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By A. E. Bibb, F. W. Kunz

A platelet form of zirconium hydride was found in zirconium and ZY-1 wt pct U single crystals containing hydvogen in the range of 50 to 100 ppm. The habit planes for the hydride plateletg in the zirconium crystals were found to be {1012}, {1121}, and (1122) while the habit planes in the ZY-1 wt pct U crystals were {1121), {1123}, and (1.231). With the exception of the {1231} plane, these have been identified as the twin planes in zirconium. The different effect of hydridc on the mechanical puoperlies of zirconium at high and low strain rates has been explained in terms of the defornzation mechanism and the habit planes of the hydride. ZIRCONIUM and zirconium-base alloys are considered for many nuclear reactor applications, where the pick-up of hydrogen is a distinct possibility, if not an unavoidable occurrence. An excellent example of this is the absorption of hydrogen by zirconium and its alloys during aqueous corrosion, where as much as 30 pct of the hydrogen produced by the corrosion reaction is picked up by the metal. Under the proper conditions, the absorbed hydrogen would precipitate as zirconium hydride and consequently alter the mechanical and physical properties of the zirconium-base alloys. The knowledge obtained from a study of the crystallographic aspects of the hydride precipitation is necessary for the interpretation of the observed changes in the mechanical and physical properties. The deleterious effect of hydrogen on zirconium-base materials is not always observed in normal slow tensile loadings at or above room temperature, but becomes immediately obvious under impact loading, where the energy absorbed decreases with increasing hydrogen content,' and in notched specimens where triaxial loadings are attained.2 This effect is of serious consequence in the applications of Zr where shock loads or high strain rates are experienced. The purpose of this investigation was to determine the crystallographic planes of the Zr and Zr-1 wt pct U matrices upon which zirconium hydride will precipitate and to correlate these with the observed mechanical property data. PROCEDURE Crystal Growth—Single crystals of Zr and Zr-1 wt pct U alloy were used in this investigation. The Zr crystals were made from sponge that had a typical analysis as shown in Table I. Large grains were grown in this material by rapid cooling an arc-melted charge in a button furnace. This operation undoubtedly lowered the volatile impurity concentration below those listed in Table I. Back-reflection Laue patterns of these large grains showed the presence of considerable substructure and lattice distortion within each grain. It was found that an 18-day anneal in an argon atmosphere at 840°C (a high a heat-treatment) followed by furnace cooling, resulted in the further growth of the large grains and removed the detectable substructure ana lattice distortion. Equiaxed crystals with a cube edge of approximately 1/4 in. were produced in this manner. Large crystals of Zircaloy-2 (1.5 wt pct Sn, 0.15 wt pct Fe, 0.1 wt pct Cr, 0.05 wt pct Ni) also were produced by this technique but the large amount of substructure formed could not be removed by annealing. The Zr-1 wt pct U solid solution crystals were produced from an alloy rod consisting of Westing-house-Foote hafnium-free crystal bar zirconium and depleted uranium. The chemical analysis of the alloy is also given in Table I. Three-inch sections were cut from an 0.120-in.-diameter alloy rod and tapered to a fine point on each end. The samples were sealed in evacuated Vycor tubes, homogenized for 5 hr at 1000°C in the ß-phase field, and slowly lowered in a gradient furnace into the a phase (800°C), annealed for 60 hr at this temperature to produce grain growth and furnace cooled. This technique produced large grains approximately 1/2 to 3/4 in. long over the entire cross section of the rod, which were free of observable substructure. Metallographic examination up to X1000 did not show the existence of any second phase in these grains. Crystal Orientation—All crystals were abraded on fine emery paper to produce two flat surfaces 90 deg to each other. The crystals were analyzed by the standard Back-Reflection Laue technique to obtain the crystal orientation with respect to the abraded surfaces. The Back-Reflection Laue Photograms of all crystals used were clear and sharp indicating that the crystals were free from any substructure that could be detected by these means. Hydriding—Only samples containing four to five grains were used for hydriding. Samples that exhibited fine grained patches were discarded. The samples were hydrided using the following technique. After etching in 48 vol. pct HNO3, 48 vol. pct H2O, and 4 vol. pct HF (48 pct) solution, the specimens

Jan 1, 1961

By M. E. Wadsworth

The chief value of a paper like this consists in its statistical tables, putting on record material useful to future inquirers. The data here given have been compiled from time to time as far back as 1874, and subsequently brought up to date. Much of the data could only be procured by personal inspection of the catalogues, as for example those relating to the Lawrence Scientific School, which were taken at that time from the catalogue of Harvard University, on file in the University Library, by the present writer, then an instructor in that institution. These tables of statistics were first prepared for publication by the present writer in 1888-1890 and published in his "Report to the Board of Control of the Michigan College of Mines " (Michigan Mining School) for 1886 to 1890. Later they were revised, enlarged and brought down to date in his reports to the same Board for 1890-92; and since that time they have been, at his request, revised, greatly enlarged and kept up to date by Mrs. Frances H. Scott, the efficient Librarian and Secretary of the Michigan College of Mines. Great credit is due to her for her devotion to this work and her untiring efforts to have the statistics complete as far as possible. The accompanying running commentary is given simply as a string to hold these statistics together, and in order to call attention to a few points. In compiling any tables like those accompanying this paper, one is confronted by serious difficulties, some of which render these results only approximate. In order to insure greater correctness and fullness in the statistics to be published the writer's reports for 1890-92 were sent to the president of every college, university, and technical school in the country, so far as known. Accompanying this was a personal letter which asked of each one his aid in correcting any errors, and in giving fuller statistics. But relatively few answers were obtained, and subsequently from one to many letters have been sent to each institution not formerly reply-

