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By R. G. Garlick, M. Garfinkle

It was observed for several bcc metal crystals that the Knoop hardness anisotropy was dependent essentially on the direction of the lung axis of the indentor alone and not on the plane of indentation. The generality of this observation was tested for an fcc md an hcp metal and an ionic crystal. For cubic crystals, this observation was valid; for the hcp structure, however, the planes of indentation did have an effect on the hardness anisotropy, although this was not nearly as significant as the direction of indentation. Because the direction of indentation is the only significant crystal-lographic parameter necessary to describe the hardness anisotropy, it is possible to represent the anisotropy of single crystals on the standard stereographic triangle. THE commonly observed1, 2 periodic variation of indentation hardness with crystallographic direction on the high-symmetry planes of various single crystals has been inadequately related to the physical or mechanical properties of the crystals examined. In fact, the hardness anisotropy curves for the various planes of a particular metal crystal, as is illustrated in Fig. 1, are uncorrelated and appear in the literature3, 4 as unrelated observations. Attempts to correlate hardness anisotropy curves with specific physical properties can be generally divided into either mechanistic or nonmechanistic approaches. A nonmechanistic approach would be to devise a mathematical expression that could describe the various hardness anisotropy curves. Such a relation could then be compared with the known anisotropy of various physical properties to determine which contribute to the observed hardness anisotropy. No such mathematical expression has been found in the literature.

Jan 1, 1969

By P. Eadington

I feel sure that the apparent anomolies between his findings and ours arise as a result of the different experimental methods used. The modem oxygen electrode method he used is sensitive to nano moles of oxygen uptake whereas the method we used was only sensitive to micro moles at best. Furthermore, our experimental method did not permit measurements to be made in the first ten to fifteen minutes of reaction, the very time he is observing. Direct comparison of his data to ours is made difficult because of not knowing the specific area of the samples he used. However, we found that precipitation of PbS using sodium sulphide gave rise to samples of area approximately 30 m2 g - 1. Noticing the rapid decline in oxidation rate over ten minutes, as reported in Table 1, one can conclude that we could not measure the rate after ten minutes using our method. Taking the above area I estimate that at these rates only a small fraction of surface would be oxidised in a period of hours. I can only conclude that at some point a change in oxidation mechanisms occurs giving rise to a much faster rate such as we observed. Finally, I would like to comment on the apparent inertness of the homogeneously precipitated lead sulphide sample 11. This method of preparation we found to give specific areas of 20 to 30 times less than other methods and this would account for the very low oxidation rate.

Jan 1, 1982

By J. Jolly

THIS short note on the probable character of the organic sulfur compounds in coal can do no more than indicate lines of research. We have no new experimental work to describe, nothing comparable in value with the careful studies of American coals by Powell and Parr1 and Yancey and Frazer.2 A study of the manner in which sulfur compounds exist in British coals (and their behavior on heat treatment) is rendered increasingly necessary by the fact that the British reserves of good coking coals of reasonably low sulfur content are fast being depleted. We believe that it is essentially by a study of the modes of formation, occurrence, and decomposition of the various types of inorganic and organic sulfur compounds in coal that it will be possible, with hope of success, to attack the problem of purifying coals, otherwise eminently suitable for coking, from these objectionable ingredients. Sulfur, so far as is at present known, does not normally occur in the free state in the coal conglomerate, but is chiefly distributed, irregularly, in three forms: 1. As primary constituents of the coal conglomerate, organic in nature and probably associated with those molecular complexes that have resulted from the degradation of the proteins of the plant tissues responsible for the formation of the coal mass. These constituents can be classed as "organic sulfur." 2. As metallic sulfides, e.g., iron pyrites. 3. As metallic sulfates, e.g., calcium sulfate and ferrous sulfate. (The occurrence of these compounds varies with the occurrence and degree of degradation of class 2.)

Jan 3, 1925

By E. Teghtsoonian, K. G. Davis

Cobalt crystals of commercial purity have been tested in tension. Their resolved shear stress-shear strain curves are very similar in form to those for zinc, magnesium, and cadmium. There is an initial linear region for shear strains up to around 150 pct, the ratio of work hardening slope to shear modulus at room temperature being about 2 X x This is followed by an upturn, which is, PLASTIC deformation in metal single crystals with close-packed structures has been found strongly dependent on stacking-fault energy. The high stacking-fault energy hexagonal metals magnesium, zinc, and cadmium have been quite extensively tested, but up to now no data have been available for a comparable hexagonal metal with low stacking-fau1t energy' An however, smaller in magnitude for cobalt than for the other metals. Values for the critical resolved shear stress rise from 97 kg per sq cm at room temperature to approximately 170 kg per sq cm at -196 °C. The Cottrell-Stokes ratio is not constant either for variations in the strain rate or for temperature changes, its value decreasing with strain. investigation into the plastic deformation of cobalt, which has a very low stacking-fault energy, has therefore been undertaken. EXPERIMENTAL PROCEDURES Cobalt crystals in the form of rods 0.3 cm in diam were grown in an electron-beam floating-zone refiner at a rate of zone travel of 25 cm per hr. Details of the growing procedure are given in Ref. 1. The zoned cobalt rods had the following analysis:

Jan 1, 1963

By Howard Smith

OF late considerable experimental and, theoretical interest has been shown in the rates of transformation from a single phase, usually a supercooled solid solution, into one or more phases. Such reactions may involve both diffusion and transformation of the major constituent, as in iron alloys, or it may simply involve diffusion, as in superstructure forma-tion and in age-hardening systems. Most of the work has been confined to ferrous alloys1-9t although two investigations have been made on copper alloys10,11. That such work may be of considerable, practical importance has been demonstrated by Bain12, by the workers at the Kaiser Wilhelm Institut fur Eisen-forschung13,14, and by the everyday use of precipitation and age-harden-inn principles15. Experiments in this country have generally followed Davenport and Bain's technique of rapid supercooling followed by isothermal treatment. In Germany16,17 the work has been extended to the study of the influence of accurately controlled and measured rates of cooling. The work on steel indicates that there are two subcritical temperature ranges where reaction starts sooner after quenching and proceeds at a more rapid rate than at other temperatures. At subcritical temperatures above Ar" where reaction is dependent upon atomic migration there is a period of time of which the length depends upon the alloy content and the temperature, before which no reaction has been detected. Daven-port and Bain1 find that different sorts of atoms in solid solution in gamma iron affect the length of this "prereaction" period differently, manganese

Jan 1, 1935

By R. S. Dean

ALTHOUGH it is obvious that in any flotation process we must have a froth, in recent years the development of collecting reagents has caused the possibilities of better frothing agents to be overlooked. Some investigators have even gone so far as to say that the number of satis-factory frothing agents was sufficient. A little consideration will show, however, that the reagents available in the past were far from ideal frothers. The properties of an ideal frother for flotation work may be set down as follows: 1. It. must form in low concentrations a copious but not too persist-ent froth. 2. It must be insensitive to hydrogen-ion concentration of the pulp; that is, it must froth equally well in an acid or alkaline medium. 3. It must be insensitive to salts, even in high concentration. 4. It must be absolutely noncollecting to both sulfides and nonsulfides. 5. Its frothing properties must not be affected by collecting reagents, including soap, the most generally used nonsulfide collector. 6. It must readily emulsify and disperse any insoluble collecting agent that is likely to be used. Clearly the existing frothers do not qualify. Pine oil, for example, is an acceptable frother for many purposes but if used in soap flotation a delicate balance between pine oil and soap must be struck because, as pointed out by Coghill1, these two reagents are incompatible in certain concentrations. The objections to soap itself as a frother are obvious, and the cresols and their substitution products all have some collecting Dower and very little emulsifying power.

Jan 1, 1935

By R. Van A. Norris

The following tests were made, during 1889, for the Susquehanna Coal Company, to determine the relative efficiency of several styles of mine-car wheels in use at their collieries at Nanticoke, Pa. The wheels experimented upon may be divided into two classes: The "old style" (Figs. 1 and 2), which are oiled at every trip; and the "new style" (Figs. 3, 4, and 5), which require oiling about once in two to four months. Fig. 1 shows a section of a plain cast wheel, with patent annular oil-chamber. This is held in position on the axle by a square, split cotter-pin. Fig. 2 is a similar wheel, with a patent cast bushing, which is readily replaced when worn. The lubrication is effected by a simple oil-hole, but the oil is delivered a little inside of the gaugeline of the wheel, where it is most needed. Figs. 3, 4, and 5 are sections of a " new style " patented, self-oiling wheel. In this, the outer end is cast closed, and the wheel is fastened to the axle by a spring cotter-pin passed through one of the plugged holes. Dirt is prevented from entering the open end by a cap, with faced end and packing-ring, fitting over the end of the hub. The lubricant is introduced into the oil-chamber through one of the plugged holes in the hub. When the wheel is in motion, the lubricant is thrown by centrifugal force away from the axle, enters the two ports shown, and is

