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By G. Donald Emigh

Nothing is more important to life-plant and animal-than phosphate. Its compounds are essential to the energy functions of all living systems and for the formation of bones and teeth. Animals get their phosphate from eating plants and other animals, or domestically from feed supplements. Plants get their phosphate from the soil. Man's most important use of phosphate is for fertilizer; however, he is also a heavy user of many industrial phosphate chemicals. Phosphate occurs in all igneous and sedimentary rocks, and in all fresh and saltwater. The average content in rocks is 0.1 to 0.2% P2O5, as documented recently by McKelvey (1973). About 200 minerals contain more than 1 % P,O,. However, the important one in igneous rocks is fluorapatite, (Ca,(PO,) ,F) containing about 42% P,O, and 3.8% F,; in sedimentary rocks the one important mineral is francolite, a carbonate fluorapatite containing up to 2% molecular CO,. Both are in the apatite family of minerals. The mineralogy of phosphate minerals was reviewed recently by Altschuler (1973). Although phosphate occurs in nearly all rocks, economic recovery is limited to deposits where natural concentration of the phosphate mineral has occurred. Occasionally natural concentration is great enough that the material can be used as mined; generally, however, the ore is low grade and must be concentrated.

Jan 1, 1975

By Robert P. Burrows

Discussion of the paper of R. P. Burrows, presented `at the New York meeting, February, 1916, and printed in Bulletin No. 107, November, 1915, pp. 2237 to 2245. EDWIN M. CHANCE, Wilkes-Barre, Pa.-I have been very much interested in the comprehensive and able discussion of the important topic of mine lighting just given by Mr. Burrows, especially as I know by common report Mr. Burrows' ability and his close touch with the development of the electric mine lamp, and its use in mines in connection with a portable electric lamp. It is regrettable that Mr: Burrows was not able to acquaint himself more closely with the cost of mine illumination, the actual cost, as produced by a portable light as carried by miners, whether a flame safety lamp or an open light. Had he been able to acquaint himself more closely with these data, he perhaps would not have arrived at some of the conclusions which he has presented to us in his paper. For example, we find Mr. Burrows advises that the open torch is by far the cheapest source of illumination, as produced by a portable light. I am very sure that is not the fact. The cost of miners' oil varies from about 25.c. a gallon to 90b. a gallon. The various States have passed laws from time to time rendering it mandatory that the miner shall use, whether he is willing or not, a so-called better or higher grade of burning oil. These laws have entailed the use of an oil so expensive that the use of the oil torch has become practically impossible, and the acetylene or carbide miners' lamp has largely taken its place. I have evolved a few figures showing the relative efficiency and usefulness of the open oil torch and the acetylene miners' lamp. For example, the acetylene miners' lamp consumes or burns 4 liters of acetylene per hour, or 0.14 cu. ft.; the oxygen consumed is 10 liters, or 0.35 cu. ft. per hour; air consumed, 50 liters, or 1.76 cu. ft. per hour; black-damp produced, 40 liters, or 1.41 cu. ft. per hour; air rendered extinctive to the acetylene flame, 112 liters, or 3.95 cu. ft. per hour; carbide con- sumed, 13 g. per hour. The open oil torch, on the other hand, burns about 20 g. of oil per hour; the oxygen consumed is 48 liters, or 1.69 cu. ft. per. hour; air consumed, 240 liters, or 8.47 cu. ft. per hour; blackdamp produced, 191 liters, or 6.73 cu. ft. per hour; air rendered extinctive to oil flame is 1,413 liters, or 49.92 cu. ft. per hour.

Jan 5, 1916

By Horace Knerr

IT has been shown1 that the resistance to corrosion of duralumin sheet is greatly influenced by the quenching medium used in heat treatment, or, more specifically, by the rate of cooling during quenching. The severity of corrosive attack after exposure to salt-water spray increases in the following order: DEGREE OF CORROSION, BY INSPECTION, QUENCHING MEDIUM AFTER 30 DAYS OF SALT-WATER SPRAY TEST; Water, cold (60° F.) Very slight. Water boiling Slight, but more than with cold water. Oil (70° F.) Slight, but more than with cold water. Air, fan blast, 65° F Severe, scaled. Air, still, 65° F Deeply scaled. The tensile strength, yield point and elongation are only slightly affected by the quenching medium, as shown in Table 1.

