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By G. H. Ashley

THE Pittsburgh coal bed stands today: as probably the largest contributor of wealth of any single mineral deposit in the world. If it is not, what other deposit is? To the present it has contributed more than 2,530,000,000 tons of high-grade coal from Pennsylvania alone, worth nearly $4,000,000,000. Since 1910 it has added more than $2,500,000,000 to the value of Pennsylvania's mineral output. There is estimated to be about three times as much coal still in this bed as has been mined. To realize the full value of this wonderful bed it must be remembered that the figures given are for one State only. To them should be added the figures for the same bed from West Virginia, Ohio and Maryland. Furthermore, as known by man, this great deposit is only a fraction of its original whole. Outliers in Somerset County, Pa., indicate that its original extent in Pennsylvania in an east and west direction was more than two times its present extent. Add to that the northward extension as indicated by outliers in northern Allegheny, Armstrong and Indiana counties,, and it seems safe to say that its original extent was not less than three times the area at present underlain by it. And as the subjacent beds of the Allegheny group are found still further eastward and northward, it is at least a possibility that it originally covered an area many times its present area.

Jan 10, 1926

Discussion of the paper of THEODORE P. HOLT, presented at the Salt Lake meeting August, 1914, and printed in Bulletin No. 91, July, 1914, pp. 1699 to 1708. F. S. SCHMIDT, Salt Lake City, Utah.-Any furnace that can make a chloridizing roast to yield an extraction of 92 to 93 per cent. and do this at a cost of less than 24c. per ton in a 10-ton unit opens great possibilities for the treatment of certain classes of ores. This cost does not include the salt and will be reduced to about 16 1/2c. per ton in the 35-ton furnace which are now being designed. On a trial run the roaster treated 9.6 ton: of Ontario stope fillings crushed to pass a ¼ -in. opening. The ore is well adapted to chlorination with the exception of insufficient sulphur and occasional days of high lime, but is not adapted to any other process The following is an analysis of the crude ore: Ag, 9.52; Au, 0.029 oz. Pb, 0.71; Cu, 0.11; SiO, 79.4; Zn, 0.57; S, 1.00; Fe, 7.9; Mn, 0.89 CaO, 1.20 per cent. The composition of the mix was: Per Cent. Dry crude ore : 83.4 Moisture 4.4 Salt 8.3 Coal dust 2.3 Pyrite, 70 per cent. pure 1.6

Jan 11, 1914

By E. J. Hall

(Butte Meeting, August, 1913.) THE iron-nail method of assaying has been used for a number of years, but has not met with the approval of all assayers. The method possesses advantages which may be given as follows : (1) no preliminary treatment is required ; (2) a lead button of proper size can be obtained (3) it is economical. On, the other hand, it has its disadvantages, which may be summed up as follows: (1) it is not applicable to ores containing large amounts of impurities other than sulphur, as practically all the base metals will contaminate the lead button ; (2) the slag is unsatisfactory in the larger number of fusions; (3) the method was known to give low silver results under certain conditions and the gold results were questionable. It was with the idea of determining the extent of this latter disadvantage that the following investigation was undertaken. It is well known that the fusion obtained in the lend assay is far more satisfactory than that in the " nails method " for gold and silver. The principal difference in the charges as a class is the presence of considerable reducing agent in the lead charge, and a limited oxidizing action in the nails charge, due to PbO. The possibility of improving the nails fusion by simulating the lead charge was the reason for using argol in some tests, even though there were reasons for expecting this would have -au objectionable effect on the results.