Jan 1, 1890

By L. O. Howard

THE practice of using acid-lined converters at the plant of the Old Dominion Copper Mining & Smelting Co. was discontinued early in January, 1913, and they were replaced by basic-lined converters. The new equipment consists of one electrically operated 12-ft. upright converter stand and two basic-lined shells for same. These shells are provided with twenty-four 1 1/4-in. tuyères. The mouths are 5 ft. in diameter. Owing to the fact that there is no bedding system or other large storage capacity between the mine and the smelter, the furnaces must handle as fast as produced ore and concentrates, which may vary considerably from day to day, both in tonnage and copper content. Consequently the converter is often crowded to its utmost capacity by the frequent fluctuations in the daily matte supply. From the foregoing, it will be seen that in no way can the converter be favored by running light charges or by transferring to it from other stands in operation. Neither can it regularly be allowed to cool between blows, and only occasionally can it be run at as low a temperature as might be wished. No copper precipitate or other foreign material high in copper is available to help out the tonnage. Repairs and alterations or the removal of defective tuyères must wait until such time as a slight falling off in the matte supply-allows the converting operations to ease up. These variable conditions all combine to interfere with the systematic operating of the converter.

Jan 7, 1914

By G. R. Leverant

RECENT investigations1,2 of the low-cycle fatigue behavior of pure copper under strain cycling conditions have shown that a unique saturation stress level is eventually attained for each value of applied plastic strain amplitude. The dislocation substructure of copper at the saturation stress level is in the form of cells whose diameter decreases with increasing saturation stress level, i.e., plastic strain amplitude. In addition, both the saturation stress level and the cellular substructure are completely reversible. That is, the saturation stress level and accompanying cell size are determined solely by the present conditions of testing and are, therefore, independent of any previous cyclic history. The mechanical and substructural reversibility observed in pure copper, which has a relatively high stacking fault energy, is not observedz for Cu-7.5A1 which has a much lower stacking fault energy. This implies that easy cross slip (wavy slip) is a prerequisite for reversible fatigue behavior. A dispersion of fine, nondeformable particles of a second phase in a metal matrix tends to stabilize substruc- tures introduced by forming operations during subsequent elevated-temperature heat treatments.3 This raises the question as to whether a finely dispersed second phase can induce an element of irre-versibility into the cyclic deformation behavior of a wavy slip material at room temperature, due to partial stabilization of the initially introduced substructure. Since nickel has a higher stacking fault energy than copper,6 pure nickel should be characterized by cyclic reversibility. Therefore, TD-nickel* (Ni-2ThO.r) was

Jan 1, 1968

By Frank Fahrenwald

INTRODUCTORY A COMPLETE list of the elements as given for 1915 includes 18 that melt above 1,700° C. There does not exist one complete thermal equilibrium diagram for any pair of these 18 elements. Several of these elements have been combined, in relatively small proportions, with metals of lower melting point: e.g., tungsten, molybdenum, and vanadium, in steels, or with nickel and cobalt; but of this refractory group, platinum is the only one that has been extensively studied in this connection. When one considers that, with few exceptions, the industries have made use of alloys to the exclusion of pure .metals, it is reasonable to expect that alloys of this refractory group will invade fields in which the pure metals have found little application. The past neglect of this class of metals has, no doubt, been partly due to the rarity of some of them, for even though alloys of very valuable properties should be developed, their cost, unless in exceptional applications, would be prohibitive. There is also a well-founded reluctance to undertake research involving very high temperatures which, in the case of most of these elements, must be accompanied by an inert atmosphere as well. This combination of high temperatures* and control of atmosphere within the heating chamber of any furnace of present design is a difficult problem. It is the purpose of this paper to give results,1 of an investigation of one binary series of this group, in which methods were employed that avoided the usual difficulties accompanying high-temperature alloy investigation.

Jan 6, 1916

By P. Somasundaran, I. J. Lin

There are several methods described in the literature for the determination of the order and the rate constant for the flotation of minerals. These often involve some type of computational or graphical procedures. A relatively simpler method developed on the basis of a technique used by Chang" in chemical kinetics is described in this paper. Chang's technique, like most others in chemical kinetics," is based on the law of mass action which states that the rate of a chemical reaction is proportional to the active masses of the reacting substances at any given time. Application of this law to the flotation of minerals would involve the adaptation of the terms "flotation" for "chemical reaction" and "floatable amount of the minerals" for "the active masses of the chemical reactants." There are indeed a large number of physical processes controlling the actual flotation rate. The most inefficient one of these could be considered equivalent to the slowest reaction in a series of chemical reactions. If variables such as aeration rate and agitation are kept at constant levels, the rate of flotation under free flotation conditions (i.e., conditions under which the suspension is dilute) will be given by the following equation: where C is the concentration of the floatable minerals in the pulp at any given time t, K is the rate constant, and n is the order of the reaction. If we represent the floated fraction of the floatable mineral at time t as m (0 m - 1) and C at t = 0 as Ca, integration of Eq. 1 yields