Jan 1, 1930

By Shiou-Chuan Sun

THIS paper presents the design and operation of a frothmeter capable of measuring the frothing characteristics of pine oils and other frothing reagents. The experimental data show that the frothability of pine oil is governed by: 1-rate of aeration, 2-time of aeration, 3-height of liquid column, 4-chemical composition of pine oil, 5-pH value of solution, 6-temperature of, solution, and 7-concentration of pine oil in solution. The effect of mineral particles on the behavior of froth also was studied, and the results can be found in a separate paper.1 The results also show that the relative frothabilities of pine oils in the frothmeter generally correlate with those in actual flotation, provided that other factors are kept constant. In addition to pine oils, the other well-established flotation frothers were tested, and the results are included. In this paper, compressed air frothing is the frothing process performed by means of purified compressed air, whereas sucked air frothing is the frothing process accomplished by purified air sucked into the glass cylinder by a vacuum system. The term vacuum frothing denotes that froth was formed by degassing of the air-saturated liquid under a closed vacuum system. Apparatus The frothmeter, shown in Fig. 1, is capable of reproducibly measuring the volume and persistence of froth as well as the volume of air bubbles entrapped in the liquid and is capable of being used for compressed air frothing, sucked air frothing, and vacuum frothing. Fig. la shows that for compressed air frothing, the apparatus consists of an airflow regulating system, 1-3; a purifying and drying system, 4-8; a standardized flowmeter to measure the rate of airflow from zero to 500 cc per sec, 9; and a graduated glass cylinder, 13; equipped with an air regulating stopcock, 10; an air chamber, 11; and a fritted glass disk to produce froth, 12. The fritted glass disk, 5 cm in diam and 0.3 cm thick, has an average pore diameter of 85 to 145 microns. The pyrex glass cylinder has a uniform ID of 5.588 cm and an effective height of 63 cm. The inside cross-sectional area of the glass cylinder was calculated to be 24.53 sq cm, or 3.8 sq in. For sucked air frothing, Fig. lb shows that the apparatus for compressed air frothing is used again, with the following modifications: 1-compressed air and its regulating system, 1-3, are eliminated; and 2-a vacuum system, 16, equipped with a vapor trap, 15, and a vacuum manometer, 17, is added. The vacuum system can be .either a water aspirator or a laboratory vacuum pump. Any desired rate of airflow can be drawn into the glass cylinder, 13, by adjusting the opening of the air regulating stopcock, 10. The sucked air stream is cleaned by the purifing and drying system, 4-8, before entering the glass cylinder, 13. When this setup is used for vacuum frothing, the air regulating stopcock is closed. The frothmeter has been used for almost 3 years and has proved to give reproducible results, as illustrated in Table I. With a magnifying glass and suitable illumination, the frothmeter also can be used to study the attachment of air bubbles to coarse mineral particles.2 Experimental Procedures Except where otherwise stated, the data presented were established by means of the compressed air method. The volume and persistence of froth were recorded respectively at the end of 4 and 6 min of aeration at a constant rate of airflow of 29.3 cc per sec which is equivalent to 71.6 cc per sq cm per min, or 462.6 cc per sq in. per min. The aqueous solution for each test, containing 1000 cc of distilled water and 19.2 ± 0.5 mg frothing reagent, was adjusted to a pH of 6.9 ± 0.2. The volume of froth is expressed as cubic centimeter per square centimeter and is equivalent to the height of the froth column (the distance between the bottom and the meniscus of the froth). The volume of froth was obtained by multiplying the height of froth by the cross-sectional area of the glass cylinder, 24.53 sq cm. Before each test, the glass cylinder, 13, was cleaned thoroughly with jets of tap water, ethyl alcohol, tap water, cleaning solution, tap water, and finally distilled water. The cylinder with stopcock,

