining system or mining machinery may be partially offset by increased dilution of the mined coal with impurities from associated rock formations. In some cases the change in the mining system and equipment has reduced the dilution. In all cases the ratio of impurities that must be removed from the raw-coal feed to the plant not only affects the maintenance and operating costs of the plant, but greatly affects the design of the refuse disposal system. The design of a mine and plant should include the location and the estimated capacity of the disposal areas for the life of the property or plant. Complete evaluation of the disposal system and an estimate of its annual cost of operation over the life of the property or plant should be incorporated in the plant and mine evaluation. Plant design should be as simple as possible, consistent with the efficient production of clean coal. Material transfer points, crushing, screening and pumping operations should be kept to a minimum to reduce degradation and the subsequent increased difficulty and cost of refuse removal. The maintenance of good process control by operating management will result in a minimum of misplaced material in both refuse and clean coal. Reduction of misplaced float material in the plant refuse is an important factor in preventing combustion in the refuse storage pile. THE REFUSE DISPOSAL AREA Combustion in refuse piles occurs when air enters the pile in sufficient quantity to support oxidation. At certain rates of air in-filtration, the heat produced by the oxidation process is not dissipated and temperature rises.

Jan 1, 1968

To the Members It has been, and is the endeavor of the A. I. M. E. to serve each and every member. One of the means of letting the membership know what is going on in the mining; metallurgical and chemical fields, and by far the most important, has been our monthly Bulletin. To publish this costs money, and to partly defray the costs, it was decided to accept such advertising as could be secured. The A. I. M. E. is the only one of the American National engineering societies whose dues are as low as $10 per year, and it actually spends more upon the Bulletin and Transactions than the sun total it receives for clues. Hence the need of advertising revenues. We are planning even greater improvements for your Bulletin-improvements that will help you in your work. It will mean a better publication, with more information than ever before. To successfully carry out our plans, we must have your co-operation. We are not asking you for financial, but for your moral support. With that we shall accomplish a great deal. What we ask of you, brother member, is to give evidence to those patronizing our advertising pages, that you not only read the editorial pages, but the advertising section as well, and that you have in mind the welfare of your Institute by consulting the advertising pages when in the market for equipment. Do you realize that if you mention your Bulletin when writing advertisers or purchasing supplies, that not only would your publication secure more advertising, but better satisfy present advertisers. We have reason to know that our advertisers secure business as a result of our publication, but they demand some evidence that you see their advertisement. Unfortunately, our members do not as a rule mention where they saw the advertisement, and as a consequence advertisers have no means of knowing whether their investment in the Bulletin is paying. The A. I. M. E. Bulletin can be made the best advertising medium in the mining, metallurgical and chemical fields, simply by each member doing his bit. It is very little to ask of you, and the returns to the mining industry will be enormous.

Jan 9, 1915

By C. E. Sims, C. A. Zapffe

AN investigation of the behavior of inclusions in steel several years ago1 led to the conclusion that some of the commonly occurring inclusions in steel have appreciable solubilities, particularly in liquid steel. In the belief that further study and clarification of this matter was warranted, a laboratory study of oxides in liquid steel was started. These oxides are generally the result of deoxidation treatment, and the basis of an understanding of their behavior must be, therefore, the behavior of the deoxidizer in liquid iron. The Fe-Si-O system was selected for the first study, and the apparatus used and experiments conducted are described herein. APPARATUS The apparatus is shown in Fig. I and the system is shown by diagram in Fig. 2. Furnace Atmosphere Commercial hydrogen (1) passes through an orifice (2) into a manometric system that measures the tankside pressure (3) and the back pressure (4) in the system. A water trap (5) guards against excess tankside pressure. A by-pass with stopcocks (6 and 7) is provided, so that the hydrogen can be routed directly from the tank to the furnace if desired. When stopcock 7 is closed and stopcock 6 is open, the gas proceeds through the conditioning train, of which the first unit is a furnace (8) that contains platinized asbestos at 350°C. The temperature is measured by a thermocouple and potentiometer (9) and is controlled by a slidewire resistance (10). In [ ] this furnace free oxygen is converted to water vapor. The exiting gas passes over a water bath (11) kept slightly below boiling temperature by an auxiliary heating unit (12). This unit also heats a surrounding copper coil (13) containing water, and the heated water rises through a collar (14)

