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By F. G. Tahmoush, N. J. Grant, E. P. Abrahamson

The effect of grain size on the brittle -ductile transition temperature of pure iron and three dilute Fe-W alloys has been investigated by slow bend tests. The brittle-ductile transition temperature for pure iron increased with increasing grain sizes from 8000 to 500 grains per sq mm where the transition temperature then decreased with further increase in grain size. The dilute additions of tungsten lowered the transition temperature for fine grain sizes, suppressed a reversal of the curve in the coarse grained portion, and raised the transition temperature for this region. The frequency of twin occurrence increased with increasing grain size and decreasing temperature. The object of the present investigation was to re-examine the effect of grain size on the brittle -ductile transition of pure iron and several dilute Fe-W alloys. Current literature normally presents a simple relationship between grain size and the brittle-ductile transition temperature, namely, that the transition temperature increases with increasing grain size. Heslop and etch' have studied the transition temperature of mild steel by V-notch Charpy impact tests for the grain size range between 200 and 6000 grains per sq mm. The result was a linear plot of In 1-1/2 vs brittle-ductile transition temperature, where 1 is the grain diameter. Recent experiments by sipos2 revealed the possibility of a reversal in the slope of the grain size vs transition temperature plot for pure iron; however, his investigation was limited in scope, and the data obtained were insufficient to permit a definitive curve. The present investigation was undertaken in an effort to confirm or extend the grain size effect observed in iron by Sipos. PROCEDURE All alloys were vacuum induction melted, using 99.95 pct Fe containing 0.03 pct 0 and 0.004 pct C. Four ingots were made, ranging from pure iron to iron with 0.035 pct W. The chemical composition of each alloy, after processing, is given in Table I. The four alloys were prepared as 45 lb heats and cast into 4 in. diam by 16 in. molds. They were then extruded into 3/4 in. rods at 1800oF. Specimens for chemical analysis, taken from various positions along the rods, revealed no variation in tungsten content along the length. The extruded rods were reduced to 0.156 in. diam stock by a series of cold swaging operations involving intermediate vacuum annealing treatments. This procedure yielded a final cold reduction in area ranging from 10 to 90 pct. The swaged rods were chemically cleaned, cold pressed to a cross section of 0.10 by 0.18 by 1.0 in. long (2.54 by 4.73 by 25 mm). The specimens were wrapped in iron foil and vacuum sealed (10-4 mm Hg) in quartz. Various heat treatments at temperatures from 700" to 1300oC were utilized to produce grain sizes from 8000 to 1 grain per sq mm. Grain sizes were determined by measuring the average area of grains in a polished section. In specimens with grain size greater than 20 grains per sq mm, the total number of grains in the cross section was counted and then divided by the area to yield grains per sq mm. Grain size was measured both for longitudinal and transverse cross sections. The average of the two measurements was plotted vs transition temperature. An Instron Table Model testing machine was used to determine the transition temperature of specimens tested in three point horizontal bending. The specimen was supported by two 1/4 in. dowels one in. apart. Bending was accomplished with a push rod, the end of which had an 1/8 in. radius. The head speed was 50 in. per min. Temperatures were established through the use

Jan 1, 1963

By G. W. Form, W. A. Spitzig

The effects of hydrogen and vacuum shtering treatments on the physical and mechanical properties of arc plasma-sprayed tungsten were inuestigated. Temperatures examined ranged from 3000" to 4000°F in vacuum and 2000" to 3000°F in hydrogen for both single and duplex sintering cycles. Densities of 92 pct of theoretical density were obtained when a long-time hydrogen treatment at 2000°Fpreceded sintering in vacuum at 4000°F for 4 hr. This cycle also produced the highest ualues for modulus of rupture and bend angle. The results of this investigation point out the desirability of using a low-temperature long-time hydrogen treatment prior to a high-temperature vacuum sinter for arc plasma-sprayed tungsten. ADVANCES in the development of arc plasma-generating equipment have provided a high-temperature heat source that makes the fabrication of tungsten shapes possible by a metallizing process. Tungsten in the as-sprayed condition is very brittle. It has a density between 80 and 85 pct of theoretical density, a lamellar structure with elongated pores, and a high interstitial impurity content. To improve these properties, sintering treatments can be applied to the as-sprayed material, similar to those used for the densification of compacted tungsten powder. However, in view of the differences in the density and microstructure of as-sprayed tungsten as compared with compacted tungsten, responses to sintering were expected to be different. EXPERIMENTAL PROCEDURES The tungsten powder used in this investigation had a particle size varying from 3 to 13 p with an average diameter of 8p. The impurity level was less than 0.1 pct. The arc plasma spraying was done with an F-40 Thermal Dynamics Corp. plasma jet. Spraying was performed in air and thus required cooling of the substrate by an air blast in order to minimize oxidation. The spraying parameters employed in the fabrication of all specimens are listed below: Power input, kw 12 Arc-gas flow, cfh 95N2 + 5H2 Powder feed rate, g per min 33 Powder carrier gas flow, cfh ION, Spray distance, in. 3 Traverse rate, in. per min 30 Mandrel speed, rpm 100 Nozzle orifice, in. 7/32 These values of the spraying parameters correspond to optimum conditions ascertained in a previous study. Sintering was conducted at 3000°, 3500, and 4000°F in vacuum (< 0.1 Hg), and at 2000 and 3000°F in hydrogen. Duplex sintering treatments investigated are listed in Table I together with the designations that will be used for reference throughout this paper. The samples were fabricated by spraying onto a copper mandrel which was removed prior to sintering. The specimens used for the sintering analyses had the shape of small hollow truncated cones 1 in. high with an inside diameter varying from 0.500 to 0.125 in. and a wall thickness of 1/8 in. Specimens for bend testing were taken from hollow hexagonal prisms 1-1/2 in. high with a 1-in. diam across the flats and a wall thickness of 1/8 in. The bend-test specimens were ground to the dimensions 0.085 by 0.350 by 1-1/2 in. Prior to bend testing 0.0025 in. of stock was removed from each surface by electro-polishing. Density measurements were made by the water-displacement method. In addition, a porosimeter was used to determine the amount of interconnected porosity for representative samples. Strength and ductility were determined from recorded values in transverse bending using a cross head speed of 0.020 in. per min. The load was applied at the midpoint of a 1-in. span. The deflection data reported herein refer only to the plastic portion of the total deflection. RESULTS AND DISCUSSION The as-sprayed samples had a density corresponding to 83 pct (l pct) of the theoretical density of tungsten. Fig. 1 shows a representative as-sprayed tungsten structure.