Jan 1, 1898

By Robert H. Richards

This is in part a review paper, indicating the various steps that have been taken in developing hindered-settling apparatus, some of the standard data that have been obtained, and some of the conclusions one is led to as to the effect of it in improving concentrating-methods and machinery, and in part it brings in some unpublished work. Causes oF Loss in ORe-ConcEntration. In making a study of the separation of valuable minerals from the waste gangue, particularly by water concentrators, it is necessary to define, first of all, what are the causes of loss that are likely to interfere with the concentration. Having made this definition, we can then study to see in what may the machines make their losses, and plan remedies for them in an intelligent way. Losses may be stated to occur as included grains, as flat or long grains, as fine free mineral, and as absolute slime. We will take these up one by one, as follows: Included Grains.—Fig. 1 shows by a set of diagrams how included grains may occur : first, where the heavy mineral grains attached to the quartz are of large size; secondly, where they are of small size; and thirdly, where very fine particles of heavy mineral are included in the quartz. We have to decide in regard to included grains whether they are rich enough to go direct to the furnace, or poor enough to throw away, or whether they lie between these two points and require recrush-ing as the only means of severing the values from the waste. This last case is the orlly one requiring special treatment at our hands. We will therefore consider that next.

Jan 1, 1911

By S. G. Epstein

Electromigration has been measured in dilute liquid alloys of lead in antimony and antimony in lead. In these alloys antimony migrates with the electron current; lead migrates in the opposite direction. These results, which contradict the mass criterion, were predicted by the electron drag model for electromigration in liquid alloys. The existing experimental data are shown to correlate with the difference in electrical resistivities of the alloy components. FOR many years investigators have attempted to relate observed electromigration phenomena in liquid alloys to the physical properties of the alloy components. The most successful correlation was found by Angus et' al.,1 who in 1959 proposed an empirical criterion for predicting the relative direction of motion of the components of a liquid alloy in an electric field: the component with the smallest atomic mass concentrates at the cathode. While this criterion is obeyed in nearly all the alloy systems which had been investigated, the physical basis for such an effect was not understood. It was also disturbing that the mass criterion predicted the wrong sign for the Haeffner effect; observations with pure liquid metals revealed that in every instance the lighter isotope was transported to the anode.2 Klemm3 explained these isotopic separations by suggesting that the lighter isotopes were more mobile and more easily carried to the anode with the electron stream. Additionally, several deviations from the mass criterion have been found in liquid alloys, notably involving transition metals such as chromium, nickel, palladium, and zirconium, which migrate to the anode in liquid bismuth.4'5 Recently, a model has been proposed6 in which electromigration in liquid alloys is attributed primarily to the interaction between the electron stream and the metal ions. In essence, this model predicts that the component with the greater electron-ion scattering cross section will be preferentially transported to the anode, displacing the other component to the cathode. The electrical resistivity of each pure component at its melting point is taken as the measure of its scattering cross section. This model was developed from the results of systematic studies with various solutes in liquid mercury,7'8 bismuth,9 and sodium.10 In every alloy, the component with the greater resistivity has centrates at the anode. Coincidentally, in every instance the component with the greater resistivity has also the greater mass, apparently satisfying the mass criterion. In order to differentiate between electron-ion coupling and atomic mass as the relevant physical prop- erty influencing electromigration, measurements were made with Pb-Sb alloys. Lead has an atomic mass nearly twice that of antimony, but lead has an electrical resistivity of 91 microhm-cm while antimony has a value of 113.5 microhm-cm at their respective melting points. The mass criterion predicts that in an alloy of the two antimony will concentrate at the cathode; the electron drag model predicts that antimony will concentrate at the anode. EXPERIMENTAL To conclusively determine the relative motion of lead and antimony in each other, solute electromigration was measured in dilute liquid alloys of antimony in lead and lead in antimony. Both starting materials were 99.999+ pct pure. The measurements were made with the same capillary-reservoir technique previously used for measuring electromigration in liquid bismuth alloys.11 Several changes in the experimental apparatus were necessary, however, to accommodate liquid antimony, which has a higher melting point than bismuth. The modified apparatus is depicted in Fig. 1. In each experiment four quartz capillaries were filled with the molten alloy. A direct current was passed through two of the capillaries; the electrode in one of these capillaries was made the cathode, and the electrode in the other was made the anode. The remaining two capillaries sampled the alloy in the reser-