Jan 1, 1974

By Roswell Johnson

THE Manual of the Oil and Gas Industry, under the Revenue Act of 1918, published by the Treasury Department for the guidance of oil companies in preparing their estimates of future recoverable oil for the purpose of calculating depletion, gives the first large public collection of comparative decline curves for the whole country. It is a matter of both scientific and practical interest to so arrange these data that the pools can be readily compared. There are certain difficulties in such a comparison, however: 1. The economic limit varies from 50 to 2000 bbl. a year in different pools taken. (2) Because of this variation in economic limit, the range of data shown makes comparison possible only for wells of intermediate size. In order to be as inclusive as possible, I have taken as an expression of the rate of decline the amount of oil produced in the period during which a well drops from 3000 to 2000 bbl. a year.. No period of smaller production could be used because of the high economic limit in California; and no period of larger production and yet include the small well areas of the Appalachian. As it is, the Lima-Indiana wells are excluded. In a few instances, curves were extrapolated to obtain the reading, where the curve seemed regular enough to warrant it. In general, the amount of oil, in barrels, produced while a well declined from 3000 bbl. to 2000 bbl. a year is shown in Table 1.

Jan 1, 1920

By A. F. Crawley

THIS paper describes part of a series of density measurements on low melting point metals being undertaken at the Mines Branch, Department of Energy, Mines and Resources, Ottawa, Canada. This program has received support from the Canadian Zinc and Lead Research Committee and the International Lead and Zinc Research Organization. Examples of the type of work being done have already been given in earlier papers' , which deal with the densities of lead, tin, and some of their alloys. Densities were measured using a graphite pyc-nometer by a technique which has already been described." The cadmium and indium, supplied by the Consolidated Mining and Smelting Co. of Canada were of 99.999 pct purity. Density determinations on indium, as for lead and tin,1,2 were made under a vacuum of about 5 x 10-6 torr because the oxidation and vaporization characteristics of the metal do not create experimental difficulties. This contrasts markedly with cadmium which, even at the relatively low temperatures of our experiments, has a high vapor pressure and a strong oxidation potential. To suppress the harmful effects of these properties, determinations on cadmium were made with success under an atmosphere of argon, the technique having been previously established in this laboratory for measurements on zinc.3 The densities of cadmium and indium are listed in Table I and plotted in Figs. 1 and 2. From the graphs, it is readily observed that the densities of both metals vary linearly with temperature. This relationship expressed mathematically is of the form:

Jan 1, 1969

By E. B. Thornhill

Discussion of the paper of E. B. THORNHILL, presented at the San Francisco meeting, September, 1915, and printed in Bulletin No. 104, August, 1915, pp. 1653 to 1670. D. B. HUNTLEY, Oakland, Cal.-About 15 years ago it chanced to be my lot to cyanide some mill tailings, assaying about $5 per toll in gold and, a few cents in silver. It was in southern Idaho, a. desert region where costs are nearly as large as in central Nevada. We knew that we had a lot of tailings that had been amalgamated and contained about 1 lb. of quicksilver per ton. We knew that we would dissolve some of the quicksilver when we cyanided them with say 0.25 per cent. cyanide solution. We figured (optimistically) that the cyanide would dissolve all of the quicksilver, and we thought to capture all of that, 1 lb. per ton; and we figured out profits as partly gold, partly silver, and partly quicksilver from the recovery in working those tailings. Actually, however, we did this: We had a battery of three large, old-fashioned silver-mill retorts. We retorted our zinc-dust precipitate, recovering about ¼ lb. of quicksilver per ton treated. That was only a loss of 75 per cent. of what we originally had, but still it was profitable by virtue of the conditions. I mention it partly to call attention to the crude old way of doing it, and partly to call attention to how chemical methods for recovering quicksilver have developed in the last 15 years.