Jan 1, 1964

By H. Herman, M. E. Fine

Kinetics of reversion and reformation of GP I were studied resistometrically in Al-1.7 at. pct Cu. The reversion process is over in roughly 1/2 minute at 205 "C irrespective of the amount of primary aging. After reversion the occurrence of an incubation time before reaging begins has been substantiated. The reaging kinetics is drastically accelerated by plastic deformation to the specimen. An incubation time is observed only if the specimen is aged before reversion. The incubation time and the effect of plastic deformation indicate that nucleation of GP I is heterogeneous. Simple clusters of copper atoms apparently do not act as nuclei for GP I. AFTER quenching aluminum-rich copper from the solid solution range, Guinier-Preston zones of the first kind, GP I, form very rapidly at room temperature. The rate, largely controlled by the concentration of vacancies, is initially most rapid1 (that is, at the time of the first measurement: 1/2 min) and decreases with time. The nucleation is thought to be athermal. If after aging for several days the GP I is dissolved by reversion at 205°C, according to measurement of Young&apos;s modulus an incubation period is observed before GP I begins to form on subsequent aging.2 Yet if the reversion is carried out immediately after quenching, both resistivity3 and modulus changes2 show no incubation effect. The zones which form after reversion have the same structure as those which form after the quench.4 Because of entropy considerations and also the short diffusion time, the solid solution after reversion, 2 min at 205°C, is probably more highly clustered than at the original solution treating temperature, 520" to 550°C. It appears most reasonable to associate with nucleation the incubation time observed on reaging after reversion. A simple cluster of copper atoms, many of which are presumed to be present after reversion, is then not a sufficient nucleus for GP I; a GP I nucleus must contain something in addition to a cluster of copper atoms. The purpose of the present note is to give some additional experimental information concerning the incubation time and rates of reaging after reversion. The existence of the incubation time has been verified by measurement of another property, the electrical resistivity. Acceleration of reaging after reversion by plastic deformation has also been investigated. In acl.dition, the kinetics of the reversion process itself was studied. EXPERIMENTAL Electrical resistance was measured by the poten-tiometric four probe method. The 1.7 at. pct Cu alloy was furnished by the Aluminum Co. of America in the form of 1/2 in. rod. The major impurities reported by Alcoa were Fe (0.002 wt pct), Si (0.003 wt pct), and Mg (0.001 wt pct). Specimens for measuremenl of resistance were prepared by rolling to 0.010 in., cutting 2 by 0.2 in. pieces, rolling the middle pclrtions of these to 0.005 in., and splitting the 0.010 in. sections up to the reduced central section to form current and potential leads. Aluminum extension wires insulated with ceramic tubes were spot welded to the leads. The specimen was supported by the lead wires. The whole specimen assembly was annealed at 500" C in an air furnace for more than 12 hr and then aged at room temperature. This was done to assure quick and complete resolution during subsequent solution treatments. These were carried out in Houghton&apos;s "430 Temper Salt" at 520&apos;C for 1 hr. Unless otherwise specified, quenching was accomplished by quickly transferring the specimen from a salt pot to 25°C water. Aging was carried out in a 3 liter dewar of distilled water, rotated and stirred. The temperature was controlled to +0.01°C with a thermomercurial regulator in conjunction with a transistorized relay