Jan 1, 1952

By John G. H. Crump, E. W. Owen, Peter P. Gregory

A noticeable decrease in activity characterized the year 1938 in the West Texas area. The total number of wells completed dropped to 2045 for 19381 as compared with 2806 completions in 1937,l a decline of 27.12 per cent. This trend contrasts the sharp increase of 76.29 per cent in completions in 1937 over the 1936 total. Of 2045 well completions during 1938,' 1788 were oil wellsll 16 were gas producers1 and 241 were listed as failures.' During 1938 the ratio of dry holes drilled to oil-producing or gas-producing wells completed was one dry hole to each 7.48 oil wells, which compares with one dry hole drilled to each 7.477 oil wells in 1937. Nearly 200 wells drilled during 1938 in West Texas were either wildcat or partly wildcat wells, an increase of about 25 over the year 1937, when approximately 175 wells drilled were so classified. The 200 exploratory wells drilled represent about 10 per cent of the total number of wells completed. West Texas produced 71,257,541 bbl.1 of oil in 1938 as compared with 75,743,000 bb1.2 of oil in 1937, a decrease of 4,485,459 bbl., or a 5.92 per cent decline. By comparison, West Texas produced 22.36 per cent more oil in 1937 than during 1936. In December 1938, the 9247 producing oil wells in West Texas1 averaged 22.08 bbl. per day per well as compared with December 1937, when 7571 wells1 produced an average of 25.18 bbl. per day per well, or a decline in daily well average of 12.32 per cent. Discoveries No outstanding new fields were discovered in West Texas during 1938, in spite of continued, active wildcatting operations. Several new oil-producing areas were, found, however, the value of which is still unknown.

Jan 1, 1939

By E. W. Owen, John G. H. Crump, Peter P. Gregory

A noticeable decrease in activity characterized the year 1938 in the West Texas area. The total number of wells completed dropped to 2045 for 19381 as compared with 2806 completions in 1937,l a decline of 27.12 per cent. This trend contrasts the sharp increase of 76.29 per cent in completions in 1937 over the 1936 total. Of 2045 well completions during 1938,' 1788 were oil wellsll 16 were gas producers1 and 241 were listed as failures.' During 1938 the ratio of dry holes drilled to oil-producing or gas-producing wells completed was one dry hole to each 7.48 oil wells, which compares with one dry hole drilled to each 7.477 oil wells in 1937. Nearly 200 wells drilled during 1938 in West Texas were either wildcat or partly wildcat wells, an increase of about 25 over the year 1937, when approximately 175 wells drilled were so classified. The 200 exploratory wells drilled represent about 10 per cent of the total number of wells completed. West Texas produced 71,257,541 bbl.1 of oil in 1938 as compared with 75,743,000 bb1.2 of oil in 1937, a decrease of 4,485,459 bbl., or a 5.92 per cent decline. By comparison, West Texas produced 22.36 per cent more oil in 1937 than during 1936. In December 1938, the 9247 producing oil wells in West Texas1 averaged 22.08 bbl. per day per well as compared with December 1937, when 7571 wells1 produced an average of 25.18 bbl. per day per well, or a decline in daily well average of 12.32 per cent. Discoveries No outstanding new fields were discovered in West Texas during 1938, in spite of continued, active wildcatting operations. Several new oil-producing areas were, found, however, the value of which is still unknown.

Jan 1, 1939

By Jerry H. Service, F. L. Partlo

The following investigation was undertaken to develop a method for determining with reasonable accuracy the depth of overburdens of 100 ft. or less. Seismic methods seemed to offer good possibilities. The problem differed from that of the familiar salt-dome location in that the depth of overburden to be determined is much less than is encountered in oil prospecting. This means that a much shorter time interval must be measured with accuracy. Refraction methods seem at present to offer greater possibilities than reflection. The air sound persists for from 0.1 to 0.5 sec., because of echoes, and seismic reflections coming during this time are difficult to detect. A seismometer sensitive to vertical vibrations only offers possibilities and has been used here with some success. It is hoped that the application of this type of seismometer to reflection shooting in this region may be investigated still further. The apparatus used consisted of a carbon-button seismometer followed by a three-stage, transformer-coupled, vacuum-tube amplifier and a General Radio string oscillograph. Time marks are provided by a 1000-cycle, 600-r.p.m., synchronous motor provided with five spokes which intercept the light to the camera at 1/50 sec. intervals. This motor is driven by a two-stage vacuum-tube amplifier of 3 watt output, actuated by a tuning fork. The power supply for the seismometer amplifier is one 2-volt storage and one 45-volt B battery. The motor amplifier is powered by a 6-volt storage battery and 6 to 225-volt, 15-watt motor generator. The temperature-frequency characteristics of the tuning fork have been determined and for ordinary working temperatures the error in time that would be introduced is less than M millisecond for time intervals up to 100 milliseconds. The impact is produced by a sledge blow for surface distances less than 100 ft. and dynamite for greater distances. Two steel balls with wires attached form an electric circuit through a 1-ft. piece of railroad rail upon which they rest. When the rail is struck by the sledge the balls rebound, opening the circuit and indicating the time of impact by a break in the oscillograph record line as at A, Fig. 3. When dynamite