Jan 6, 1913

By R. V. Whetsel, V. R. Garfias

Petroleum production in the Mexican fields during 1932, estimated at 32,400,000 bbl., was only 564,000 bbl., or about 2 per cent less than the 1931 total. Production in the northern fields declined approximately 1,100,000 bbl., the Tehuantepec output showed a drop of 340,000 bbl. and the South fields gained 865,000 barrels. Wildcatting continued at a reduced rate, the only successful completion being Presa No. 2 well which at a depth of 1535 ft. produced about 7,000,000 cu. ft. of gas. This well is an offset to Alberca No. 1 completed during 1931. General conditions in the petroleum industry coupled with the additional burden of the 21c per bbl. duty on oil imported into the United States further discouraged development activity in Mexico during 1932. Production of the Mexican fields in 1932 was distributed as follows: Production (U. S. Barrels) 1931 1932 _______________________________________________1________________________ Northern fields.................................... 14,092,000 13,000,000 South fields....................................... 10,535,000 11,400,000 Tehuantepec fields............................... .. 8,000,000 32,964,000 32,400,000 Since their discovery to the end of 1932, the fields have produced as follows: (U. S. Barrels) Northern fields..................................... 681,300,000 South fields........................................ 967,200,000 Tehuantepec fields.................................. 40,540,000 1,689,040,000 The tremendous productivity of the Mexican wells and the very small number actually drilled in the proven areas is shown in the following table:

Jan 1, 1933

By E. P. Barrett

THE high-frequency laboratory induction furnace with a rotating liquid crucible enables research workers to conduct certain investigations heretofore very difficult or impossible to realize because vessels are not obtainable that are capable of resisting the physical conditions or the chemical actions to which they are subjected. Applications for patents covering commercial uses of centrifugal liquid crucibles were filed in the United States in 1919,1 in France in 1925, in the United States and Germany in 1926,2 and in France in 1927.3 In 1928, Schuette and Maier,4 of the Bureau of Mines, reported the construction of a whirling table beneath a high-frequency induction furnace. SHAPE AND SIZE OF CENTRIFUGAL LIQUID CRUCIBLES When a vessel containing a liquid is rotated, the inner surface of the liquid takes the shape f a paraboloid under the simultaneous action of centrifugal force and gravity. The internal dimensions of the paraboloid rotating liquid crucible are governed by the diameter of the container and its speed of rotation. Melted Wood's metal was poured into cylinders 2 ½ in. in diameter, which were rotated at 180, 300, and 468 r.p.m. When the metal was solid, a slurry of plaster of Paris was added, and rotation continued until the plaster had set. Fig. 1, a photograph of sections f the cylinders, shows the effect f speed f rotation of the containers upon the shape f the inner surface f the rotating liquid crucibles.

Jan 1, 1938

ARTICLE I: NAME AND OBJECTS Section 1: This Division shall be known as the Iron and Steel Division of the American Institute of Mining and Metallurgical Engineers. Section 2: The objects shall be to furnish a medium of cooperation between those interested in the metal-lurgy and industry of iron and steel manufacture and use; to represent the A. I. M. E. in so far as ferrous metallurgy is concerned, within the rights given by A. I. M. E. By-law XVII, Section 3, and not incon-sistent with the Constitution and By-Laws of the A. I. M. E.; to hold meetings for social intercourse and the discussion of ferrous metallurgy; to stimulate the writing, presentation and discussion of papers of high quality on ferrous metallurgy; to reject or accept such apers for publication and distribution by-the A. I. M. E. within the limits of the funds available for such purpose. ARTICLE II: MEMBERS Section 1: Any Member, Associate, or Junior Asso-ciate of the A. I. M. E. in good standing may become a Member, Associate or Junior Associate of this Divi-sion upon registering in writing a desire so to do. Section 2: But no one who has been continuously indebted to the. A. I. M. E. or to this Division for more than three months shall be entitled to vote or to receive publications to which, as a member of the Division, he would be entitled.