Jan 1, 1942

By Kenneth A. Moon

An exact statistical treatment of a one-dimensional model is used as a basis for evoluating the reliability of certain simplified expressions for the activity of the solute in interstitial solutions, including one obtained from the exact expression by setting the repulsive interaction equal to infinity. The latter approximation is found to be satisfactory at low and moderate concentration if the repulsive interaction is large, even though not infinite. A similar expression (identical if the co-odination number is two) is derived from the quasichemical expression of Lacher, and is recommended as the best available expression for the excess configurational entropy of interstitial solutions with excluded sites. Some reasonable models are discussed, and the nature of the saturated solutions is determined by inspection. Some of the models reduce to the one -dimensional case. An analysis is given of the excess partial entropy of hydrogen in V-H; Nb-H; and To-H solutions. MOST treatments of the statistical thermodynamics of interstitial solid solutions have followed the classic paper1 of Lacher in making the simplifying assumption that the configurational entropy of the solution is ideal. However, it is becoming increasingly apparent that there are many interstitial solutions with very large so lute-solute repulsions, and for these the assumption of ideal entropy is not valid or useful. It is important to realize that with substitutional solutions large repulsions between the component atoms must lead to phase separation, whereas in interstitial solutions the free energy of the solution is not drastically increased by large solute-solute repulsions until intrinsic saturation is reached at the concentration where further solute would be forced to enter a site in which it would experience the repulsive effect of one or more solute atoms already present. In the limiting case of an infinitely large repulsive interaction, the excess free energy would be attributable entirely to excess entropy, the enthalpy of mixing being zero. AS will be shown below, even if the repulsions are less than infinite, a treatment based on an assumption of infinite repulsions may be very satisfactory up to moderately high concentrations of the interstitial component. Often in solutions where large repulsive interactions exist, there are also small interactions — often attractive—between solute atoms in configurations other than that corresponding to the large repulsion. In such cases the excess free energy will consist of an excess entropy term attributable to the large repulsive interactions, and an enthalpy term corresponding to the other small interactions. Nomenclature to differentiate succinctly between important cases would be a convenience. In this paper the nomenclature shown in Table I will be used. In Table I, and in the preceeding discussion, excess quantities are defined in terms of standard states which are pure solid solvent and pure (possibly hypothetical) solid saturated phase of the structure in question. In practice, it is more convenient to choose the interstitial element as a component, and its conventional standard state. This will add a composition-independent term to the excess entropy and the enthalpy. The earliest paper known to the present author which treats the thermodynamics of athermal interstitial solutions was given by schei12 in 1951, but the statistical derivations in that paper are open to criticism. Speiser and Spretnak were the first to give a correct statistical treatment,3 limited, however, to concentrations sufficiently low that the number of empty sites excluded from occupancy by more than one filled site is negligible. The purpose of the present paper is to extend the statistical treatment to more concentrated solutions, and to examine the magnitude of the errors introduced by assuming that the repulsive interactions are infinite when in fact they must be finite. THE QUASICHEMICAL APPROXIMATION Fortunately, a standard method already exists for taking into account the effect of large interactions upon the entropy of mixing. This is the quasi-chemical method, in which the probability of existence of a given pair of solute atoms in a certain proximate configuration is assumed to be proportional to exp(-w/kT), where w is the energy increase of the solution when the two atoms are moved from isolated locations in the solution to the configuration in question. A quasichemical treatment of interstitial solutions was given in 1937 in a widely neglected paper by Lacher.4 The result comes out