Jan 1, 1962

By G. C. Wallick, J. S. Aronofsky

This paper presents an experimental verification of numerical solutions of the differential equation describing the transient flow of an ideal gas through a porous material including gas slip effects. Several experiments previously proposed by one of the authors are described together with the correlation of the experimental results with the numerical solutions. Excellent agreement is shown between experiment and theory, thus demonstrating the validity of both the basic assumption made in the derivation of the differential equation and of the numerical solutions of the differential equation. INTRODUCTION In a recent paper,&apos; one of the authors has discussed a numerical solution of the differential equation describing the unsteady flow of an ideal gas through a porous material. This paper was primarily concerned with the effect of gas slip on the flow behavior. In steady state measurements, Klinkenberg2 and others have observed that the apparent gas permeability Kn of a porous material may be expressed as a linear function of the reciprocal average pressure 1/P of the form, ka = b + m/P........(1) where the intercept b is a constant for a given porous material and the slope m is a constant for a given porous material-gas combination. Aronofsky1 assumed that Equation (1) could be used to describe transient flow if P was replaced by the average pressure in an infinitesimal volume element. A number of numerical solutions of the resultant differential equation were presented and specific flow experiments were proposed as a means of testing the numerical solutions. The purpose of the present paper is to describe the results of several of these experiments and the correlation of the experimental data with the results of the numerical analysis. Reference should be made to the previous paper&apos; for details of the mathematical and numerical analysis. EXPERIMENTAL PROCEDURE A simplified schematic drawing of the experimental apparatus is shown in Fig. 1. An 8.89 cm diameter limestone core of length L = 14.82 cm was mounted in a conventional rubber sleeve permeameter cell. The external sleeve pressure in this cell was maintained equal to 500 psig during all experimental tests, thus permitting only longitudinal flow through the core. One end of the core, X = L, was connected to an adjustable cavity of volume V as well as a pressure gauge or manometer. The other end of the core, X = 0, was connected to a Nullmatic pressure regulator which was in turn connected to a nitrogen cylinder or vacuum pump. In each experiment, the core and adjacent dead volume were charged with nitrogen to a uniform gas pressure P1. The pressure at X = 0 was then suddenly raised or lowered to a constant pressure P, and the resulting pressure buildup or pressure decline at X — L was recorded as a function of the time. The porosity + and the permeability constants m and b were determined using the transient method which was suggested by the results of the numerical analysis and which was described in the earlier paper.&apos; The following average values for these constants were obtained as a result of 19 separate evaluations: 171 -0.259 2 0.005 md-atm; b = 0.374 5 0.008 md; and F = 0.098 ± 0.005*. It should be noted that in order that transient phenomena will be slow enough to be observed conveniently, it is desirable to use a porous material of very low permeability, e.g., less than I md. Moreover, it is in this low permeability range that the gas slip effects are most significant. Thus, such a low permeability sample is very suitable for use in an experimental verification of the numerical solutions previously described.

Jan 1, 1955

By E. I. Alessandrini, A. U. Seybolt

Selective oxidation (preferential oxidation of a single alloy component) can be an important oxidation mode in the case of alloys such as Si-Fe, Al-Fe, and so on, when heat-treating in atmospheres of low oxygen potential. It was the purpose of this work to identify the oxide films formed on iron containing 31/4 pct Si at low oxygen potentials, and to make some observations on the H2O/H2 ratios required to form them. EXPERIMENTAL METHOD HYDROGEN of varying water content offers a very convenient method of establishing a wide range of oxidizing power, or oxygen potential. The method chosen to provide a desired H2O/H2 ratio was to nearly saturate hydrogen at room temperature by bubbling the gas through water at room temperature, and then to wring out the excess water by passing the wet gas through a long glass spiral immersed in a refrigerated liquid at a desired dew point. After oxidation, the samples were examined by electron diffraction in order to identify any film which might be present. PREPARATION AND TREATMENT OF SAMPLES The samples were prepared from a Si-Fe alloy made in the laboratory using electrolytic iron and 96 pct ferro-silico11, vacuum-induction melted, hot-rolled then cold-rolled to 0.015-in. thickness. After the cold-rolling the samples were annealed at 1000°C. Transmission Laue X-ray patterns showed very little evidence of preferred orientation, but it is likely that a weak texture could have escaped notice. The chemical analysis was as follows: 3.34 Si, 0.01 Al, 0.001 0, 0.006 C, 0.002 N. Before each sample was oxidized, it was polished through 4/0 emery paper, cleaned and dried using benzene, carbon tetrachloride, acetone, absolute alcohol, and ether. The method of oxidizing the samples was as follows: Samples about 1/2 by 1 by 0.015 in. were held in the upper, cool part of a vertical vacuum furnace until the desired temperature was established in the furnace, Fig. 1. The sample was then lowered into the uniform hot zone where it was heated quickly to the desired temperature, and subjected to hydrogen of controlled moisture content (dew point) as mentioned previously. Temperatures from 400" to 1000°C were used, and dew points from room temperature to —78°C were explored. In general, the runs lasted about 6 hr, but a few runs were of different duration, as will be indicated later. After the predetermined period of time had elapsed, the specimens were withdrawn by the hollow stainless steel-quartz holder to a cool zone at the top of the furnace. EXPERIMENTAL RESULTS The results are summarized in Table I. Most of the electron-diffraction patterns were obtained by glancing-angle reflection, but in a few cases it was possible to strip the oxide films from the surface by a total immersion in a 3 pct bromine-methanol solution. Some of the thinner stripped films yielded quite satisfactory transmission patterns. However, both diffraction techniques yielded the same results; the patterns while most frequently showing a (low) tridymite, also showed a (low) cristobalite in some cases. A few patterns showed evidence of both phases. Because of the known nonequilibrium behavior of silica, it is not surprising that both forms of silica could coexist on one sample. It was noted that at fairly low dew points such as —40°C, there was a tendency for diffuse diffraction rings, suggesting a very small crystallite size. Also some subsequent experiments to be reported later show that thin silica films can be amorphous.