Jan 1, 1969

By A. M. Turkalo

IT is a well-known fact that martensitic steels show a greater resistance to brittle fracture than do pearlitic and bainitic steels. It was, therefore, thought worthwhile to investigate the mode of brittle fracture with respect to structure by studying the effect of various austenite decomposition products on the propagation of brittle fracture in steel by means of electron microscopy. Newly developed replication techniques together with the advantages of the electron microscope such as great depth of field, available high magnification and easy adaptation to stereophotography make electron microscopy very suitable for fracture studies. EXPERIMENTAL PROCEDURE An essentially plain carbon steel containing 0.56 pct C, 1.30 pct Mn, 0.02 pct P, 0.03 pct S and 0.22 pct Si was used in this investigation. The following table gives the heat treatments used to obtain the various austenite decomposition products: The resulting austenite grain size from the 870°C austenitization treatment was about an ASTM No. 7 grain size. The specimens which were 2 in. long, 1/4-in. diam bars were austenitized in a tube furnace through which argon gas was blown. The tube was not, however, air-free and the specimens were not completely oxide-free. Isothermal treatments were done in a lead bath. With the exception of the fully hardened specimen and the one as-isothermally transformed at 300°C the heat treated specimens were notched in the following fashion with a jeweler's saw. A cut about 0.08 in. deep was made perpendicular to the length of the bar. The specimen then was rotated about 45 deg and another cut about 0.08 in. deep was made. In the case of the hard martensitic and bainitic specimens, only one cut was made and the depth was not controlled. The design of the two-cut notch caused fracture to initiate at the point of intersection of the two saw cuts. The specimens were broken at -196°C in a Charpy impact testing machine. In order to hold the specimens securely in the impact machine two square pieces of mild steel were made about 5/8 in. long having the same cross section as that of a standard Charpy specimen but containing a hole 1/4 in. diam through the center of the cross-section. These adapters were slipped over the ends of the test specimen which was then secured tightly by means of set screws in the adapters. The specimen with the adapters was cooled to -196°C in liquid N,, then placed in the impact machine and broken within 3 sec. One half of the broken specimen was used for the electron microscope study of the actual fracture surface. The other half was nickel-plated and a cross section through the notch and fracture was polished for electron microscope examination. Carbon replicas of the fracture specimens for the electron microscope study were made essentially according to Bradley's evaporation technique.' Both direct carbon and two-stage carbon replication techniques were used. In the case of the direct carbon technique, a thin layer of carbon was evaporated first at an angle of about 45 deg to the mean fracture surface and then another film of carbon was evaporated normally to the fracture surface. The carbon replica was freed electrolytically.2 The specimen was made an anode in a 10 pct Nital polishing solution. It was etched intermittently by shutting off the power now and then. The freed replica was washed in 40 to 50 pct water solution of nitric acid for 10 min or so, then washed in water and picked up on a screen for examination. The two-stage carbon replication technique involved first making a primary replica of cellulose * acetate from which a carbon replica was then made. One side of a strip of cellulose acetate wet with acetone was pressed lightly against the surface of the specimen, allowed to dry and then stripped. Prior to the deposition of carbon, which was done at 90 deg to the cellulose acetate replica surface, chromium was evaporated at 45 deg. After the carbon evaporation the cellulose acetate was dissolved in acetone according to the Jaffe method3 leaving the carbon replica preshadowed with chromium for examination.

Jan 1, 1961

By P. Barnes

The sums given in the accompanying table are those actually paid for material and labor up to about August, 1875; but, as some parts of the machinery were not wholly completed at the starting of the works in September, 1875, the statement cannot be taken as an absolutely correct note of the total cost. A complete description, with engravings of the building and machinery, was given in Engineering, April 26th, 1878, in a paper by Messrs. A. L. Holley and Lenox Smith, to which convenient reference may be made. A detailed list of the construction accounts has been given in a paper, by the present writer, in vol. vi, Transactions of the Institute. A summary is given in the table of the items in each class which enter into the total cost, and also a note of the proportion which each of these items forms of the whole. A concise view may thus he obtained of the facts embodied in the statement as a whole, even though it cannot lay claim to completeness in showing the entire or final cost. An urgent suggestion has reached the writer from a distant country that such statements of cost to be really most serviceable should give the details in days of labor, in weight of iron, and in number of brick, and to this an assent is most cordially yielded. It is true, however, that the mere labor of copying arid compiling these details to such a degree of minuteness, would be very great, and, in any event, the probable difference between the plans of an existing establishment and one projected, would be so wide as to render even so complete a statement of cost of little more real service than the approximate notes given herewith.

Jan 1, 1879

By P. Barnes

THE sums given in the accompanying table are those actually paid for material and labor up to about August, 1875; but, as some parts of the machinery were not wholly completed at the starting of the works in September, 1875, the statement cannot be taken as an absolutely correct note of the total cost. A complete description, with engravings of the building and machinery, was given in Engineering, April 26th, 1878, in a paper by Messrs. A. L. Holley and Lenox Smith, to which convenient reference may be made. A detailed list of the construction accounts has been given in a paper, by the present writer, in vol. vi, Transactions of the Institute. A summary is given in the table of the items in each class which enter into the total cost, and also a note of the proportion which each of these items forms of the whole. A concise view may thus be obtained of the facts embodied in the statement, as a whole, even though it cannot lay claim to completeness in showing the entire or final cost. An urgent suggestion has reached the writer from a distant country that such statements of cost to be really most serviceable should give the details in days of labor, in weight of iron, and in number of brick, and to this an assent is most cordially yielded. It is true, however, that the mere labor of copying and compiling these details to such a degree of minuteness, would be very great, and, in any event, the probable difference between the plans of an existing establishment and one projected, would be so wide as to render even so complete a statement of cost of little more real service than the approximate notes given herewith.