Jan 1, 1963

By F. W. Luerssen, J. F. Elliott

F LUSHING the early slag from a stationary open Fhearth having a high percentage of hot metal in its charge is necessary in order to remove silica from the system. The flush slag is strongly oxidizing and is somewhat acidic. It has, however, considerable capacity to extract phosphorus from the bath and it also removes considerable manganese. It seems probable that factors which control the distribution of phosphorus and manganese between slag and metal in the refining period also should be dominant in the flush and postflush periods. Several studies, as summarized elsewhere,1,2 support the viewpoint that conditions closely approaching equilibrium for these elements are rather readily established during the refining period. Over the years these studies have repeatedly demonstrated that 1—high slag v01ume, 2—low bath and slag temperature, 3—basic slag, and 4—strongly oxidizing slag favor rapid elimination of phosphorus from the bath to the slag. They also show that the following conditions favor retention of manganese in the bath: 1—low slag volume, 2—high bath and slag temperature, 3— basic slag, and 4—minimum oxidizing power of slag. When it is considered that the flush slag often carries as high as 75 pct of the manganese charged and only 25 to 60 pct of the phosphorus charged, it is evident that in removing silica much manganese is sacrificed but phosphorus removal is far from conplete. Because of overriding circumstances, this is accepted in most operations and actually it is considered to be inevitable. This may account for the fact that little attention has been paid to conditions affecting the elimination of phosphorus and manganese in the flush slag. A recent study of the behavior of various charge oxides has developed considerable information on the flush and postflush periods. Because the data are felt to be of general interest, they have been brought together and Presented in this paper. The object is to show the various factors in the flush and postflush periods which influence elimination of phosphorus and manganese. Physical Conditions During and After Flushing Physical conditions existing during the flush vary from plant to plant, from shop to shop, from furnace to furnace, and even from heat to heat. They are strongly influenced by the physical and chemical character of the charge oxide which is ordinarily necessary to provide sufficient oxidizing power early in the heat. Invariably the period is characterized by a vigorous reaction between the principal re-actants: the hot metal being added and the charge oxide. During the flush, it is probable that the slag acts to some extent as an oxidizer; but, because of the critical influence of the behavior of the charge oxid'e on flushing action, it seems apparent that the oxide itself is the dominant oxidizer. Fig. 1 shows the course of two heats which were selected as being typical of the group studied. Heat A was charged with 55 pet hot metal, based on the total metallics charged, and heat B had 57 pct hot metal. As indicated in Table I and Fig. 1, the melt-down slag, which is not usually voluminous and which is principally FeO, expands greatly in volume and will show rather high levels of SiO2, MnO, and P2O5 very soon after the beginning of the hot metal addition. Simultaneously, large volumes of CO are liberated which cause violent mixing of slag and metal. It is of interest to note that the time required to bring carbon down to a low level is very much longer than that required for the removal of silicon, manganese, or phosphorus. At the end of flush, carbon in the bath is still approximately 2 pct. When strongly reducing hot metal is brought into contact with strongly oxidizing conditions within the furnace! it is probable that the rate of mass transfer to the slag (and atmosphere) of silicon, manganese, phosphorus, and carbon initially depends principally on the rates at which the two participating phases are brought into contact That is, it depends on the nature of the various reactions. Later in the flush period, when the scrap is virtually all dissolved and the action of the bath has settled down to a steady and somewhat gentle boil, it is likely that other factors, such as the transfer of oxygen across the slag-metal interface, become dominant. The temperature of the slag-metal system is far from uniform. Heat is being driven by the flame down through the slag. Bubbling and surging of the metal also frequently brings portions of the bath in contact with the flame. At areas of contact between the ore and liquid metal, or slag and liquid metal, the oxidizing reactions generate much heat. On the other hand, scrap is being melted which tends to absorb large quantities of heat. Because the liquid bath is high in carbon, the steel scrap is brought into solution rapidly. This can proceed at a rather low temperature; and until much of the scrap has been taken into solution, the bath temperature would not be expected to increase appreciably. Consideration of these factors leads to the conclusion that during the flush period the slag should be rather hot and the bath relatively cold. Both observation and temperature measurements bear this out. Experimental Data The extended program of charge oxide evaluation permitted study of the widely varying conditions existing during the flushing period. Slag and metal analyses and bath temperatures reported herein (Tables I and 11) were obtained toward the latter portion of the work. Four different types of charge oxide, sinter, two types of hydraulic cement-bonded soft ores, and a pyrobonded agglomerate were used in the study. Although the heats reported were from only one 205 ton furnace, they show variations in flush slag analyses all the way from 25 pct FeO, which is typical with the use of a hard natural charge ore, to 45 pct FeO which resulted when a very poorly agglomerated fine ore was used. The physical behavior of the flushes showed a correspondingly wide variation from well controlled reactions to violent surges following periods of inac-

Jan 1, 1956

By AIME AIME

FOR the purpose of subsequent discussion let me reiterate certain points in my paper. The things we are certain of are that individuals differ in their accident liability, and that the bulk of accidents in any industrial group is sustained by comparatively few individuals; further, that this difference in liability cannot be wholly accounted for by differences of exposure, since some of the personal factors involving a high accident rate have already been measured in certain industrial groups.