Jan 1, 1934

By D. W. Fuerstenau, P. C. Kapur

The kinetics of green pelletization in a laboratory balling drum have been studied, using pulverized limestone as a model system. The growth characteristics of green pellets were found to be extremely sensitive to the moisture content of the material. Empirical kinetic equations, which incorporate a function of specific surface of the pellets as the criterion for growth potential, have been found to describe growth in a nucleation region and in a ball growth region. The rate constants in the kinetic equations are strongly dependent on the moisture content of the material being pelletized. Size distributions of the balls at different stages of pelletiz-ing are also discussed. In many industrial chemical processes, particulate matter can only be utilized if it is in an agglomerated form, such as pellets. Pelletizing is now widely used in iron ore technology1, and it has also been applied to a number of diverse fields such as the production of cement-kiln feed2, fertilizers3, and fluorspar4. Recently, it has been proposed to pelletize dispersion-type ceramic nuclear fuel elements5. In iron ore technology, for example, the production of agglomerates by pelletizing involves two major steps: 1) the preparation of green balls by rolling particles in a suitable balling device and 2) the firing of the green balls to form compact, strong bodies upon sintering. The critical step in a successful iron ore pelletizing operation is generally considered to be the balling operation1. In this paper, which is not concerned with the sintering of green pellets, the words green pelletizing and balling will be used interchangeably. Green pelletizing, or balling, will be defined as the process of forming larger bodies by rolling fine particles on a surface without the application of direct pressure. Two recent literature surveys6" indicate that in spite of the considerable amount of industrial pelletizing, very little is known about the fundamental principles of balling and its kinetics. The first reported research on the kinetics of pelletizing is the work of Newitt and Conway-Jones8. Using silica sands of different sizes in a batch laboratory balling drum, they found that the average green pellet diameter increased linearly with time at constant drum speed, and qualitatively the growth rate increased with moisture content. Generalized conclusions cannot be drawn from their research since the materials which they pelletized were sand and sand-silt mixtures rather than comminuted materials. Moreover, Newitt and Conway-Jones used testing sieves to estimate the size distribution of the green pellets, and this technique limited the range over which they could study the growth kinetics of the pellets. Bhrany and co-workers9 investigated the kinetics of balling iron ore fines on disk pelletizers ranging in diam from 1 to 18 ft. In their investigation, balling was carried out as a continuous operation, and growth kinetics were studied in terms of retention time of the material on the disk. Although the feed material in their study was quite coarse (the maximum size being about 1/2 in.), they also found qualitative relationships between pellet growth and water content, and feed size. In the present investigation, a number of innovations were introduced that refined the experimental measurements and established the reproducibility of balling experimentation. This enabled extension of the range of measurements to include study of agglomerate nucleation phenomena in the fractional mm size. This paper presents a detailed analysis of the nucleation and growth of green pellets in a laboratory balling drum. MATERIALS AND METHOD Pulverized limestone of specific gravity 2.72 was used as a model system in these studies. It has already been established that the balling characteristics of limestone and silica are similar to those of iron ore concentrates 2,8,10, depending on physical, rather than chemical, properties of the particles. The size distribution of the limestone was determined by a wet-dry sieving technique in the sieve range and by a sedimentation balance in the sub-sieve range. Fig. 1 presents the size distribution of the limestone used in this research. This figure shows that the material is finer than 200p (65 mesh) and that 25% of it is finer than 12. The specific surface area of this powder, as measured by BET gas adsorption methods,