Jan 1, 1959

By Jean Howard

ThE formation of the (100) [001) texture in 3-1/4 pct Si-Fe strip was first reported by Assmus ef a1.l in 1957. Since then much experimental work has been carried out with a view to establishing the mechanism involved. The papers cited above state that the (100) [001] texture was developed in strip rolled from material melted and cast in vacuum. (The impurity content of the ingot is reported as 0.005 pct.) The present note records that similar results can be obtained in material processed by powder metallurgy. A processing schedule is described.which enables the texture to be formed in strip up to 0.010 in. thick, but there seems no reason why this should not be achieved in thicker strip, provided that large grains are developed after sintering. The materials were prepared from Carbonyl Iron Powder Grade MCP (particle size 5 to 30 p) of the International Nickel Co. (Mond) Ltd. The powder contains about 0.15 pct 0, 0.01 pct C, 0.004 pct N, <0.002 pct S, $0.005 pct Mg and Si, and 0.4 pct Ni— that is, it is substantially free from metallic impurities other than nickel, which is thought to be unimportant in the present work. The silicon powder was 99.9 pct purity, or material of transistor quality (ground in pestle and mortar). The mixed powders (3-1/4 pct Si to 96-3/4 pct Fe) are heated in hydrogen at 350" and 650°C to deoxidize the iron before sintering loose at temperatures between 1350" and 1460°C (depending upon the ultimate thickness of strip required) for up to 24 hr. The object of the high-temperature sinter is to develop a large grain size at this stage. Alternatively, the loose sintering can be done at a lower temperature followed by rolling or pressing and then annealing at temperatures between 1350" and 1460°C. Both methods produce large grains, which remain large throughout the process. The compact is then hot-rolled to approximately 1/8 in. with high-temperature interstage anneals if necessary. This step is taken to avoid intercrystalline cracking which would occur if the material of such large grain size were cold-worked. The bar is then annealed at 1050°C and reduced to its final thickness by approximately 50-pct reductions and 1050°C interstage anneals. Throughout the process the dew point of the hydrogen furnace atmosphere is maintained at about -40°C. Samples were annealed in hydrogen at various temperatures and times. Secondary recrystalliza-tion to (100) [001] was developed on the thinner material (i.e., up to 0.002 in.) by annealing in hydrogen at 1050" to 1200°C with a dew point of - 40°C or in vacuum (10-5 Torr) at 1050°C. With the thicker materials (i.e., up to 0.010 in.) the best results were obtained by annealing in hydrogen at 1200°C with a dew point of - 55°C. Complete secondary recrystal-lization to (100) [001] textures was obtained. Above these temperatures secondary recrystallization to (110) [001] tended to develop. The final annealing of samples was normally carried out with the samples placed between recrystal-lized alumina plates, but some experiments were performed with the samples suspended so that their surfaces were not in contact with anything except hydrogen, and these were equally successful in developing secondary crystals. An approximate determination of the proportion of material (before secondary recrystallization took place) having crystals with the (100) or (110) planes in or near the rolling plane showed that 11 pct of the sample had (100) and 16 pct (110). The method used for the determination is described below. A sample was annealed at a temperature just below the secondary recrystallization temperature and etched to reveal the (100) planes. The approximate area covered by crystals having (100) or (110) in or very near the surface was measured on the screen of a Vickers projection microscope. This was repeated for twenty positions chosen at random and a mean of the results calculated. The main hindrance to developing the secondary crystals in the thicker materials was the difficulty of obtaining a large enough initial primary grain size before secondary recrystallization. This was overcome by increasing the particle size of the silicon powder used. During the course of the work, it had been observed that the larger the grain size after sintering the more likely it was that the material would be successful in developing secondary crystals at a later stage. An experiment was therefore carried out to determine whether the material with the larger grain was more successful in developing secondary crystals due to the large grain produced at the sintering state per se or whether it was due to the greater reduction of silica brought about when the sintering temperature was raised in order to increase the grain size. A comparison was made between two compacts, one of which was made with silicon powder of 60 to 100 mesh, the other with silicon powder which was finer than 200 mesh. F?r this experiment, use was made of a phenomenon previously observed that the larger the particle size of the silicon powder employed in making a compact, the larger is the grain size of the compact. The silicon powder was ground

Jan 1, 1964

By D. C. Sisti

A technical evaluation of actual performance of the preparation facilities at Beaver Consolidated Coal Co.&apos;s Stinson plant is presented, with special emphasis on sulfur reduction in 1-1/2 x 3/8 in., 3/8 in. x 28 mesh, and 28 mesh x 0 size fractions. Evaluation of the heavy medium section of the plant and the treatment of the 28 mesh x 0 coal is included. Design criteria considered for sizing and selection of equipment required to process 1-3/4 million tpy of raw coal on coals of divergent washability characteristics are summarized.

Jan 1, 1976

By P. Shahinian, R. L. Stegman, M. R. Achter

Creep strength has been determined as a function of oxygen pressure for nickel at 510" and 600°C. Creep-rupture life drops from its highest value at the ultimate vacuum of 10-7 torr to a high pressure plateau of nearly constant life which, at 600°C, commences at torr. This behavior is described in terms of a model that relates surface gas adsorption and the generation of fresh crack surfaces. In a calculation based a this model the predicted pressure beyond which the creep strength should not decrease further has been found to agree well with the observed value. The introduction of oxygen during creep in vacuum was found to cause a prompt rise of the creep rate. The magnitude of the environmental effect was much less than generally observed in fatigue and this is attributed to the diffarent crack morphologies in creep and fatigue. GASEOUS environments are known to affect creep resistance adversely1-5 but the effects have received less attention than the much larger ones in fatigue. At low temperatures it has been shown for nickel that the creep rates are faster and the rupture lives are shorter in air than in vacuum and that these environmental effects can be correlated with faster crack growth rates in the reactive environment.&apos; In support of a mechanism of gas adsorption at the crack tip to explain the above effects, a calculation based on kinetic gas theory showed that surface coverage by gas was not as rapid as the exposure of fresh metal at the crack tip in the ultimate vacuum but was in air.7 In fatigue a number of investigations have demonstrated that the reduction of life with gas pressure usually follows a step curve with most of the reduction occurring in a transition range at intermediate pressures and little or no change at high and low pressure.8 There have been no studies, however, in which creep strength has been determined as a function of reactive gas pressure to see whether similar effects would be found. This investigation was undertaken to study the kinetics of the environmental effect in the creep of nickel. EXPERIMENTAL PROCEDURES The environmental creep apparatus was constructed to minimize many of the experimental conditions which can cause scatter in data. Dead weight loading is employed and weights are contained within the environmental chamber to eliminate bellows and the necessity for compensation for gas pressure changes. Elongation over the specimen gage length is recorded from a Riehle Model DV Controlled Environment Extensometer which provides readout to 2.5 x 10- in. Temperature is monitored and controlled from a thermocouple at- tached to the specimen gage length to +0.5oC or better. The freon trapped oil diffusion pump vacuum system included an auxiliary liquid nitrogen trap and, with a wide range variable conductance leak valve, pressures from the ultimate vacuum of 10"7 to l03 torr of any desired gas are obtainable. Pressure is measured by means of a hot filament ionization gage below 10"3 torr and a NRC Model 530 Alphatron Vacuum Gauge above 10-3 torr. The oxygen, which was leaked into the environmental chamber, was an Aviator&apos;s Grade of 99.5 pct purity with a dew point of -80°F. Analysis of the nominal 99.8 pct Ni showed the following percentages of major impurities: 0.02 C, 4.01 Mn, 0.005 Si, 0.01 Cu, 0.02 Fe, and 0.034 Mg. Cylindrical specimens were machined with a 0.180