Jan 1, 1879

By J. J. Egan, A. B. Kinzel

Much work has been done recently in an attempt to analyze the physicochemical mechanism involved in the production of steel by the open-hearth process. This has resulted in reducing the process to a series of interrelated phenomena obeying the usual laws of mass action and diffusion. Of these, the reaction of the iron oxide and carbon in the molten steel is of most interest from a technical point of view as it constitutes the main action in the usual steelmaking processes. A. L. Feild' has formulated a basic differential equation expressing the open-hearth reactions and Herty has done considerable experimental work on the determination of a number of constants involved in the basic open-hearth reaction. In considering the application of the law of mass action to the reaction FeO + C + CO + Fe, the iron will be taken as constant, as is the case in the open hearth and the carbon monoxide pressure will be assumed constant at one atmosphere. From this xy = m at equilibrium, where x is the percentage weight of carbon, y percentage weight of iron oxide and m the weight-concentration equilibrium constant. While it is customary for physical chemists to express equilibrium constants in terms of molar concentrations, the constant is here expressed as the product of the percentage-weight concentrations for ease of comparison with the constants quoted by Herty and by Beild, and for more ready applicability to the open-hearth reactions. Herty and his associates have attempted to calculate the value of this constant from data on open-hearth heats. So many variables affect these results that an adequate calculation presents very great difficulties. A value of 4 X lop2 was first arrived at, but this was later changed to 1.6 X 10-2. Feild, in order-to illustrate the operation of the differential equation of the open hearth, has assumed a value considerably lower than Herty's, namely, 1.0 X 10-2, the largest value consistent with certain theoretical

Jan 1, 1929

By Henry M. Howe

SECTIONS 1. INTRODUCTION.—In this investigation the meltingpoint and the specific heat of certain artificial silicates were determined by the method of mixtures, using a large platinum-ball pyrometer. The silicates were placed in platinum crucibles on the hearth of a small regenerative gas-furnace (Figs. 1 and 2), and the platinum ball was placed between them. The temperature of the furnace was usually raised very slowly, the behavior of the silicates being observed as they gradually grew hotter; and their temperature was ascertained indirectly from time to time by determining that of the platinum ball, which to that end was temporarily withdrawn from the furnace and immersed in a known weight of water in a calorimeter. The weight and specific heat of water and of platinum ball being known (the specific heat of the latter approximately), it mas possible to calculate the temperature of the platinum ball, which was assumed to have been substantially that of the silicates which surrounded it in the furnace. The specific heat of the silicates also was determined by the method of mixtures. Their temperature having been determined as just described, one of them was dropped into a known weight of water in a calorimeter, whose rise of temperature was then noted. Knowing the weight and initial temperature of the silicate, its specific heat was wily calculated. The reults obtained, especially as regards the melting-point, must be regarded as first approximations. The technical difficulties encountered were so serious as to raise doubts, now from one cause, .now from another, as to the accuracy of most of the results: hence I give but a few, those which were reached without mishap, and with proper observation of the various precautions. The difficulties encountered are referred to again in Section 6. The investigation was carried out in the metallurgical laboratory of the Massachusetts Institute of Technology, and part of. The

Jan 1, 1890

By John T. Norton

In recent years, the damping capacity of metals has come to be recognized as an important index of certain types of structural change. In a number of instances, this property has proved to be particularly sensitive, but insufficient work has been done to permit a general interpretation. There is considerable question at the present time as to just what factors are responsible for the internal dissipation of energy when a metal is carried through a cycle of stress, and these factors must be ascertained if the value of the damping method as a metallurgical tool is to be determined. Since internal stresses are among the chief causes of dissipation of internal energy, or damping capacity, it was thought that a study of the changes in damping during the recovery and recrystalliza-tion of a cold-worked metal might throw some light upon the subject, particularly if the damping changes were correlated with other properties that are better understood. Probably more work has been done on the recrystallization phenomena of alpha brass than on any other metal, so this was chosen as the material for the present investigation. Damping measurements on brass have been made by Förster and Köster.1 They showed that the annealing of a brass that had been cold-drawn to 50 per cent reduction produced a rapid fall in the damping, a flat minimum occurring at approximately the temperature of recrystallization. The damping remained at a low value until grain growth was well under way and then it increased rapidly with increasing grain size. Köster and Rosenthal2 continued the work in greater detail. They pointed out that the damping decrease does not correspond to the hardness drop but occurs at a lower temperature, suggesting that the relief or redistribution of internal stresses has a large effect while the actual recrystallization effect is small. They also show the increase in damping at the higher annealing temperatures. Their curves are reproduced in Fig. 1.