Jan 1, 1964

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

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

Jan 1, 1953

By E. T. Turkdogan, J. H. Swisher

The solubility of oxygen in zone-refined iron was determined in the temperature range.from 881" to 1350°C. The solubility in a iron at 881°C ms found to be about 2 to 3 ppm; in y iron, the solubility was found to increase from about 2 to 3 ppm at 950°C to about 25 ppm at 1350°C. The permeability of oxygen in an iron -0.1 pct Al alloy was determined in the y iron range, using an internal oxidation technique. By combining the permeability and solubility data, the diffzisivity of oxygen in y and a iron was calculated. The oxygen diffusivity in solid iron may be s~immarized as follows: 8820 For 6 iron and IN a recent paper, Hepworth, Smith, and Turkdogan1 reported on the solubility, permeability, and diffusivity of oxygen in 6 iron, together with permeability data for oxygen in a iron. In the present investigation, similar measurements were made in the ? phase region. In addition, a solubility measurement was performed in the a phase region to permit calculation of the diffusivity of oxygen in a, iron. References to early work on this subject are given in the previous publication.' EXPERIMENTAL Solubility Measurements. The oxygen solubility was determined by equilibrating cylindrical samples 0.3 in. diam by 14 in. long of zone-refined iron in water vapor-hydrogen gas mixtures. The zone-refined iron was prepared by B. F. Oliver of this laboratory, using an apparatus and technique described elsewhere.2'3 Six zone-melting passes were used to achieve a total impurity level of about 30 ppm. Of this 30 ppm, the combined nickel and cobalt content was about 20 ppm, oxygen was 4 ppm, and all oxidizable impurities less than 1 pprn each. A vertical resistance furnace wound with molybdenum wire was used for the experiments. The temperature was measured before and after each experiment with a Pt/Pt-10 pct Rh thermocouple. In the gas train, flow rates of hydrogen and argon were measured with capillary flow meters, and the resulting mixtures were passed through a column containing 90 pct oxalic acid dihydrate and 10 pct anhydrous oxalic acid to obtain predetermined ratios of H2O to H2. The vapor pressure of H2O above this mixture as a function of temperature is well-known.4 The exit gas was ana- lyzed periodically for H2O, and good agreement (+3 pct) with the calculated composition was obtained. The zone-refined iron specimens were held in the furnace for a sufficient length of time for equilibration, e.g., 18 hr at 1350°C and 1 week at 881°C, then quenched in a brine solution. After removing the surface oxide from the samples by machining, duplicate analyses were obtained by a combined vacuum fusion-infrared method; oxygen analysis was reproducible within 2 ppm. Permeability Measurements. The permeability of oxygen in alloys containing about 0.1 pct A1 was determined by internal oxidation and measurement of the subscale thickness as a function of time. The experimental alloys were prepared by adding aluminum to electrolytic iron (grade 104A plastiron) that had previously been vacuum-carbon deoxidized. The resulting ingots contained about 20 ppm O, 100 pprn C, 40 pprn Si, 50 ppm Mo, 20 ppm P, 20 ppm S, and 20 pprn Zr as the principal impurities. After hot rolling the ingots to 1-in.-thick slabs, specimens were machined from the stock in the form of rectangular plates, 4 by 5 by 2 in. The general procedure for the permeability experiments was the same as those for the solubility measurements. The specimens were cooled in a reducing atmosphere rather than quenched, however, in order to maintain a clean surface for measurement of the sub-scale thickness. This measurement was made on a polished cross section of each specimen, using a microscope with a micrometer stage. The inclusions formed at the lowest temperature 1033°C were too small to be seen with an optical microscope. An electron micrograph showing the size and shape of individual particles is shown in Fig. 1. The dark band in the picture is a boundary between two subgrains. The subscale thickness in these samples was measured with an optical microscope after heavily etching in 2 pct nital, which gave contrast between the subscale and the unoxidized zone.