Jan 1, 1970

By G. R. Wilms

A study has been made of the structural changes in polycrystalline high purity aluminum during the tertiary stage of creep under conditions of constant tensile load. It appears that there is no basic modification in the particular mechanism of deformation that characterized the preceding secondary stage of creep, but that the changes in crystalline structure produced during the tertiary stage are only a consequence and not a cause of the accelerated strain. Intercrystalline fissures were observed on entry into the tertiary stage, and these might supplement the accelerated rate of strain owing to local stress concentrations. There is evidence that the formation of these fissures may be associated with the presence of surface imperfections, and it is suggested that a more generalized treatment of the results may explain certain creep characteristics of commercial alloys. IN previous work&apos;-4 a study was made of the changes produced when specimens of annealed aluminum were deformed at various temperatures and rates of strain, especially under conditions leading to creep under constant tensile load. It was shown that, as the temperature was increased or as the rate of strain was decreased, elements of the substructure produced within the grains became coarser, and with the strain rate constant at a given temperature, their size tended to an equilibrium value. The preliminary process of the breaking down of the grains into a substructure was identified with primary creep.&apos; The subsequent equilibrium, condition was associated with secondary creep. The question then arose whether the tertiary stage corresponded to any further significant change in the substructure. The question is also of interest in view of the opinion, expressed for instance by Andrade,5 that the tertiary stage is merely an accelerated rate of strain due to the reduced area of section of a specimen under continuous tensile load, and the other opinion, as suggested by the observation by Sully, Cale, and Willoughby6 of a tertiary stage in com-pressive loading, that this third stage is a real effect in its own right. The object of this paper is to record some observations on the tertiary stage of high purity aluminum. Experimental Procedure The material was aluminum of 99.98 pct purity as previously used. The specimens had a rectangular section of l/8 x l/2 in., and extensions were measured over a 1 in. gage length. After machining to shape, the specimens were annealed to give a standard grain size of 0.2 mm and then electropolished. The general procedure involved metallographic and X-ray diffraction examination at progressive stages of elongation (marked by arrows on the curves shown in Figs. 1 and 2), the specimen being extended to fracture under constant load at a given temperature. The X-ray tests were made by the back-reflection method from a stationary specimen, using CoK radiation. The longer edge of the micrographs in the paper corresponds to the direction of applied stress. Results The previous work showed that, in the secondary stage of creep in aluminum, three basic types of structure could be developed according to the temperature and rate of strain. These were: 1—slip, which predominated at the lower temperatures and higher rates of strain and produced the finest and least perfect substructure; 2—cell structure, which superseded slip as the temperature was raised and the rate of strain decreased and which was characterized by a coarser and more perfect structure and an absence of slip lines; and 3—a stage termed "boundary microflow," which predominated at still higher temperatures and lower rates of strain when the cell size had increased and become comparable

Jan 1, 1955

By W. H. Bassett, J. C. Bradley

In their paper on the directional properties in cold-rolled and annealed commercial bronze,&apos; Phillips and Samans suggest that cupronickel, under distinctly different treatments, shows both "45" ears" and "90" ears. Fig. I shows the ears on some cupronickel cups made some 17 years ago for bullet jackets for small arms ammunition. In this case the material heated to 425° C. had "45" ears, while that annealed at 950°C. showed long "90" ears" when drawn with the same tools. The method of cupping, the shape of cupping tools, etc., were found to have very little influence on the earing tendency, but the deeper the cup was drawn, the higher the ears would be. Method of Manufacture Cupronickel cast bars were 1 in. thick. Ordinarily, they were rolled with numerous passes to a thickness of 0.4 to 0.2 in., according to conditions. They were then given a single intermediate anneal, and rolled to finish thickness, frequently 0.032 in. After a last anneal the material was cupped with a "cut and draw" operation. Progress of this is indicated in Fig. 2, illustrating five different stages at which the drawing