Jan 12, 1915

By B. E. Eakin, A. L. Lee

Atmospheric pressure viscosity values For light hydrocarbons were calculated by a simple mixing rule based on the Sutherland constants for pure components. This method was further extended so that the atmospheric pressure viscosity of a mixture may be calculated based on the molecular weight information only. INTRODUCTION A proven method for estimating the gas-phase viscosity of a mixture is the one by Herning and zipperer.l This mixing rule has the following form: One method for calculating the pure component viscosity i is the Sutherland equation,2 which has the following form: The Sutherland constants B and S are determined from experimental data. A set of Sutherland constants for light hydrocarbons based on the data of several investigators3-5 is presented in Table 1. APPLICATION The Herning-Zipperer equation and the Sutherland equation were used to obtain an equation for calculating the gas-phase viscosity of light hydrocarbons. This equation has the form, Eq. 3 was used successfully in the study of methane-n-butane mixtures.6 Further analysis indicated that the Sutherland constants are a function of molecular weight.7 The gas-phase viscosity may be calculated based on molecular weight information only. The following equation was developed: The atmospheric pressure viscosity of ethane, propane, n-butaneand four methane-propane mixtures calculated on the basis of Eq. 6 are compared with the data of other investigators in Tables 2, 3, 4 and 5, respectively. A plot of atmospheric pressure viscosity vs molecular weight based on Eq. 6 is presented in Fig. 1.

Jan 1, 1965

Department of Conservation and Development, State of North Carolina, Raleigh, N C H J Bryson, State Geologist. The latest list of publications will be sent upon request. Of the many Bulletins, Economic Papers, Circulars and Volumes issued by the Department of Conservation and Development, the following are available and relate to mining and geology of the state ? Bulletin 18, Bibliography of North Carolina geology, mineralogy and geography (1909), 50 cents, 21, The Gold Hill mining district (1910), 15 cents, 22, Report on Cid mining district (1911), 15 cents, cloth 75 cents, 25, Zircon, monazite and other minerals, 15 cents, cloth, 75 cents, 28, Limestones and marls, 15 cents, 29, Kaolins of North Carolina, 50 cents, 31, Deposits of brown iron ore, 50 cents, 32, Magnetic iron ores, 15 cents, 33, The Deep River coal field, 50 cents, 37, Pyrophyllite deposits, 35 cents A series of the Economic Papers review the mining industry in North Carolina for the years cited Those now available are Economic Paper 23 (1908-1909-1910), 10 cents, cloth, 50 cents, 49 (1913-1917), 20 cents, 55 (1918-1923), 25 cents, 60 (1924¬1925), 15 cents, 63 (1927-1928), 25 cents. Other available Economic Papers on geology and mining are No 3, Talc and pyrophyllite deposits (1900), 25 cents; 58, Oil prospecting well near Havelock (1927), 5 cents, 59, Oil-bearing shales of Deep River Valley (1927), 10 cents Available volumes on geology. Vol 1, Corundum and the basic magnesian rocks (1905), 35 cents, cloth, $150, 5, The Cretaceous formations of North Carolina (1923), cloth $1 75

Jan 1, 1933

(Under this heading will be published notes sent to the Secretary of the Institute by members or other persons introduced by members.) No. 504.-Member, technical graduate, draft exempt, who has been employed as research chemist in cyanidation and flotation for past 5 years, desires position with large company as metallurgist or assistant mill superintendent. Especially experienced in flotation of gold and silver ores, but am also familiar with flotation of lead-zinc ores. Foreign service not desired. Will be at liberty after Dec. 1, 1918. No. 505.-Member, graduate mining engineer, with 8 years' practical experience, including experience as superintendent. Desires position as engineer, foreman or superintendent of mine. No. 509.-Petroleum geologist and engineer, member, now engaged in consulting work, with five years' experience in Mid-Continent and Eastern fields, desires position with responsible concern either in South or South American countries. No. 510.- Chemical engineer, member, technical graduate, at present officer in Chemical Warfare Service of the United States Army, desires position in the East. Several-years' experience in design, construction, and operation of chemical and metallurgical plants. Minimum salary, $200. Available Jan. 1, 1919. No. 511.-Mining engineer, 32 years old, single, desires position. Speaks Spanish and French. Recently manager of large copper mines. Experience in steam shovel and underground mining. No. 512.-Mining engineer, technical graduate, member, 32 years old, single, 10 years' experience in United States, Mexico and Central America in mining, prospecting, milling, chemical research and business experience. Speaks Spanish. Open for engagement as superintendent or assistant. Can give references as to ability and integrity.