Jan 7, 1928

By Frederic P. Dewey

Having shown1 the difficulty of assaying so-called cyanide bullion and the extreme variations often found in the results, an investigation was undertaken to discover, if possible, the causes of these variations by a series of tests upon the specific action of various metals during cupellation. Zinc.—In order to test the effect of zinc, 48 assays were made in sets of 6, 2 rows of 3. The charge for the middle cupels consisted of 500+ mg. Au, 1,125 mg. Ag, 10 mg. Cu. To the end cupels 50, 75, 100 and 125 mg. Zn were added, and a set of each proportion was cupelled with 4 and 8 grams Pb. The cupels were assayed and showed the following gold contents in milligrams, the figures being arranged as the cupels stood in the muffle: In many instances the zinc does not appear to affect the cupel gold, but various exceptions are apparent, generally in the cupels in the back row. With 100 and 125 mg. Zn, in some cases the Zn burned with its characteristic flame' before it could alloy with the other metals. Also, less fusible oxidized lumps were observed during the cupellation and some cupels showed a scum. In order to lessen the premature burning out of the Zn, an alloy of 2 parts Ag to 1 part Zn was used. A uniform charge of 500+ mg. Au,

Jan 1, 1918

By Frederick K. Allgaier

As part of an ongoing research program, the Bureau of Mines, U.S. Department of the Interior, is monitoring surface subsidence over six longwall panels at three Utah coal mines. These sites are characterized by mining depths of 244 to 610 meters (800 to 2,000 ft .), thick and massive sandstone layers in the overburden strata, multiple seam mining, extraction heights of approximately 1.8 to 3 meters (6 to 10 ft.), and rugged surface topography. Maximum subsidence, angle of draw, timing relative to mining, horizontal strain, and rate of subsidence development are being determined and correlated with mining and geologic variables. Results to date indicate the maximum vertical subsidence over the monitored panels ranges from 0.6 to 0.9 meters (2 to 3 ft.). The major factors controlling the amount of subsidence are the panel dimensions and the status of adjacent panel mining. Only minor surface cracking at the panel ends was evident at any of the sites. In all cases, there was a time lag of several months between the start of mining and subsidence at the surface. As subsequent panels are monitored and additional data become available, better estimates of the effect of various site characteristics on the subsidence will be possible. Ultimately, improved prediction capabilities will allow mine operators in the West to evaluate the potential for subsidence-related damage which could affect the current or future land use above the mine.

Jan 1, 1982

By W. W. Tyler, A. C. Wilson, L. B. Nesbitt

INVESTIGATIONS of thermal conductivity and impact strength of the titanium alloy RC-130-B and 316 stainless steel were undertaken because of interest in strong, nonmagnetic, commercially available alloys of low thermal conductivity for use in low temperature experiments. Measurements of electrical resistivity and thermoelectric power were also made for some of the samples studied. The titanium alloy designated as RC-130-B is manufactured by Rem Cru Titanium Inc. It contains 0.14 pct C, 3.99 pct Al, and 4.7 pct Mn. A general discussion of properties of the two phase Ti-4Mn- 4A1 alloys is given by Finlay and Vordahl.' The alloy is machinable and has a yield strength greater than 130,000 lb per sq in. at 0.2 pct offset. The 316 stainless steel sample used for both conductivity and impact strength measurements was obtained from the Allegheny-Ludlum Steel Corp. and is designated as Allegheny metal 18-8M, Type 316, Grade 316. The sample had received 25 pct minimum final cold reduction and had a Brine11 hardness rating of 255. Several impact tests were made on a sample of 316 stainless which had not received the 25 pct cold reduction. Also several data points are reported giving thermal conductivity and electrical resistivity for a sample of 304 stainless steel taken from stock. Figs. 1 and 2 give thermal conductivity and electrical resistivity data for the titanium alloy and for

Jan 1, 1954

By Frank Firmstone

In 1871, two furnaces at the Glendon Iron Works, which had been blown out on account of the "coal strike," were altered from the open-top plan with side flues for collecting the gas, to closed tops with cup and cone. In one furnace the suppression of the side flues permitted a considerable alteration in the profile, but in the other (No. 5) no change in this respect was made; the side flues were simply bricked up and new ones cut through the sides close to the top. This furnace was in blast over four years, and we can, therefore, form a pretty good idea of the effect of the alterations on the furnace process. The principal dimensions are; Height 72'; greatest diameter, 18'; diameter at tuyeres, 8'; diameter of top, 10'; diameter at stock line (point at which the top of the materials is kept), 11'; cubic contents, 11,900 cubic feet. The table below shows the average results for periods of twentysix weeks each. 1st, of the open-topped furnace; 2d, of the furnace with the first charger used, which was an ordinary cup and cone (diameter of cone 5' 2") 3d, with the charger used ever since, a " double " cone 7' 5" diameter outside, having a central opening 3' in diameter. The diagram (Plate 11) shows the daily variations, in the grade of the irons for the same periods.*