Jan 1, 1933

By E. C. Harder

INTRODUCTION FEW mineral deposits have in recent years attracted such general and Widespread attention as the Brazilian iron-ore deposits, due mainly to the quantities of rich ore occurring here, in contrast to the ever-decreasing grade of ores shipped from many large producing iron-ore districts of the world. The general average grade of the iron ores shipped from the Lake Superior district&apos; has decreased to approximately 50 per cent., natural, in recent years. The Rubio ore of Bilbao, Spain,2 in 1890 averaged 55.5 per cent. metallic iron, dried; in 1902, 52.8 per cent., While at the present time a large proportion of the ores shipped from Bilbao are obtained by reworking the old dumps. In northern Sweden, where large magnetite deposits have only in recent years been extensively developed, selective mining is even now necessary in order to obtain high-grade Bessemer ores. During the last two years the iron ores of Chile have attracted much attention on account of the activities of the Bethlehem Steel Co. and others in the Chilean iron-ore region. Many of these ores are of good grade, yielding 67 and even 68 per cent. metallic iron, but judging from the Writer&apos;s observations in this region a large proportion of them Will be found to he of non-Bessemer grade. The most important variety of iron ore in Brazil is hard, dense to specular hematite, occurring in Minas Geraes. A large number (89) of analyses of this type of ore have been averaged, 3 giving the following composition: Per Cent. Iron 69.65 Phosphorus 0.0125 Silica 0.24 Combined H,0 0.38

Jan 10, 1914

By Colin C. Rae

The absence of paraffin and other oil hydrocarbons in the soil although they are concentrated in extensive deposits in some localities, the common distribution of plant remains through many formations that are not productive for oil, and many other factors, seem to indicate the existence of an intermediate organic compound between the complex plant compounds and the petroleum hydrocarbons; and much evidence points to the humus acids or associated organic compounds, which are probably collected by surface waters and concentrated in certain areas by means of precipitation by electrolytes, which would be contained in sea water or possibly in various inland seas or lakes. Present-day Evidence There are many present-day evidences of the association of petroleum with humus acids. Binney, in 1912, made observations without explanations on the peat mosses of Down Holland, England, where he found petroleum being formed by decomposition in the presence of an infiltration of sea water. The analysis of a typical peat will show its relationship to the humus acids under consideration. Sample No. 1, SamplE No. 2. PXr Cent. PER CENt. Water......................... 20.0 29.6 Ash.......................... 3.0 3.05 Fiber.......................... 47.0 54.95 Humus acids................ 30.0 12.50 J. D. Haseman and others have noted the association of asphalt and hydrocarbons with the swampy, boggy areas, particularly adjacent to the sea. Many of the rivers carry much humus acid in solution, and some tropical rivers carry in the aggregate millions of tons of humus each year. The amount of humus is a variable factor, depending on climatic conditions, and on the salts and alkalies present in the water, also on the density and temperature.

Jan 1, 1923

By Colin C. Rae

The absence of paraffin and other oil hydrocarbons in the soil although they are concentrated in extensive deposits in some localities, the common distribution of plant remains through many formations that are not productive for oil, and many other factors, seem to indicate the existence of an intermediate organic compound between the complex plant compounds and the petroleum hydrocarbons; and much evidence points to the humus acids or associated organic compounds, which are probably collected by surface waters and concentrated in certain areas by means of precipitation by electrolytes, which would be contained in sea water or possibly in various inland seas or lakes. Present-day Evidence There are many present-day evidences of the association of petroleum with humus acids. Binney, in 1912, made observations without explanations on the peat mosses of Down Holland, England, where he found petroleum being formed by decomposition in the presence of an infiltration of sea water. The analysis of a typical peat will show its relationship to the humus acids under consideration. Sample No. 1, SamplE No. 2. PXr Cent. PER CENt. Water......................... 20.0 29.6 Ash.......................... 3.0 3.05 Fiber.......................... 47.0 54.95 Humus acids................ 30.0 12.50 J. D. Haseman and others have noted the association of asphalt and hydrocarbons with the swampy, boggy areas, particularly adjacent to the sea. Many of the rivers carry much humus acid in solution, and some tropical rivers carry in the aggregate millions of tons of humus each year. The amount of humus is a variable factor, depending on climatic conditions, and on the salts and alkalies present in the water, also on the density and temperature.

Jan 1, 1923

By Frank Foote, Willard L. Bruner, Eric R. Jette, Y. New york

The alloys of gold and iron were investigated in 1907 by Isaac and Tammann,l who determined the thermal diagram for the entire system by thermal analysis and microscopic examination. They also reviewed the previous literature. Since that time the present authors have been able to find only two additional references. Guertler and Schulze2 examined the electrical resistance of iron alloys containing up to 40 per cent by weight of gold between 0" and 200" C.; the alloys were in the form of wires. The main result of this work was to confirm the solid solubility limit found by Isaac and Tammann; namely, about 20 per cent Au. More recently, Shih3 has examined the magnetic properties of gold alloys containing up to 10 weight per cent iron and particularly the range below 5 per cent. The alloys in the lower range were found to be paramagnetic; the 10 per cent alloy was ferromagnetic. The present investigation was undertaken to determine the solid solubility limits at various temperatures, particularly below the a-y transformation point of iron, since these solubilities are of some importance in connection with the working of the alloys in the manufacture of certain "grey" and "blue" golds. Materials and Methods The gold was obtained from the U. S. Metals Refining Co. and contained 99.99+ per cent Au. The electrolytic iron had been annealed in hydrogen and contained impurities as follows: P, 0.035; Si, 0.001; S, C, Mn, Cu, each 0.01 per cent. Weighed quantities of the two metals were placed in small crucibles lined with pure sintered MgO; a saturated solution of magnesium nitrate