Jan 1, 1968

By R. S. McCaffery, D. E. Krause

There has been some discussion among blast-furnace operators regarding the relative merits of tuyeres of the converging type and tuyeres designed in an attempt to produce a diverging jet of air. An article1 on Progress in German Blast Furnace Practice indicates the interest in this subject abroad. This article illustrates a diverging type of tuyere which is shown here in Fig. 1A. The design appears to be rather poor as regards known properties of air flow. The adoption of this tuyere, the arlicle states, resulted in a decrease of blast pressure of about 4 Ib. per sq. in. and an increase of the output of the furnace. If the improvements mentioned are due entirely to the change in tuyere design, the subject of tuyere design seemed worthy of investigation and this paper is a report of such work. Because of the gain in efficiency brought about by the use of a diverging tuyere in the German plant, it was thought desirable to investigate the shape of the air streams issuing from various types of tuyeres to ascertain whether the gain was due to the tuyere itself or to the distribution of the air in the furnace. Since it is difficult to do experimental work on a full-sized furnace, or even on full-sized tuyeres, and because of the equipment available for the work, it was decided to carry out the work on scale models of tuyeres. Therefore, in this work, single tuyeres were used and the blast discharged into the atmosphere. The shape of the air stream was determined by means of a Pitot tube suitably supported in the air stream at various positions. The air was furnished by a Roots blower driven by a 10-hp. direct-current motor having field control, and capable of discharging 250 cu. ft. per min. with a pressure on the discharge of 4 in. of mercury. A modern blast furnace with 21-ft. hearth requires about 50,000 cu. ft. per min. of free air at from 16 to 23 Ib. per sq. in. pressure, depending upon the type of burden. This pressure is the total pressure required to force the air through the burden and through the tuyeres. Upon computation the pressure drop through the tuyeres is about 1 to 2 lb. per sq. in. By making the tuyeres to a one-fifth scale, and by using a pressure of 1.5 in. of mercury, the shape of the air streams should be

Jan 1, 1931

By J. W. Sandelin, L. S. Birks

The group five metals, vanadium, niobium, and tantalum all show cold-rolled textures of {100)(011) and {112)(0ll) with a preference for the (100) in vanadium and niobium and for the {112) in tantalum. Recrys-tallization texture of (100) and (111) was reported1 for vanadium after annealing (no temperature stated). For tantal~m ,~ annealing below 1200°C strengthened the (112) texture but the (111) texture increased and was predominant as the annealing temperature was raised to 2500°C. Annealing niobium up to 1100°C strengthened the ( 100) texture and developed a weak (111) texture.' In the present work niobium has been annealed up to 2000°C. Nearly 70 pct of the grains showed {111) texture with only a weak (112) component and an insignificant (100) component remaining. In addition, double-crystal rocking curves were used to follow the increase in crystal perfection of the grains with increased annealing time. Material and Treatment. Samples i by 4 in. were sawed from & -in.-thick cold-rolled niobium sheet obtained from Wah Chang. Chemical analysis of the material showed it to be 99.4 pct pure with tantalum as the major impurity. Individual pieces were annealed for 2, 15, 30, and 60 rnin in a vacuum of 10'* Torr using an rf generator. They were etched until the grain boundaries were well-defined, Fig. 1. Average grain size varied from 1 mm for 2 min annealing to 2 mm for 60 rnin annealing. Experimental Results. Preferred Orientation. The orientations of 97 of the 117 grains in the specimens of Fig. 1 were determined by back-reflect ion Laue patterns. A General Electric 10-cm-diam cylindrical camera was used rather than the conventional flat camera in order to record more of the low-index spots. The method proposed by Forest, Barton, and schieltz4 was used to transform the cylindrical film patterns to standard stereographic projections. Table I gives the compilation of data. Even 2 rnin anneal at 2000°C is sufficient to yield a strong (111) preferred orientation, and the percentage of grains with this orientation increases steadily with annealing time at the expense of all other orientations. Crystal Perfection. X-ray topographs were taken of each specimen in both the (111) and (112) orientation using the method described by Birks and Grant.' As the anneal time increases, the grains become larger and the individual reflections become slightly more uniform in intensity, indicating an increase in crystal perfection. For a more quantitative measure of crystal perfection, it was necessary to measure the double-crystal rocking curve. The spectrometer employed was a Gaertner instrument of Compton design. LiF was chosen for the first crystal because the (400) reflection with d spacing of 1.05 AU is a good match to the (222) niobium reflection with d spacing of 0.95 AU. CuKp radiation was used in order to further reduce the d spacing mixmatch correction.' A variable aperture was placed between the LiF and the niobium specimen so that a single grain or even a small portion of a grain could be examined. Fig. 2 shows typical rocking curves for the four annealing times. For the 2-min specimen, a single peak is observed with 10' of arc full-breadth at half maximum. As the annealing time is increased to 15 or 30 min, several sharper peaks of 40 to 80" breadth can be seen within a single grain. After 60 rnin anneal only a single peak of about 30" is observed. Table I1 shows the corrected rocking curve breadths and the dislocation densities, ND. The latter were calculated from the equation7 where W is the corrected rocking curve breadth at half maximum in radians and b is the effective Burger's vector. For (110)(111) slip in niobium, b is 2.86 AU. Discussion. The annealing of cold-rolled niobium at 2000°C causes rapid preferential growth of grains with {ill} orientation. After only 2 rnin annealing time, 35 pct of the grains have the (111) orientation, and after