Jan 1, 1919

By M. J. Marcinkowski, Gordon E. Lakso

An extensive investigation has been made of the deformation behavior associated with the Fe3Si super-lattice using transmission electron microscopy techniques. Above 243°K the stress-strain curve exhibits three stages. Stage I occurs at a very low stress level and is related to the generation of perfect superlat-tice dislocations. Stage II is characterized by an extremely rapid rate of work hardening and is associated with the Taylor type locking of these superlattice dislocations. Finally Stage III is related to dynamic recovery processes since the work hardening rate is very small. Below 243ºK, only Stage I is observed, but it occurs at a much higher stress level. This latter observation is related to the generation of imperfect dislocations in Stage I with the consequent production of second nearest neighbor antiphase boundaries. The reason for this is that insufficient thermal energy is available at these low temperatures to generate the complete and perfect superlattice dislocations. It has been shown that the fully ordered FeCo alloys, i.e., those possessing the B2 type structure, exhibit three distinct stages of work hardening whereas the corresponding disordered alloys show only one.&apos;" This difference in behavior between the disordered and ordered alloys has been attributed to the fact that dislocations in the former case travel only as ordinary 1/2ao(111) types whereas in the latter case the move through the lattice as coupled 1/2a0(111) dislocations separated by an antiphase boundary (APB), i.e., the so-called superlattice dislocation. Although some preliminary work has been carried out concerning plastic deformation in ordered alloys possessing the DO3 type superlattice,3 no detailed analysis similar to that described in Refs. 1 and 2 has been attempted. Specifically, it has been suggested that the superlattice dislocation in this particular type structure should consist of four ordinary 1/2ao<111> types bound together by first and second nearest-neighbor APB&apos;s. Fe3A1 and Fe3Si are the two classic alloys possessing the DO3 type lattice; however, because of the somewhat higher ordering energies associated with the FesSi alloy, which in turn assures that dislocations will travel through the lattice as perfect superlattice dislocations under at least some conditions, it was chosen for the present investigation. Because of the extreme brittleness of Fe3Si, all deformation was done in compression. Stress-strain curves were obtained using both polycrystalline samples as well as single crystals. In the latter case the crystals were oriented so that deformation could be controlled either by single or double slip. They were then wafered parallel to and at various angles to the operative slip planes. These wafers were in turn examined by transmission electron microscopy (TEM) techniques in order to determine the extent of the interaction from the dislocation configuration contained therein. EXPERIMENTAL PROCEDURE The alloys used in this investigation were arc melted under helium from electrolytic iron of greater than 99.90 wt pct purity and transistor grade silicon of 99.99 wt pct purity. A typical analysis of interstitial impurities showed 120 ppm 0, 15 ppm N, and 65 ppm C Because of the extremely low ductility of the Fe3Si alloys, it was necessary to spark cut 0.230-in. diam polycrystalline cylinders 0.400 in. long from arc-melted fingers using a thin-walled brass tube as a cutting tool. The polycrystalline alloys could not be recrystallized since very little strain was induced in preparation. However they were annealed at 1273°C for 15 min in evacuated vycor capsules to relieve any cooling stresses that may have developed during solidification and then air cooled. The resulting grain size of the alloy was 0.50 mm. According to warlimont4 1273ºC is just within the single phase field where FesSi possesses the DO3 type lattice. In addition because of this high critical ordering tem-ature, air cooling from this temperature was believed sufficient to fully order all of the Fe3Si samples used in the present investigation. For the same reason, no attempt was made to achieve any degree of disorder by quenching. In fact, rapid quenching from 1123°K caused cracking. Such cracking was first suggested by sato5 with respect to the experimental observations of Glaser and Ivanick.6 Single crystal compression specimens were spark cut from single crystal ingots grown in a Bridgman type furnace. The iron and silicon for the crystals was prealloyed by arc-melting two 130-g buttons which were cut into small pieces before remelting in the furnace. This procedure resulted in a long-range inhomogeneity of 0.5 at. pct Si between the top and bottom of the 2-in.-long single crystal ingot, which was assumed to be negligible in the present investigation. The single crystals, after orienting and spark-cutting, were about 0.37 in. by 0.37 in. in cross section and about 0.5 in. long. True stress-strain curves were obtained using an Instron Tensile Testing machine in conjunction with techniques described previously. 1,7 The strain rate was 0.05 in. per in. per min. Prior to testing, the ends of all the compression cylinders were hand polished using a special jig to insure parallelism after which the sides of the samples were electrochemically polished to eliminate stress risers and to facilitate slip line observations. Test temperatures between 77" and 823°K were obtained using various cooling and heating media as described in Ref. 7 while at the upper end of this temperature range, a mixture of equal