By C. L. Dake

Iron is much more soluble in the ferrous than in the ferric form. Where, as in the case of the ferrous silicates and. the sulphides, the iron is already in the ferrous form, it may go at once into solution and be removed, upon the breaking down of the parent rock. If in the ferric form, it must first be reduced; usually by the decay of organic matter, the demand of the decaying carbonaceous matter for oxygen being so great that the latter is abstracted from the ferric compounds and the iron is thereby reduced and rendered soluble. The iron may go into solution as the sulphate, or in the presence of excess CO2 as ferrous carbonate. It is probably soluble as salts of the organic acids.' Recent work indicates that these are important in the formation of bog ores.2 There is considerable variety of opinion concerning the behavior of these organic compounds.3 The secretions about the roots of plants and trees also cause the solution and removal of iron and a consequent bleaching of the soil,4 While the matter is not yet well understood, we can probably say definitely that the so-called organic acids are a group of colloids which possess slightly acid properties, and the salts of which are partly soluble and partly insoluble.5 Their iron salts readily change from the ferrous to the ferric form, and their solubility is greatly modified by the presence of ammonia.

Jan 1, 1916

By H. E. Rowen

As high grade iron ore deposits dwindle and costs rise, sintering becomes more and more important. The steel industry is now faced with beneficiation problems once peculiar to nonferrous work. Succeeding articles describe recent advances in this field. Here is presented the first chapter of a history still being written. SINTERING, for the purpose of this discussion, is defined as the art of burning a solid fuel with 90 to 95 pct ash content. Considering problems of combustion involved in keeping a home furnace burning properly with 12 to 20 pct ash in the fuel, it is evident that combustion represented by the definition has to be right or nothing is going to happen. Our forefathers discovered that many ores containing metals essential to the steadily rising standards of living were associated with elements such as sulfur and arsenic, which had to be removed before refining. This they did by utilizing the solid fuels they had available-the sulfur or other readily combustible components-to create roasting heat. One of the early methods is demonstrated in an old woodcut of the roast heap, Fig. 2. Ore was broken into chunks, piled on an ignition layer of solid fuel-logs in this case-and then. ignited. The sulfide ores roasted as the sulfur burned out. As shown in the background, the countryside was rapidly denuded of all vegetation by the great quantities of SO2 and other liberated gases.

Jan 1, 1961

By Takahide Wakamatsu, Yoshiaki Numata, Charn Hoon Park

INTRODUCTION A technique is needed to apply the flotation method successfully to apply the flotation method successfully to low grade and complex ore bearing hard-to-float oxide minerals. Thus it is necessary to find a new selective, powerful collector or to develop a new flotation process. Some attempts to use two or more kinds of collectors combined in flotation have been made but the principle of the reaction between the collectors used and the surface of mineral as well as the effect of combined collectors on flotation has not yet been fully understood. As part of the study on the improvement of selective collection in flotation, we have been investigating the flotation of minerals using two kinds of organic reagents, one of which is a conventional collector. We found xanthates were able to adsorb even onto the surface of oxide mineral, with the help of another organic reagent, e.g. a chelate compound (1). Furthermore, a notable effect of combined reagents such as the xanthate-amino acid combination (2) was found on the reagent adsorption phenomena and the collection phenomena, depending on the combination of reagents. The present study was carried out to clarify the effects of adding two kinds of collectors to the collection of mineral in flotation in the following two cases: (1) joint use of xanthate and di-alkyl dithiophosphate for galena collection and (2) joint use of a cationic collector with xanthate for scheelite collection.