Jan 1, 1940

By John T. Norton

In recent years, the damping capacity of metals has come to be recognized as an important index of certain types of structural change. In a number of instances, this property has proved to be particularly sensitive, but insufficient work has been done to permit a general interpretation. There is considerable question at the present time as to just what factors are responsible for the internal dissipation of energy when a metal is carried through a cycle of stress, and these factors must be ascertained if the value of the damping method as a metallurgical tool is to be determined. Since internal stresses are among the chief causes of dissipation of internal energy, or damping capacity, it was thought that a study of the changes in damping during the recovery and recrystalliza-tion of a cold-worked metal might throw some light upon the subject, particularly if the damping changes were correlated with other properties that are better understood. Probably more work has been done on the recrystallization phenomena of alpha brass than on any other metal, so this was chosen as the material for the present investigation. Damping measurements on brass have been made by Förster and Köster.1 They showed that the annealing of a brass that had been cold-drawn to 50 per cent reduction produced a rapid fall in the damping, a flat minimum occurring at approximately the temperature of recrystallization. The damping remained at a low value until grain growth was well under way and then it increased rapidly with increasing grain size. Köster and Rosenthal2 continued the work in greater detail. They pointed out that the damping decrease does not correspond to the hardness drop but occurs at a lower temperature, suggesting that the relief or redistribution of internal stresses has a large effect while the actual recrystallization effect is small. They also show the increase in damping at the higher annealing temperatures. Their curves are reproduced in Fig. 1.

Jan 1, 1940

By G. S. Brooks, L. G. Duncan

During the past few years, the Mineral Point Zinc Co. has had under consideration the improvement of various types of gas-filtering apparatus used in the removal of dust from crushing and milling plants, in the manufacture of oxide, and on blast-furnace fume and sintering furnaces. The original equipment of the various plants of the company was, of course, along lines of the standard stationary bag house. These houses required large surfaces, hand shaking, and varied only in the manner of the collection of solids and in the distribution of the gas. , Early in 1908, the first trial of a mechanical bag house was made at Nassau Plant at Depue, Ill. The duty of this installation was on dust-laden gas from a fine-crushing mill. The Printz and Rau bag machine was finally adopted and put into operation. This ingenious machine embodied what were then to us two novel features in bag-house practice: 1. An intermittent crinkling and snapping of the filtering fabric to free the meshes of solids. 2. A reversal of gas flow for a short period by a temporary connection with the suction trunk. This equipment worked fairly well except in cold weather, when we ran into condensation troubles. Had we at that time understood more fully some of the limitations of fabric filtering work, these might well have been remedied. We were impressed by this experience, however, with the efficiency of sudden tension on the fabric under suction. After a study had been made of some of the western blast-furnace houses using the reversal-of-flow feature, experiments were started early in 3 914 with a view to developing an automatic equipment along the best lines of our past experience. The objects sought were: 1. Keeping labor out of the houses for hygienic reasons. 2. Reduction of labor costs. 3. Reduction in size of bag houses. 4. Accessibility. 5. Ability to handle relatively hot gases where required.

Jan 1, 1918

By John Norton

IN recent years, the damping capacity of metals has come to be recognized as an important index of certain types of structural change. In a number of instances, this property has proved to be particularly sensitive, but insufficient work has been done to permit a general inter-pretation. There is considerable question at the present time as to just what factors are responsible for the internal dissipation of energy when a metal is carried through a cycle of stress, and these factors must be ascertained if the value of the damping method as a metallurgical tool is to be determined. Since internal stresses are among the chief causes of dissipation of internal energy, or damping capacity, it was thought that a study of the changes in damping during the recovery and recrystalliza-tion of a cold-worked metal might throw some light upon the subject, particularly if the damping changes were correlated with other properties that are better understood. Probably more work has been done on the recrystallization phenomena of alpha brass than on any other metal, so this was chosen as the material for the present investigation. Damping measurements on brass have been made by Förster and Köster.1 They showed that the annealing of a brass that had been cold-drawn to 50 per cent reduction produced a rapid fall in the damping, a flat minimum occurring at approximately the temperature of recrystal-lization. The damping remained at a low value until grain growth was well under way and then it increased rapidly with increasing grain size. Köster and Rosenthal2 continued the work in greater detail. They pointed out that the damping decrease does not correspond to the hard-ness drop but occurs at a lower temperature, suggesting that the relief or redistribution of internal stresses has a large effect while the actual recrystallization effect is small. They also show the increase in damping at the higher annealing temperatures. Their curves are reproduced in Fig. 1.