Jan 1, 1968

By J. J. Gilman

THEORIES of fracture in metals have been based primarily on the dependence of fracture strength on grain size. This dependence was first observed by Masing and Polanyi.l These workers, as well as 0rowan12 and Davidenkov and Wittman,' thought the grain size could be equated with the crack size in the Griffith condition for crack propagation.4 In this way they could account for the observed proportionality between fracture stress and the reciprocal square root of the grain size. The chief results of recent investigations of the fracture strength of polycrystals are summarized in Fig. 1. Low for iron,5 Petch for iron,' Greenwood and Quarrel for zinc, Petch and Zein for zinc,' and Hauser, Landon, and Dorn for magnesium'' have all found that the fracture stress of a polycrystal is proportional to the reciprocal square root of the grain size. Also, they find that, for large grain sizes, the fracture stress lies near the extrapolation of the yield-stress curve determined at small grain sizes; where measurable plastic strain precedes fracture. Low9 has gone a step further and shown that, in Range 1, the fracture stress in tension is almost identical to the yield stress in compression for a given grain size. Homes and Gouzou, 10 and Low also have shown that, in Range 2 of Fig. 1, microcracks form when the yield stress is reached, but they do not cause failure until the stress reaches a much higher value. The fact that yielding always precedes fracture suggests that fracture is induced by plastic flow. A mechanism by which this might occur was first proposed by Zener.11 He pointed out that blocked dislocations would cause stress concentrations which might cause fracture. The blocking would be caused by grain boundaries. This idea has been developed by Eshelby, Frank, and Nabarro,12 by Koehler,13 and by Stroh.14 By means of etchpits blocked dislocations have been observed in brass by Jacquet,15 in zinc by Gilman,16 and in lithium fluoride by Gilman and johnston. The blocked-dislocation theory and the experiments that bear on it have been summarized by Mott.18 One of the strong points of the blocked-dislocation theory is that it can explain the grain-size dependence of the fracture stress in a natural way. However, Low9 has pointed out that the theory is not satisfying when it is considered quantitatively. Gilman10 also has criticized the theory and presented an alternative interpretation of the relation between fracture stress and grain size. Since the blocked-dislocation theory is not the only theory that can explain in the grain-size effect, it is necessary to find other evidence either to support or deny it. In this investigation the following points were studied: 1) If blocked dislocations normally cause fracture, then the fracture stress ought to be very high in the absence of plastic glide. Is it? 2) If dislocations must be blocked in order for metals to fracture, then certain types of grain

Jan 1, 1959

For. the year ending February, 1917 PRESIDENT L. D. RICKETTS,1 NEW YORK, N. Y. PAST PRESIDENTS BENJAMIN B. THAYER,1 NEW YORK, N. Y. WILLIAM L! SAUNDERS,2 NEW YORK, N. Y. FIRST VICE-PRESIDENT SIDNEY J. JENNINGS,1 NEW YORK, N., Y. TREASURER GEORGE C. STONE,1 NEW YORK, N. Y SECRETARY EMERITUS ROSSITER W. RAYMOND, NEW YORK, N. Y. SECRETARY BRADLEY STOUGHTON, NEW-YORK, N. Y.