Jan 1, 1980

By Oliver C. Ralston, Foster Fraas

Electrostatic methods of separation are used only when some peculiar advantage is gained. Such cases are minerals that are not separable by differences in specific gravity or magnetic response and that are desired in particles as large as 10-mesh, a size on which flotation separation is inefficient. This paper covers several separations of this type and others. It includes studies in the electrostatic behavior of kyanite, sillimanite, and zircon, simple silicates that cannot be called either acid or basic but are more nearly neutral. Kyanite and sillimanite are both desired in 10-mesh size and are difficult to bene-ficiate from low-grade ores to give that type of concentrate. A separation of garnet from diopside was studied because this mixture had been removed from a wollas-tonite product by drying and magnetic separation, and no special or extra-preparation for electrostatic separation was necessary. The Separator The separator used in these tests is of the nonhomogeneous field type shown in Fig Ia. It consists of a 11.4-cm-diam rotating metal roll 2 at ground potential over which the dry mixture of minerals is fed. The roll serves as one electrode of the separating field, and the other electrode is that of 3, a smaller 5-cm-diam rotating metal cylinder which is held at a high direct-current potential. In this paper the term "electrode" will be confined to the electrode at 3, roll 2 being designated only as "roll."

Jan 1, 1949

By Shiou-Chuan Sun

Most previous work on sedimentation of coal1 and mineral2,3 suspensions has been conducted in graduated 1-liter glass cylinders of 6-cm diam. With this type of large container it is often difficult to see through the suspension and tedious to perform a large number of tests. Furthermore, the heavy glass walls and the graduation lines of glass cylinders cause internal and stray reflections, respectively. To obviate these difficulties, an Atlab Emulsion Viewer from Arthur H. Thomas Co. was adopted as an alternative apparatus. Equipment: The viewer,4 shown in Fig. 1, consists of: 1) a stainless steel frame rack holding 21 flat-bottom Nessler tubes or an ungraduated replica 1.64 cm ID and 1.80 cm OD, 2) a movable masked 150-w lumaline lamp behind the tubes, and 3) a scaled glass panel with 100 vertical divisions in front of the tubes. The tubes are snugly held by springs in slots formed by spacer bars, which also serve as shields to eliminate stray light. The lumaline lamp is mounted behind a slit in a movable housing so that it can be positioned behind the suspension to be examined. The lowest or 100-division line on the front glass plate is leveled with the upper side of the bottom of all tubes. The scaled portion of each tube, roughly 19 cm high and 40 ml in volume, is used to study coal and mineral suspensions.

Jan 1, 1959

The Institute maintains a dual relationship with students (1) an individual relationship with a Student Associate, and (2) a relationship with local organizations of students, known as Affiliated Student Societies or Student Chapters 1 The conditions of Student Associate¬ship are set forth in Section 9, Article I, of the Bylaws of the Institute (see page 74 and following pages) During 1934, sundry amendments were made for the purpose of improving the student relationship Post-graduate students are now eligible, and associateship can be maintained, with the payment of the regular dues of $2 per year, for 18 months following graduation in June With his regular dues, each Student Associate is entitled to receive during the year his choice of MINING AND METALLURGY, METALS TECHNOLOGY, MINING TECHNOLOGY, PETROLEUM TECHNOLOGY, or COAL TECHNOLOGY, and on payment of an additional fifty cents he can have both MINING AND METALLURGY and any one of the others He is accorded the privilege of getting special publications such as "The Porphyry Coppers" and "Elements of the Petroleum Industry" at the reduced prices applicable to Members, he has the privileges of the Engineering Societies Personnel Service and the Engineering Societies Library, and he is not only invited but urged to attend all meet¬ings of the Institute, its Divisions and its Local Sections The Institute wants to extend the hand of professional fellowship to students following mineral industries curricula