Jan 1, 1940

MARCEL R. DALY (communication to the Secretary?).-The fundamental disagreement between Eugene Coste and the writer proceeds essentially from the contradictory views they hold on the origin of petroleum. This difference cannot be bridged, nor can inorganic and organic theories be discussed here. The writer has suggested that the proper thing in such a case would be to agree to disagree. Coming to the detailed objections further presented by Mr. Coste, the writer feels that, in the main, they take their source in a wrong interpretation of the theory, and the writer is sometimes too generously invested with views that are not his own. 1. The only requirement for the theory is that the oil proceeding from organic remains be distributed in a water-laden sediment, and that this sediment be submitted to the increasing compression due to the continuous accumulation of superimposed strata, which would tend to squeeze out the liquid contents (p. 1152). This squeezing out would be further aided by the distortion of the strata (p. 1148, a). Nothing here makes impossible the slow formation of the oil, if this is considered necessary, as the piling up of the strata in the syncline would require by itself a protracted length of time, and, further, the squeezing-out process is a slow one. Possibly the formation of the oil may even continue during part of the process of distortion. But the mode of formation of the oil and the time and temperature required for it are left to the chemist to decide. The diastrophic theory, which is essentially a theory of motion and accumulation dependent on the laws of mechanics, is not directly concerned with them, provided the general points heretofore outlined be agreed upon. Perhaps it would be wise not to claim too many "eons" for the formation of the hydrocarbons, if the statement made by Sir Boverton Redwood is correct that "the coral reefs of the Red Sea are charged in places with recent petroleum, formed in that torrid climate from the swarming organisms occupying the shallow pools."1

Jan 5, 1917

By E. N. Aqua, C. M. Owens

The microstructure in cold-rolled Zircaloy-4 sheet has been characterized by transmission electron microscopy and X-ray diffraction line-broadening techniques. The rate of work hardening is measured in terms of microstrains, particle sizes, micro hardness, the tensile yield strength. The tensile yield strength of Prestrained (less than 10 pet) Zircaloy-4 sheet is found to be a linear function of the square root of the dislocation density, us predicted by work-hardening theories. ZIRCALOY is one of the most important structural alloys for nuclear reactor applications.''2 In order to understand the effects of the nuclear environment on Zircaloy structural members, the preirradiation microstructure must be characterized. This report will describe the substructure existing in cold-rolled Zircaloy-4 sheet as observed by electron microscopy and by X-ray diffractometry. I) EXPERIMENTAL PROCEDURE Commercial Zircaloy-4 strip was cold-rolled and annealed in argon at 760°C for 1 hr. The annealed sheet was again cold-rolled to a maximum of 50 pct reduction in thickness with segments of the strip being retained after 2.5, 5, 10, and 20 pct reductions. One-inch-square portions were chemically polished (50 parts HNO3, 50 parts H2O, 10 parts HF) and mounted onto lucite blocks using double-sided tape to prevent bending during handling. Thin foils suitable for transmission electron microscopy were prepared from each of the sheet samples. The sheets were mechanically polished through 600-grit paper to a 3 to 4 mil thickness and were chemically polished by immersion for 1 to 2 min in a solution containing: 50 parts HNO3, 50 parts H2O, and 10 parts HF, and rinsed in distilled water. The final metallographic procedure was to electropolish for less than 10 sec with an electrolyte of 10 parts perchloric acid and 90 parts glacial acetic acid, at 20 v, at room temperature using stainless-steel point cathodes and a vigorous stirring action. These foils were examined in a Philips EM 200 electron microscope using a 100-kv accelerating voltage.

Jan 1, 1968

By Lyall Zickrick

As a result of the studies on recrystallization and crystal growth made in this laboratory, certain theories have been developed. These are expressed briefly in a paper by Dean and Hudson.1 One of the principal points brought out in that paper is that in the deformation of a crystal, the energy supplied is distributed to the atoms of the lattice, probably by the forced formation of molecules. It is found that a Maxwellian distribution of the energy among these atoms will account for the grain growth at various temperatures. According to such a distribution the number of atoms with energy above a certain critical value, E, necessary for recrystallization at the absolute temperature T is given by n Ne(-E/kT) where N is the total number of atoms. It is apparent that if this line of reasoning is correct, a metal which has been cold-worked and reheated to a temperature below that of complete annealing will have the atoms with the higher energy recrystallized, that is, reduced to normal energy and there will remain only atoms below a certain energy. If this metal is again cold-worked the peak in the number-energy distribution curve will be displaced toward the regions of lower energies, that is, higher temperature of recrystallization. By a repetition of this process the position of this maximum and hence the recrystallization temperature of the metal could be raised considerably. In order to' check this theory, experiments have been made on copper wire. The wire was drawn from 1/4-in. rod to 22 B & S gage and then sample lots were annealed at 400 and 220° C., respectively. The wire annealed at 400° C. gave an elongation of 34 per cent., whereas that annealed at 220° C. gave only 23 per cent. These wires were then drawn by identical practice to 34 B & S gage and the elongation determined after an anneal of 3 mm. in an oil bath held at various temperatures.