Jan 1, 1929

By Arthur T. Ward

WHEN the Board of Directors of the Institute in June 1931 approved the formation of the Committee on Eastern Magnetite and its then membership of eleven, little did any of those concerned envision that twelve years later the annual Committee luncheon would attract 34, and the technical session, jointly with the Iron and Steel Division, more than 70. Yet that was exactly what happened during the February meeting just passed. And what is more important, some members of the Committee are now predicting that by 1944 over 10 per cent of the iron ore produced in the United States will come from these Eastern Magnetite properties. Chairman Crockett, in opening the meeting, advised that due to the serious illness of Meredith E. Johnson, State Geologist of New Jersey, Mr. Johnson would be unable to brief his scheduled paper, which would therefore be reserved for a later date.

Jan 1, 1943

By N. K. Chen, C. H. Mathewson

Single crystals of high purity aluminum of various orientations were carefully documented after plastic extension. Special attention was given to the formation of slip lines, deformation bands, and asterism. An explanation for the geometry and mechanism of formation of deformation bands is considered. WHILE the general process of plastic extension of face-centered cubic metals is well understood,' the accompanying structural changes due to slip and rotation are far more complex than ordinarily assumed. In the case of stretched single crystals of aluminum, the complicated behavior is especially marked by the formation of deformation bands, as first indicated by Collins and Mathewson." Such bands were believed by them and also by others,".'7 who have discussed banded structure in general, to represent one of the important modes of lattice reorientation and to be intimately connected with the recrystallization process. Yet, despite their fundamental importance to the understanding of the mechanism df both plastic deformation and recrystallization, practically no study of the crystallographic features of these bands in their relationship to the conventional slip process has been attempted. This paper describes part of an extensive investigation on the structural behavior during plastic deformation of aluminum single crystals and is especially concerned with the characteristics of deformation bands. The investigation of the subsequent re-crystallization of deformed aluminum single crystals will be discussed in a later publication. Experimental Procedure Single crystal specimens of 99.996+ pct pure aluminum, Yz in. in diam and 5 to 6 in. in length were made both by the Bridgman method5 nd by a modified temperature gradient method.'* Crystals were selected in which the lineage deviation did not exceed 2"; i.e., as determined from the back-reflection Laue X-ray photograms. These crystals were radiographed to insure that no internal porosity was present. The orientations showed good coverage of the whole area of the Taylor and Elam triangle.' Orientations of the crystals were obtained by the back-reflection Laue technique described by Greninger." Crystals so selected were tapered very carefully in a lathe to obtain a linear decrease in diameter from 0.500 to 0.350 in. along a gage length of 3 in. This is considered desirable because it permits a strain gradient to be introduced in a single specimen at one initial orientation. The advantages of tapered crystals for studying the development of slip lines and recrystallized grains have been pointed out by previous investigators." The cold-worked layer resulting from the machining operation was removed by alternate etching in aqua regia and careful polishing with 2/0 emery paper until undistorted Laue back-reflection spots were obtained. A homogenization treatment at 600 °C for 24 hr was then introduced to insure the removal of residual stress. Two of the crystals so prepared were also checked by use of a glancing angle technique. Using a copper target, at 30 kv and 10 microamperes, a monochromatic beam was positioned at right angles to the axis of the crystal about which it rotated. The time of exposure was 24 hr. From these X-ray photograms, it was concluded that the present method of preparation of single crystals is satisfactory. Following this procedure, the crystals were elec-trolytically polished in a 2:l solution of methyl alcohol and concentrated nitric acid. Intermittent