Jan 1, 1952

By B. Ramaswami

INTERNAL oxidation occurs readily in silver due to the rapid diffusion of oxygen in silver.' It has a marked effect on creep in polycrystalline silver2 and raises the critical resolved shear stress in single crystals of silver.3 However, the effect of oxygen on the work-hardening parameters of silver is not known. It is the aim of this paper to describe the effect of internal oxidation on the work-hardening characteristics of single crystals of silver and an Ag-0.1 at. pct A1 alloy. The materials used were: 99.99 pct Ag from Handy and Harman and 99.993+ pct A1 from Alcoa. Single crystals, 6 mm by 6 mm in cross section of silver and Ag-0.1 at. pct A1 of mo.5 orientation, i.e., the orientation with the Schmidt factor m = 0.5. were grown by the Chalmers technique.4 One set of specimens, referred to herein as oxidized specimens, was annealed at 940°C for 24 hr in a muffle furnace, in air, and furnace-cooled to room temperature. Another set of specimens, referred to as nonoxidized specimens, was annealed in oxygen-free helium at 940°C for 24 hr and furnace-cooled over a period of 7 hr to room temperature. The annealed single crystals were tested at room temperature in a floor-model Instron testing machine. The results are presented in Figs. 1 and 2. A

Jan 1, 1965

By K. A. Jackson, J. D. Hunt

A general theory for the growth of lamellar and rod eutectics is presented. These modes of growth depend on the interplay between the diffusion required for phase separation and the formation of interphase boundaries. The present analysis of these factors provides a justification for earlier approximate theovies. The conditions for stability of rod and Lanlellar structures are consitleved in terms of the mechanisms by which the structure can change. The mechanisms considered include both small adjustments to the lnnzellar spacing due to the motion of lamellar faults, and catastrophic changes due to instabilities. It is concluded that stable growth occurs at or near the minimum interface undevcooling for a gizierz growth rate. The conseqrlences of the existence of a diffusion boundary layer at the interface are discussed. The experimental results for the variation of growth rate, undercooling, and Lanzellar spacing are cornpared with the theory. We believe that the theory presented in this paper provides an adequate basis for understanding the complex phenomena of lanzellar and rod eutectic growth. The growth of lamellar eutectics has been the subject of several theoretical and many experimental studies. The foundations for the theoretical work were laid by zenerl and Brandt2 in their analyses of the growth of pearlite. Zener estimated the effect cf diffusion, and took into account the surface energy of the lamellar structure. He found that the lamellar structure could grow in a range of growth rates at a given undercooling provided the lamellar spacing was appropriate for the growth rate. Since pearlite grows with only one growth rate and one lamellar spacing at a given undercooling, there is clearly an ambiguity in the theory. Zener removed this ambiguity by postulating that the growth rate was the maximum possible at the given undercooling. He predicted then that the product of the growth velocity v and the square of the lamellar spacing A should be constant, i.e., A2v = const. Brandt2 started out by assuming that the interface between the lamellae and austenite was sinusoidal. Because of this, the ambiguity encountered by Zener did not arise. Brandt was able to obtain an approximate solution to the diffusion equation, but, since he did not take into account the surface energy, his considerations are incomplete. Tiller3 applied some of these ideas to the growth of eutectics, and proposed a minimum undercooling condition to replace the maximum velocity condition used by Zener. These conditions are formally identical. Hillert4 extended the work of Zener. He found a solution to the diffusion equation assuming the interface to be plane. Taking surface energy into account, and applying Zener's maximum condition, he was able to calculate an approximate shape of the interface. Jackson et al.5 used an iterative method employing an electric analog to the diffusion problem to refine the calculation of interface shape. It was found that the interface shape calculated from a plane-interface solution to the diffusion equation was negligibly different from the exact solution. The method provided an analog only for eutectics for which the volumes of the two phases are equal, growing from a melt of exactly eu-tectic composition. There has also been considerable experimental work on eutectics, Several experimenters8-10 found that A2v is constant as predicted by Zener.1 Hunt and chilton10 demonstrated that ?T/v1/2 is also a constant for the Pb-Sn system as predicted. Lemkey et al.11have recently found A2v to be constant for a rod eutectic. In the present paper, we present the steady-state solution for the diffusion equation for a lamellar eutectic growing with a plane interface, for the general case, that is, with no restriction on the relative volumes of the two phases, and with the melt on or off eutectic composition. A similar solution is also found for a rod-type eutectic. Expressions are obtained for the average composition at the interface and the average curvature of the interface. These equations for the average composition and curvature are similar in form to those derived by Zener1 and Tiller,3 and provide a justification for some of the approximations made by these authors. The mechanisms by which the spacing in a lamellar structure can change are considered. The important mechanism for small changes in lamellar spacing involves a lamellar fault. Examination of the stability of lamellar faults leads to the conclusion that the growth occurs at or near the extremum.* The insta- bilities which can develop in a rodlike structure are also discussed, resulting in the conclusion that this structure also grows at or near the extremum. Comparison of the conditions for rod and lamellar growth permits a prediction of the surface-energy anisotropy required to produce rods or lamellae for various volume-fraction ratios. The diffusion equation predicts the existence of a diffusion boundary layer at the eutectic interface unless the eutectic has 0.5 volume fraction of each phase and is growing into a liquid of eutectic composition. This boundary layer is such as to make the composition in the liquid at the interface approximately equal to the eutectic composition. This boundary layer permits changes in composition during the zone refining of eutectics. Photographs of the eutectic interface of a growing transparent organic eutectic system have been made. Both the components of this eutectic are transparent organic compounds that freeze as metals do.12 The in-