Jan 1, 1970

By R. W. Gould, B. G. LeFevre, A. G. Guy

The resistivity anomaly known as the K state was studied in Ni-Mo alloys containing 10.5 and 14.0 at. pct Mo. Both these alloys exhibit a large K effect which depends on the mechanical and thermal treatment. On the basis of X-ray diffuse scattering studies which were correlated with resistivity measurements, it appears that the K state in dilute Ni-Mo alloys can be associated with changes in the degree of short-range order within the a phase. An interesting phenomenon that has received much attention in recent years is the K state. The K state is marked by anomalous changes in some of the physical properties of certain alloys without the occurrence of observable microscopic structural changes. One of the early pieces of work in this area was by Thomas&apos; who studied alloys of Ni-Cr, Ni-Cu, Ni-Cu-Zn, Fe-A1, Fe-Si, and Ni-A1. Upon annealing specimens which had been previously cold-worked or quenched from an elevated temperature he found an anomalous increase in resistivity over a certain temperature range. He also found that specimens which had been appropriately annealed to develop the K state showed a decrease in resistivity upon subsequent cold working. These effects are opposite to those found in normal alloys. Although the resistivity anomaly has been rather arbitrarily taken as the "definition" of the K state, there are several other interesting effects which accompany the resistivity increase. In Ni-Cr alloys,2, 3 for example, it was found that the hardness increases with increasing resistivity. It was also found that specimens which have been treated to develop the K state can be cold-worked for as much as an 80 pct reduction of area without an increase in the hardness. In Fe-A1 and Fe-Si alloys4 the K state is accompanied by an increase in flow stress and by a lattice contraction. In Ni-A1 alloys,5 specimens which have been treated to develop the K state also show an increase in elastic modulus. In Ag-Pd alloys6 the increased resistivity observed on annealing a cold-worked specimen is accompanied by an increase in the thermoelectric power and an increase in the Hall coefficient. The explanations of the K state phenomena are varied and depend upon the particular alloy in question. Several theories have been advanced to explain the increased conductivity with cold work on the basis of changes in the electronic configuration of the alloy as a result of local lattice distortions.7"9 Most investigators, however, believe that some type of local order in the solid solution, either short-range order (SRO) or clustering, is responsible for this effect. Theories concerning the relationship between ordering and the K state have for the most part been speculative, since there is little direct X-ray evidence that can be correlated with the above property changes. Much of the previous work on the K state was done in the Ni-Cr system where the small difference in the X-ray atomic scattering factors of the components nickel and chromium makes it very difficult to use X-ray diffuse-scattering measurements to determine the role of local order. In the Ni-A1 system, however, Starke et al.10 succeeded in detecting a connection between local order and the K state. It was found that a small but measurable K effect correlated with increasing SRO in the nickel-rich a phase. The manner in which local order might increase the resistivity of K state alloys is not completely clear. Since most of the known K state alloys contain at least one transition element, significance has frequently been attached to the presence of an unfilled d shell. It has been suggested that during the formation of the K state the number of conduction electrons decreases as a result of the transfer of s electrons to the d shell where they are more tightly bound.1&apos;11&apos;12 Koster and Rocholl13 have proposed that SRO can cause an increase in resistivity for alloy systems in which the number and mobility of charge carriers are reduced when the percent solute is increased. According to this hypothesis, the local environment of a given solvent atom changes in the same manner with increasing percent solute as it does with an increasing degree of SRO; hence the change in physical properties should tend in the same direction. In this hypothesis, SRO is considered only in a statistical sense, and the increased resistivity of the K state is attributed to a change in the mean distribution of electrons and holes in the s and d states as a result of SRO. From the work of Chen and Nicholson on Ag-Pd alloys,6 it appears that the K state can occur in systems for which the d shell is completely filled. These investigators explained the increased resistivity by picturing the SRO as small domains of some form of long-range order (LRO). According to ~ibson,&apos;~ the number of effective electrons can be reduced by the creation of a new Brillouin zone boundary near the Fermi surface of an alloy as a result of the changing crystallographic symmetry that accompanies the formation of a superlattice. This idea may be expressed in terms of the superzone concept.15 In the present work the role of local order in the formation of the K state in Ni-Mo alloys was investigated. The principal tools used in this study were X-ray diffuse scattering and electrical resistivity measurements; however, these data were supplemented by electron microscopic and field-ion microscopic data. The purpose of the work was to determine whether or not the K state in Ni-Mo alloys can indeed be attributed to the formation of SRO as has been proposed by previous investigators.