Jan 1, 1934

By F. Louis Grammer

THE difference between blast-furnace gas and ordinary producer-gas is chiefly that blast-furnace gas is richer in CO, and poorer in hydrocarbons and hydrogen, as is shown in Table I. TABLE I.-Volume-Composition of Producer-Gas and Blast-Furnace Gas.. Producer-Gas. Blast-Furnace Gas. Per Cent. Per Cent. (Volume.) (Volume.) CO . 22 to 33 25.5 00., . 6 to 3 13.0 H . . 13 to 7 1.5 CH, 3 to 1.5 0.0 N . 54 to 60 60.0 If natural gas, water-gas, or by-product coke-oven gas be available, blast-furnace gas can be made to resemble very closely in calorific value the average producer-gas by merely mixing in one of these products, which are richer in hydro-carbons and, hydrogen. Blast-furnace gas, however, possesses a virtue which is sometimes absent in producer-gas, especially with coals very high in sulphur-namely, that blast-furnace gas is relatively free from sulphur. In some regions the sulphur in coal is an acute problem, and it is highly desirable to find uses for the products which are specially high in sulphur-content. An advantage would be gained if coal was coked before charging into the gas-producers, but this adds to the expense. Sulphur may be partly eliminated from coal by washing it, the success depending upon the form in which the sulphur occurs, and upon the efficiency of the washer, but it cannot always be removed to the extent desired at most American plants. It is not practicable to remove all the sulphur from producer-gas by washing it, though Mr. Reinhardt, of Germany,

Sep 1, 1908

By George B. Lee

During the two years in which the new reduction-works of the Copper Queen Consolidated Mining Co. have been in operation at Douglas, Ariz., there has developed a remarkable condition in regard to the corrosive action of the water used to cool the jackets of the blast-furnaces. Were it not for the many contradictory features, it might pass as one of the unavoidable troubles due to the composition of the water. This water, obtained from wells 600 ft. deep, is also used in the steam-boilers, and its composition, as shown by the following analysis, does not indicate the presence of any ingredient which would explain the corrosion: Grains Per U. S. Gal. Silica,...........0.861 Iron oxide and alumina,....... 0.223 Calcium carbonate,....... 0.261 Calcium sulphate,................. Magnesium carbonate,........... Sodium and potassium sulphates,..14.850 Sodium and potassium chlorides,.9.732 Sodium and potassium carbonate, . 6.482 32.409 The jackets are made of inner plates 0.5 in. thick and an outer plate # in. thick, with 3/8-in. stiffeners between the inner and outer plates. In from 10 to 12 months the inner plates have been reduced by corrosion to a thickness of from + to & in., while the outer plate in the same time is reduced by less than 1/16 in., and the stiffeners show very little corrosion. The plates are pitted and eaten away in some places more than in others. There is practically no scale found on the jackets, but when cleaned considerable iron oxide is found in the bottoms. With an action so marked, serious trouble would be expected in the boilers, but, on the contrary, a recent inspection by a

Jan 1, 1908

By F. Louis Grammer

The difference between blast-furnace gas and ordinary producer-gas is chiefly that blast-furnace ga,s is higher in CO2 and lower in hydrocprbons and hydrogen, as is shown in Table I. Table I.— Volume-Composition of Producer-Gas and Blast-Furnace Gas. Producer-Gas. Blast-Furnace Gas. Per Cent. Per Cent. (Volume.) (Volume.) CO......22 to 33 25.5 CO2........ 6 to 3 13.0 H...13 to 7 1.5 CH4........ 3 to 1.5 0.0 N..54 to 60 60.0 If natural gas, water-gas, or by-product coke-oven gas be available, blast-furnace gas can be made to resemble very closely in calorific value the average producer-gas by merely mixing in one of these products, which are richer in hydrocarbons and hydrogen. Blast-furnace gas, however, possesses a virtue which is sometimes absent in producer-gas, especially with coals very high in sulphur—namely, that blast-furnace gas is relatively free from sulphur. In some regions the sulphur in coal is an acute problem, and it is highly desirable to find uses for the mine-products which are specially high in sulphur-content. An advantage would be gained if the coal were coked before charging into the gas-producers, but this adds to the expense. Sulphur may be partly eliminated from coal by washing it, the success depending upon the form in which the sulphur occurs, and upon the efficiency of the washer, but it cannot always be removed to the extent desired at most American plants. It is not practicable to remove all the sulphur from producer-gas by washing it, though Mr. Reinhardt, of Germany,

Jan 1, 1909

By Mark J. Klein

The behavior of nitrogen in Cr-0.12 at. pct Y was studied in specimens of varying interstitial concentration and thermal history. It was found that soluble nitrogen can be introduced into this alloy by increasing the concentrations of either oxygen or nitrogen. For low nitrogen concentrations the nitrogen in solution is low relative to that in unalloyed chromium. However, the nitrogen in solution increases with increasing nitrogen concentration, approaching that in unalloyed chromium. When the alloy is supersaturated with nitrogen, the nitrogen precipitates readily from solution as a chromium nitride. The stress -induced relaxation of nitrogen is influenced by internal oxidation or internal nitrification of this alloy. THE addition of small concentrations of reactive elements such as yttrium have been found to enhance the low-temperature ductility of chromium.&apos; However, the mechanism by which the ductility is increased is not known. It has been suggested that this effect is caused by a drastic reduction in the concentration of nitrogen retained in solution and therefore a decrease in the number of dislocations locked by nitrogen, a factor that has been associated with an increase in ductility.1,2 However, a change in the type of interstitial precipitate induced by yttrium could also contribute to enhanced ductility of the alloy, since chromium nitride precipitates appear to be embrittling.&apos; In this regard, it has been shown that yttrium scavenges nitrogen in chromium to form YN,4 thus reducing the embrittling chromium nitride phase. However, the change in nitrogen solubility induced by yttrium and the partition of nitrogen between chromium and yttrium nitrides are not known. The object of this investigation is to study the effect of yttrium on the behavior of nitrogen in chromium to obtain information relevant to the mechanism by which scavengers enhance the ductility of chromium. EXPERIMENTAL PROCEDURES The experimental procedures used in this investigation have been described in detail elsewhere.5,6 Wires of Cr-0.12 at. pct Y, 15 cm in length and 1 mm in diam, were drawn from rods 0.6 cm in diam supplied by the General Electric Co. The grain size of the wires after recrystallization at 1150°C was somewhat nonuniform, varying from 0.006 to 0.06 mm in diam. The interstitial analysis for the wires in ppm by weight was about 160 0, 80 N, 12 C, and <2 H. Heat treatments were carried out after encapsulation of the specimens in quartz tubes containing argon. Changes in interstitial concentrations, or interstitial "loading" as it is termed in this study, were generally accomplished by annealing in oxygen, ammonia or methane at 1150°C. The internal friction was measured using a conventional torsional pendulum enclosed in an evacuated chamber. Electrical-resistivity measurements were made at liquid-nitrogen temperature.