Jan 1, 1967

By R. W. Carpenter, J. C. Ogle

It is possible, by using pack-rolling instead of conventional rolling, to reduce a number of metals to thicknesses of 2µm or less. Such thinfoils are generally made at room temperature without intermediate annealing. In addition, pack-rolled foils fail by developing pinholes at thicknesses near 2µm instead of developing the shear cracks usually observed in cold-rolled ductile metals. This paper presents the results of a general investigation of the deformation substructure and texture developed in copper and iron pack -rolled from 130 to about 2µm thickness. Electron microscopy showed that in both metals a fine (0.2 to 0.5?µ m) deformation subgrain structure formed during pack-rolling; in neither case was this substructure grossly different from substructures formed during conventional rolling. The deformation texture formed in pack-rolled iron was quite similar to usual bcc textures; however, in the case of copper, the cube texture was stable during pack-rolling and the normal copper deformation texture was unstable. It is shown analytically that the constraining pack induced a large hydrostatic pressure in the foils during pack-rolling. The pinhole failure mechanism is attributed to the presence of the large hydrostatic pressure during pack-rolling; this strongly suppressed the growth of shear cracks. The stability of the cube texture in copper is also probably due to the unusuul stress distribution developed during pack-rolling. EXPERIMENTS at several laboratories have shown that very thin foils of the common structural metals and many of the rare earths can be made by "pack-rolling". 1-3 The technique was originally developed to make specimens for nuclear scattering experiments and foils for X-ray filters. It is also useful for making experimental laminar metallic composite bodies and foils thin enough for direct examination by ultra-high voltage electron microscopy without the need for special thinning techniques. Pack-rolling in the present context means a three-layer pack, with the material to be rolled into foil comprising the center layer. The outer two layers, which constrain the foil during reduction, are ordinarily austenitic stainless steel. Typically, a 130 µm (0.005 in.) metal strip can be reduced to a final thickness of 2 µm or less by this process. This is accomplished at room temperature, without intermediate annealing. It has been observed that foils produced by this process do not exhibit at any stage of their reduction the severe work-hardening found in strip rolled by conventional cold-rolling methods. Neither is the failure characteristic the same."&apos; Conventionally cold-rolled ductile metal strip fails by developing shear cracks on planes whose normals nearly bisect the angle between the rolling direction and normal to the rolling plane; these are planes of maximum shear stress. In pack-rolling this mechanism has not been observed; failure occurs by the formation of pinholes on the foil surface (penetrating the foil). If pack-rolling is continued the hole density increases. These differences in behavior imply the existence of appreciably different substructure in pack-rolled foils compared to substructure in conventionally rolled material, or perhaps that the geometry of pack-rolling has an effect on the foil behavior. This paper describes an investigation of deformation substructure and texture in some specimens of pack-rolled copper and iron, and some considerations of the stress distribution in the foils during rolling that result from the geometry of pack-rolling. EXPERIMENTAL DETAILS Three different materials were used for pack-rolling in the present work: soft copper sheet (99.8 pct Cu, 0.03 pct 0, electrolytic tough pitch) and two types of iron, Ferrovac E* and Armco iron. Each was "Crucible Stccl Co. initially in the form of 130 µm annealed strip with grain size ranges of approximately 10 to 40 µm. The initial texture of the copper (determined as noted below) was the normally observed cube type (001)[100]; there was evidence of a small amount of material in the cube-twin orientation reported by Beck and Hu.4 The initial texture of the Ferrovac E was similar to that reported for recrystallized iron by Kurdjumov and sachs,5 who list the principal orientations as {111}<112>, {001}<110> 15degfrom RD and a weak component {112}(110) 15 deg from RD. The starting texture of the Armco iron was not determined. Pack-Rolling Procedure. A four-high mill was used for all specimens. The work roll and backing roll diameters were 1.625 and 5.25 in., respectively. The peripheral roll speed of the work rolls was about 2.5 in. per sec. All foils were initially reduced from 130 to 100 µm by conventional straight rolling and then inserted into a pack, without any intermediate annealing, for further reduction. The pack consisted of an 0.033 in. (838 µm) thick 3 by 6 in. polished sheet of austenitic stainless steel, folded to make a 3 by 3 in. jacket. After folding, the jacket was given a small reduction to close the fold tightly before insertion of the foil. During pack-rolling a constant change in roll spacing was made every third pass. The roll-spacing change corresponded to a 5 pct reduction in thickness for a new pack. This approached a 10 pct reduction when the pack had decreased to about half its original thickness. At this point the deformed pack was discarded and a new one