Jan 1, 1952

By Y. C. Liu, R. H. Richman

From rolling textures of polycrystalline AgCl determined as a function of temperature, changes in the amounts of the individual textural components are correlated with temperature-dependent changes in glide geometry. The preferred orientations are influenced by the slip behavior as follows: 1) pencil glide, characterized by (110) slip directions and a greater participation in the deformation the higher the temperature, leads to a(012) fiber texture; 2) low-temperature deformation, primarily on (110) (110) systems, generates the {237}-(11, 9, 7) component; and 3) slip on {111}(110), comprising a significant portion of the room-temperature deformation, generates the {135}(211) and {110}(112) components. Typical re crystallization textures are also presented and briefly discussed. SPECIFIC relations between flow mechanisms in crystals and the individual orientations or components in deformation textures are necessary for a thorough understanding of the origin of such textures. Within each ordinary class of crystal struc- tures there is insufficient variety in the observed preferred orientations to permit direct and unambiguous correlation between flow mechanism and texture. A second approach to this problem is the correlation of textural changes with some known variation in glide geometry within one substance,1 In this paper, the latter approach is applied directly to a material in which there are distinct changes in the character of glide with changes in temperature. Silver chloride, although a nonmetal, is reported to exhibit slip,2,3 fiber textures,4 and rolling textures5,6 crystallographically similar to those of the well-studied fcc metals;7,8 in addition, there is a marked temperature sensitivity of the glide planes upon which flow occurs.3 Previous investigations of textures in AgCl unfortunately did not employ methods sufficiently sensitive to define possibly important minor components in the texture, nor did they utilize the temperature dependence of the glide systems. Thus, in order to clarify the effects of changes in slip mechanism, this paper reports a survey, using semiquantitative methods, of preferred orientations in rolled AgC1. Inasmuch as the influence of prior deformation texture upon preferred orientations after annealing is also of interest, some representative annealing textures are presented.

Jan 1, 1965

By T. B. Counselman

PRobably the earliest concentration of iron ore in this country was carried on in the northeastern magnetite areas. Magnetic concentration was relatively simple and gave a concentrate that, after agglomeration, and in spite of beillg high in phosphorus hecause of the dry concentrating methods then in use, was satisfactory blast-furnace feed. Production from the northeastern magnetitc area languished after the discovery and development of the Lake Superior ores, where there was seemingly an unlimited tonnage of high-grade ore, first the Michigan ores, and subsequently the still larger deposits of Minnesota. For years only the higher grade, direct shipping ores of the Lake superior district were mined. Those of Michigan, and of the Vermilion Range in Minnesota, were hard ores and came principally from underground mines. The softer ores of the Mesabi came partly from underground mincs, but mostly from the enormous deposits that could be worked by open-pit methods. The costs of ore from these open-pit deposits, even with the high initial cost of stripping, were so low that the underground mines of the Mesabi could hardly compete. The so-called Old Range ores, of Michigan and of the Vermilion Range of Minnesota, were hard and lumpy, and opened UP the burden in the blast furnace, therefore making possible harder driving with greater output. Also, some of these Ores were of such grade and physical characteristics that they were suitable for charge ore in the open hearth. These ores, therefore, commanded a price premium. and could compete with the softer, finer, but cheaper, Mesabi ores. The big tonnage reserves, however, are on the Mesabi. and it is these big open-pit deposits that contitue- our stock pile of iron ore, from which we are drawing so heavily during this war period. On the western end of the Mesabi the ore was found to be high in silica, and not suitable as furnace feed. As early as 1902, attempts were made to concentrate this so-called wash ore and by 1910 the first washing plant was put into operation. The Process was very simple, consisting essentially of a sizing and washing operation, with scalping screens, logwashers and tables, which later were replaced by classificrs. Ore particles finer than I00 mesh were deliberately wasted, because these fines were undesirable in the furnace. Fortunately, these tailings were impounded, and already are being reworked. Before long some of the low-grade ores began to require more elaborate treatment than the simple washing operation and, tables having been discarded because of their low capacity, in favor of classifiers, jigs were next introduced. These were able to discard coarser pieces of tailing than classifiers. Jigs are in active use today, various improvements having been made in their design and application. Various other machines and methods of concentration have been tried from time to time, and have in turn been discarded for more improved processes., The latest and most important process that has been 38

Jan 1, 1944