Jan 1, 1967

By Jose A. Ruiz

INTRODUCTION For heterogeneous non-catalytic solid-gas reactions carried out in fluidized bed reactors, nominal bed temperature is an average value between gas and solid. For highly exothermic reactions, actual particle temperature can be up to hundred degrees above termocouple temperature, since heat dissipate at slower rate than heat generation during some steps of transformation. These micro instabilities at particle level can displace thermodynamic equilibrium from the desired phase to others. This effect is important when relatively narrow range of phase stability exists, like in sulphation roasting of sulphides, where bed discharge contains, in addition to the desired sulphate others metastable phases such as basic sulphate and ferrite. For example, for copper-iron sulphide concentration roasted below 680°C, no cupric ferrite is formed, as shown by Jakob et al., therefore the separate Kellogg&apos;s stability phase diagrams Cu-S-O represent the roasting (Fig.l). At temperature above this one, like 760°C for example, phase stability changes from CuSO4 to the basic sulphate Cu0•CuSO4. Solid state reaction between Cu0•CuSO4 and Fe203 also occurs to form cupric ferrite, Cu0•Fe2O3, therefore the Cu-Fe-S-O Kellogg&apos;s phase diagram of Fig. 1 (continuous line) represents this condition of roasting. Although both Cu0•CuSO4 and Cu0•Fe2O3 are metastable phases under normal operating conditions of sulphation roasting(1-10% SO2, 1-10% 02 and 680°C, points A and B,Fig. 1) sulphation of these species and particularly ferrite are slow and limited due to diffusional control. This explain why reactors discharge contains several phases: CuSO4, Cu0•CuSO4, CuO•Fe203 plus small amounts of CuS and FeS due to the baclonixed conditions of fluidized bed reactors. The presence of cuprous ferrite due to reducing conditions inside individual particles also occurs, but in very limited extent at the reaction interface, as it is demonstrated by the low soluble iron levels of calcines. On the other hand, the presence of cupric ferrites can be explained only due to the higher temperature achieved by particles, since below 680°C cupric ferrite formation does not take place. [ ] This phenomena also occurs for others non-ferrous metal sulphides concentrates roasted under sulphation conditions, such as 7n, Co and Ni. Therefore the prediction of discharge composition of fluidized beds is not possible based only on kinetics and mechanistics models alone or purely thermodynamical considerations, since all factors should be integrated to describe the overall phenomena. SINGLE PARTICLE TRANSFORMATION Assuming a first order reaction with respect to the gas and zero for solid, such as

Jan 1, 1984

By P. W. Bakarian

Previous determinationl,2,3 of the texture of magnesium and its alloys have shown only slight variations in the principal features of the structure. This investigation presents pole figures for magnesium and two of its alloys, in which differences of some magnitude will be shown. Schmid and Wassermann have considered the texture of magnesium in analogy with that of zinc—also a hexagonal lattice. Whereas the zinc texture is said to be derived primarily through basal slip and secondarily through {IO2}† twinning, the {102} twinning is considered impossible at the later stages of the rolling in magnesium because of its smaller axial ratio. This state of affairs appears reasonable for pure magnesium, but for alloy textures the situation is more complex. A double orientation similar to that found in zinc has been reported by J. D. Hanawalt,4 and the addition of small amounts of calcium to magnesium and its alloys to produce a double texture was noted by J. C. McDonald.5 The pole figures of this investigation, using an improved X-ray technique, show these various textures. The dependence of directional properties of rolled sheet on modifications of texture is well recognized. Correlation of physical properties with existing texture should be even more significant if quantitative valuations are attached to the various areas on the pole figures. Such a quantitative technique is developed herein. Experimental Method Two alloys were used, besides high-purity magnesium. In each case, the metal was extruded to bars 1/2 in. thick and hot-rolled to a thickness of about 0.075 in. It had been established previously that such a reduction was more than sufficient to eliminate the extruded structure. The rolling proceeded in the same direction as that of the extrusion, without any cross rolling. The temperatures corresponded to normal commercial practice, averaging around 600°F. A unique method of preparing the sample was developed in this work. Instead of using a flat specimen, a stem of the metal was cut out of the rolled sheet in the desired direction (rolling direction) as shown in Fig. I. From a sheet of 0.075 to 0.065-in. gauge, the stem was cut to a square cross section with a jeweler&apos;s saw, rounded with a file and polishing paper to a diameter of 0.060 in. and evenly etched in dilute hydrochloric acid to a diameter of 0.038 + 0.001 in. In this way, a cylinder of the original sheet with its axis in the desired direction was produced. By using this type of specimen for the pin-point pictures, any variance in the absorption of the diffracted beam at the various angular settings of the specimen, was completely eliminated.*

Jan 1, 1942