Jan 2, 1917

For the year ending February, 1917 PRESIDENT L. D. RICKETTS,1 NEW YORK, N. Y PAST PRESIDENTS BENJAMIN B. THAYER 1 NEW YORK, N. Y. WILLIAM L. SAUNDERS,2 NEW YORK, N. Y. FIRST VICE-PRESIDENT SIDNEY J. JENNINGS,1 NEW YORK, N. Y. TREASURER GEORGE C. STONE,1 NEW YORK, N. Y. SECRETARY EMERITUS ROSSITER W. RAYMOND, NEW YORK, N. Y SECRETARY BRADLEY STOUGHTON NEW YORK, N. Y.

Jan 10, 1916

For the year ending February, 1916 PRESIDENT WILLIAM L. SAUNDERS,1 NEW YORK, N. Y. PAST PRESIDENTS CHARLES F. RAND,1. NEW YORK, N. Y. BENJAMIN B. THAYER,3 NEW YORK, N. Y. FIRST VICE-PRESIDENT PHILIP N. MOORE,1 ST. Louis, Mo. TREASURER GEORGE C. STONE,1 NEW YORK, N. Y. SECRETARY EMERITUS ROSSITER W. RAYMOND, NEW, YORK, N. Y. SECRETARY BRADLEY STOUGHTON; NEW YORK, N. Y.

Jan 10, 1915

For the year ending February, 1917 PRESIDENT L. D. RICKETTS,1 NEW YORK, N. Y. PAST PRESIDENTS BENJAMIN B. THAYER,1 NEW YORK, N. Y. WILLIAM L. SAUNDERS,2 NEW YORK, N. Y. FIRST VICE-PRESIDENT SIDNEY J. JENNINGS1 NEW YORK, N. Y. TREASURER GEORGE C. STONE,1 NEW YORK, N. Y. SECRETARY EMERITUS ROSSITER W. RAYMOND, NEW YORK, N. Y. SECRETARY . BRADLEY STOUGHTON NEW YORK, N. Y.

Jan 5, 1916

For the year ending February, 1916 PRESIDENT WILLIAM L. SAUNDERS,1 NEW YORK, N. Y. PAST PRESIDENTS CHARLES F. RAND,1 NEW YORK, N. Y. BENJAMIN B. THAYER,3 NEW YORK, N. Y. FIRST VICE-PRESIDENT PHILIP N. MOORE,1 . . . ST. Louis, Mo. TREASURER GEORGE C. STONE,1. NEW YORK, N. Y. SECRETARY EMERITUS ROSSITER W. RAYMOND, NEW YORK, N. Y. SECRETARY BRADLEY STOUGHTON NEW YORK, N. Y.

Jan 11, 1915

For the year ending February, 1917 PRESIDENT L. D. RICKETTS,1 NEW YORK, N. Y. PAST PRESIDENTS BENJAMIN B. THAYER,1 NEW YORK, N. Y. WILLIAM L. SAUNDERS,2 NEW YORK, N. Y. FIRST VICE-PRESIDENT SIDNEY J. JENNINGS,1 NEW YORK, N. Y. TREASURER GEORGE C. STONE,1 NEW YORK, N. Y. SECRETARY EMERITUS ROSSITER W. RAYMOND, NEW YORK, N. Y. SECRETARY BRADLEY STOUGHTON, NEW, YORK, N. Y.

Jan 7, 1916

For the year ending February, 1916 PRESIDENT WILLIAM L. SAUNDERS,1 NEW YORK, N. Y. PAST PRESIDENTS CHARLES F. RAND,1 NEW YORK, N. Y. BENJAMIN B. THAYER,3 NEW YORK, N. Y. FIRST VICE-PRESIDENT PHILIP N. MOORE,1 ST. Louis, Mo. TREASURER GEORGE C. STONE,1 NEW YORK, N. Y. SECRETARY EMERITUS ROSSITER W. RAYMOND NEW YORK, N. Y. SECRETARY BRADLEY STOUGHTON, NEW YORK, N. Y.

Jan 1, 1916