Jan 1, 1927

By J. B. Newkirk, W. G. Martin

Oxidized cobalt powder is known to have a magnetic hysteresis loop which is asymmetric with respect to the magnetization axis. The experiment described herein shows that the orientation relationship between the basal plane of hexagonal cobalt and the oxide which forms upon it at 400°C is {111}ux//{100.1 }co <110>ux//<11.O> This orientation relationship allows a magnetic interaction between the antiferromagnetic oxide and the ferromagnetic substrate which could account for the offset hysteresis loop. Oxidized nickel powder has a symmetrical hysteresis loop and so is apparently not influenced by any magnetic interaction between metal and oxide. The orientation of the oxide (cubic) was found to be identical with that of the nickel substrate when the oxide forms on a polished surface parallel with {111} Ni. IN 1956 W. H. Meiklejohn and C. P. Bean discovered that fine particles of cobalt which had been prepared in a certain way have a magnetic hysteresis loop which in a strong field is asymmetric relative to the magnetization axis.&apos; The cobalt powder exhibited this unusual magnetic property only after it had been oxidized in air or oxygen; it lost the shifted hysteresis loop when the oxide was reduced in hydrogen. X-ray and neutron diffraction&apos; experiments showed the presence of cobaltous oxide (COO) and hexagonal cobalt in samples exhibiting the biased hysteresis loop and specifically showed no indication of any other compound with the exception of mercuric oxide.* The magnetic hysteresis loop becomes symmetrical above the Nee1 temperature (paramagnetic state) of COO. Therefore, it was concluded that the anomalous magnetic behavior is associated with the influence of cobaltous oxide upon the metallic cobalt. It has been proposed that crystallographic coherency may exist between the cobalt and a plane of some antiferromagnetic material which has unbalanced spin distribution and sufficient magnetic anisotropy to hold its spin in the direction which existed when the specimen was cooled. COO has these properties. Therefore, Roth&apos; has suggested that cobaltous oxide may form with a {111} plane parallel and coherent with the basal plane of the hexagonal cobalt metal and proposed that, as consequence of the antiferromagnetic interaction between COO and the underlying cobalt, the magnetization direction in oxidized fine Co particles may be ro-lated from the easy c-direction.2 Such a relationship, he proposed, would explain the observed magnetic effect in oxidized cobalt powder. The main purpose of this study was to determine the orientation relationship, if any, between the basal plane of cobalt and the oxide which forms upon it. Attempts to produce a film of COO which was strong enough to be handled were not successful. However we did succeed in making a film of CoCo2O, which was strong enough to be removed from the cobalt substrate and mounted on an electron-microscope grid. Because of the close structural similarity of COO and CoCo2O, we believe the orientation relation found for CoCo2O, on cobalt probably also holds for COO on cobalt. The epitaxial relationship of NiO and Ni also was investigated. To date no shifted hysteresis loop has been observed with nickel powder. However, the similarity of atomic array in cobalt and nickel leads to the prediction that a {111} of NiO may be parallel with a (111} of nickel. Experimental Method Cobalt-Cobalt Oxide—A coarse-grained specimen of a (hexagonal) cobalt was prepared by allowing a large crystal of fee cobalt to transform slowly at 400°C. The crystal was then cut to expose a surface parallel with the basal plane. A back reflection Laue X-ray photograph showed that the 00.1 plane was within 2" of the cut surface. The surface was mechanically polished and then electro polished in 85 pet orthophosphoric acid after which the crystal was held for 30 min at 400°C in air. During this heat-treatment the surface darkened slightly due to the oxide film which formed. The film was not thick enough to give an X-ray diffraction pattern, even by a glancing-angle technique. Glancing-angle electron diffraction was not possible either, owing to the interference of the electron beam with the high magnetic fields which exist at the 00.1 surface of the cobalt. However, it was possible to make an electron-diffraction photograph of the oxide film by stripping it from the cobalt substrate using the method described later. By maintaining reference marks carefully, it was possible to preserve the orientation relationship between the stripped film and the substrate on which it was formed. The oxidized surface of the crystal was first covered with a 1 pet solution of collodion (cellulose nitrate) in amyl acetate. When the film was dry, small rectangles were scored on the surface with a needle point. The specimen was then repolished

Jan 1, 1959

By G. S. Brooks

DURING the past few years, the Mineral Point Zinc Co. has had under consideration the improvement of various types of gas-filtering apparatus used in the removal of dust from crushing and milling plants, in the manufacture of oxide, and on blast-furnace fume and sintering furnaces. The original equipment of the various plants of the company was, of course, along lines of the standard stationary bag house. These houses required large surfaces, hand shaking, and varied only in the manner of the collection of solids and in the distribution of the gas. Early in 1908, the first trial of a mechanical bag house was made at Nassau Plant at Depue, Ill. The duty of this installation was on dust-laden gas from a fine-crushing mill. The Printz and Rau bag machine was finally adopted and put into operation. This ingenious machine embodied what were then to us two novel features in bag-house practice: 1. An intermittent crinkling and snapping of the filtering fabric to free the meshes of solids. i 2. A reversal of gas flow for a short period by a temporary connection w th the suction trunk. This equipment worked fairly well except in cold weather, when we ran into condensation troubles. Had we at that time understood more fully some of the limitations of fabric filtering work, these might well have been remedied. We were impressed by this experience, however, with the efficiency of sudden tension on the fabric under suction. After a study had been made of some of the Western blast-furnace houses using the reversal-of-flow feature, experiments were started early in 1914 with a view to developing an automatic equipment along the best lines of our past experience. The objects sought were: 1. Keeping labor out of the houses for hygienic reasons. 2. Reduction of labor costs. 3. Reduction in -size of hag houses. 4. Accessibility. 5. Ability to handle relatively hot gases where required.