Jan 1, 1969

By E. J. Nielsen, P. R. Strutt

A study has been made of the progressive changes in the distribution of etch-pit structures occurring during high-temperature creep in copper + 7 wt pct Al single crystals oriented with a [113] tensile axis. The two equally stressed glide systems with the highest Schmid factor would be expected to form subboundaries of the type predicted by Kear.2 The alignments of etch-pits on sections parallel to different (111} planes consistent with these types of boundaries were not observed. However, they were consistent with planar subboundaries (on a macroscopic scale). From an analysis of Amelinckx1 it may be shown that stable cross-grid dislocation boundaries may form in the primary slip planes. These boundaries form when dislocations with a Burgers vector not in the slip plane move into the plane by combination of climb and glide. THE geometry of subboundaries formed by the interaction of dislocations of two glide systems has been analyzed by Amelinckx,1 and the particular types produced by deforming fee crystals are predicted by ear.&apos; In this paper types of boundaries which may be formed when climb as well as glide occur are discussed as this is relevant in high-temperature creep. It is assumed in the present investigation that the etch-pits observed in Cu + 7 wt pct A1 on surfaces parallel to {111} planes delineate the sites of dislocations. Although there is no direct evidence for this previous work on a-Cu/Al single crystals by Mitchell, Chevrier, Hockey, and Mon-aghan,3 would show this assumption to be reasonable. The alignments of etch-pits which form during creep are studied on sections parallel to each {111) plane. It is then deduced that these alignments are consistent with a specific type of planar subboundary. The Cu + 7 wt pct A1 single crystals had a [113] tensile axis and Fig. 1(a) shows schematically the relation of the slip planes and slip directions (as represented by tetrahedron ABCD) with reference to the tensile axis. The two equally stressed glide systems with the maximum Schmid factor namely ß-AD and (a-BD, from the analysis of Kear,2 would be expected to form the boundaries shown in Fig. l(a) and (b), also Fig. 5(a) and (b). EXPERIMENTAL PROCEDURE The a-Cu/Al single crystals were grown and annealed in a "gettered" argon atmosphere. Chemical analysis showed the aluminum content to be uniform in each crystal and the difference between crystals was maintained to an accuracy of ± 0.25 wt pct. The initial dislocation density and mean subgrain diameter after annealing was -106 cm-2 and 250 µ, respectively. Surfaces parallel to (111) planes were produced by specially developed electrolytic machining processes. The {111} faces were next electropolished for 5 min in a solution consisting of 25 g chromium trioxide, 113 ml glacial acetic acid and 40 ml water; the applied potential was 8 v. Dislocation etch-pits were revealed using l an etchant described by 1 ml bromine, 45 ml HCl, and - 250 ml water. RESULTS In crystals strained into secondary creep at higher stresses (443 and 750 g - mm-2 at 650° C aligned rows of etch-pits parallel to slip plane traces were evident in sections parallel to the (1111, (ill), and (111) planes, see Fig. 3. As well as the longitudinal alignments in Fig. 3, well formed randomly oriented arrays indicative of an equiaxed subgrain structure are evident. At the lower stresses (100 to 230 g . mm-2) only an equiaxed structure formed during creep. The sections in Fig. 3 are from a crystal crept for 70 hr at 650°C with a CRSS of 443 g.mm-2. Two identically oriented crystals were also deformed at the same temperature and stress for 5 min and 4 hr. In the crystal crept for 5 min, the etch-pits were randomly distributed with no tendency for directional alignment, see Fig. 2(a). As shown in Fig. 2(b) aligned arrays were evident after 4 hr creep but they were not nearly so well defined as in Fig. 3. The alignments (parallel to the arrows) in Fig. 3 are consistent with the existence of boundaries in the two main slip planes a and ß. The way in which this is deduced is seen by reference to Fig. l(c), where the existence of boundaries in the a and ß planes is verified by sectioning parallel to a,ß, and d. The (111) and ß(111) planes intersect the d(111) plane along BC [101 ] and AT [011] and alignments parallel to [101] and [011] are clearly evident in Fig. 3(c) in a section parallel to the d(111) plane. Similarly the a, and ß planes in Fig. l(a) intersect each other along DC [110] and hence there will be an alignment parallel to [110 ] in sections parallel to the a-plane and the ß-plane; this is evident in Fig. 3(a) and Fig. 3(b). It is interesting to note that alignments of etch-pits consistent with the boundaries predicted by Kear2 were not observed; see Figs. l(a) and l(b). The geometry of boundaries in {111} planes as shown in Fig. l(c) is discussed later. In Fig. 4(a) the individual etch-pits are resolved and the alignments are exactly parallel to the slip trace direction [101]. However, in some areas alignments deviate away from the slip trace direction by as much as 10 to 15 deg, this is evident in Fig. 4(b), and in Fig.

Jan 1, 1969