Jan 11, 1917

By Henry M. Howe

This paper is a discussion of the extremely valuable one of Mathewson and Phillips, The Recrystallization of Cold-Worked Alpha Brass on Annealing,1 which not only gives us a wealth of important data reached with great intelligence, but also shows both uncommon powers of imagination and a perfectly fair spirit. Let me try to analyze some of their results, and to enunciate some of the laws to which these results point. For brevity I refer to them as "The Authors." The page numbers in parentheses refer to their paper. 1. The Visible Aspects of Recrystallization.—Plastic deformation in a single direction, as in cold-rolling, draws the grains out in that direction, that is, inequiaxes them, without destroying their apparent individuality. Each grain seems to endure the drawing out without changing either its volume or its orientation materially, for the etching tint of each grain seems to be as uniform after as before the drawing out, save for the "etch bands,"2 shown in Figs. A to D of the Authors&apos; Plate I. As the drawn-out metal is heated progressively, on reaching a certain "disintegration temperature" these old grains seem to break up, probably into submicroscopic fragments, and this apparent disintegration is followed by a coalescence of these fragments, so that their number decreases and their size increases, till they may become very much coarser than before the drawing out. Ruder3 coarsened the grains of silicon steel in this way till single grains reached an area of 50 cm. (7.75 sq. in.). The deformation itself probably breaks each grain up into many very small fragments, but the fact that each grain continues to have a uniform etching tint different from that of its neighbors indicates that these fragments retain the initial common orientation of the grain. The apparent disintegration which we observe, then, is rather an abandonment of community of orientation for individuality of orientation, by the fragments formed earlier during the deformation. Hence we

Jan 1, 1917

By R. J. Charles, G. Agar

Experiments on single particles show that the amount of material created during impact that is finer than any chosen size is proportional to the energy of the impact. As the underlying principle of comminution, it might be stated that each unit of energy input to a given comminution system tends to add to the system an identical assembly of new particles and subtract an equivalent volume of larger particles. Thus, two of the consequences of the fact that each unit of energy tends to add identical assemblies of new particles to the system are: 1) on continued application of energy the total charge in any batch comminution system tends to assume the characteristics of this assembly, and 2) the process of comminution may be described by a relationship such as E = Ak-a. Recently Schuhmannl presented a theory of comminution which puts rational perspective on the extensive controversy surrounding most of the existent theories of comminution. With hindsight the origin of controversy can be ascribed to a relatively simple circumstance. In general, a progressive shift of a size distribution curve towards finer sizes is observed as energy is added to a comminution system. It is also observed that, with continued grinding, the size distribution curves usually change and appear to approach some constant shape. Inves-tigators generally felt that an appropriate method of relating and generalizing such data would be to consider the hypothetical case where particles in the system were uniformly subjected to comminution such that each of these particles, receiving its proportion of input energy, was transformed into a number of smaller particles of uniform size. Since the changes in shape of the size distribution curves during size reduction were clearly associated with the coarse particles in the system, it was also assumed that these changes accounted for little of the input energy and one could deal solely with the equilibrium shape towards which the size distribution curves tended. Although the unrealistic nature of the foregoing points of view was realized some justification was felt for such treatments since, in most cases, the resulting mathematical formulae could, by the adjustment of at most two parameters, satisfactorily describe experimental observation. Difficulties arose, however, in that the formulae required a specific influence of the feed size on the comminution process. In actual fact, the application of a feed size term in fitting experimental data was often found to be unnecessary or contrary to the above formulae. Secondarily, much discussion arose concerning the appropriate energy number that would relate the size change of one particle to the amount of comminution energy it received. As has been previously shown3 all the above theories that treat comminution as a continuous process of size reduction may be related to a proposition of the following form: dE = -Cfn [1] where dE is the increment of energy, dx is the size change, x is the particle size, and C and n are constants. It is now clear, as pointed out by Schuhmann, that Eq. 1 is inapplicable to comminution processes, since comminution cannot be considered other than as a discontinuous mixing process in which the overall size distribution of the product results from mixing, in various proportions, finished material with unfinished, and sometimes untouched, material. A striking illustration of this mixing phenomena may be obtained by comparing the size distributions of grinds in a typical batch ball mill with size distributions calculated on the basis of mixing various proportions of feed material with a ground material which obeys a power law size distribution relationship. Figs. la and lb illustrate such a comparison and the similarity of these figures indicates that mixing plays an important role in determining the overall shape of the product size distributions. Figs. la and lb illustrate, additionally, the underlying basis of the comminution theory presented by Schuhmann.&apos; In the preliminary grinding of relatively close sized feed particles in a batch ball mill, one may visualize that, when a successful encounter of a ball with a feed particle occurs, then the particle undergoes severe size reduction and the size range in which the resultant particles reside is far removed from the size of the feed particles. After a number of feed particles are reduced by independent but similar impacts and one examines the size dis-

Jan 1, 1961