Jan 1, 1970

By Nicholas J. Grant, Joseph T. Blucher

High-purity aluminum and an Al-10 pet Zn alloy zvere tested in axial fatigue from 80" to 900oF, at struzn vales of 5 and 150 pct per min, at a strain amplitude of 1 pcl. Cycles to failure were recorded as well as the load per cycle during the entive test. Several grain sizes were examined in each material. Examination was made of modes of deformation, initiation and growlh of&apos; cracks, and vecovery mechanisms such as srbgrain formation and boundary migration. Strain rate effects on cycles to failure are first observed ahoi&apos;e 50O0F, the highev vate vesulting in longer lije. Crack initiclion at room temperature may be truns-or iutercrystalline but fructures are transcrystalline. Abore 600&apos;F, crack iniliation and growth ave largely inlercvystalline. Boundary wzigratiotz to 45-deg positions is observed above 70Oo F, and fractrrves are a combination of grain bol~ndary voids and cvacks. It is only in recent years that studies of deformation and fracture which prevail in fatigue at elevated temperatures have attracted significant attention.&apos; Of such studies considerably less attention was given to high strain-low strain rate fatigue. Moreover, the majority of high-temperature fatigue studies were performed at conventional machine speeds (1000 to 10,000 cpm). As it is well-demonstrated in uniaxial creep-rupture series, at high strain rates, even at high temperatures, metals undergo work hardening with little or no attendant recovery or recrystallization thus the nature of deformation and fracture which is observed is similar to that encountered at lower temperatures.&apos;-" Thus, for example, fatigue testing of a stainless steel at 750°F does not involve high-temperature deformation processes,2 and might more correctly be termed "fatigue testing at an elevated temperature". It was the purpose of this work to study deformation and fracture in fatigue as a function of low strain rates and temperature, selecting conditions which would result in grain boundary sliding, migration, fold and subgrain formation, and intercrystalline cracking in high-purity aluminum and a high-purity A1- 10 pct Zn alloy. Grain size was an additional variable. Extensive studies of the deformation and fracture behavior of these aluminum materials in simple creep had been done in the authors&apos; laboratory, and were to serve as a basis of comparison for the observed effects in fatigue:&apos;-&apos;&apos; the range of the creep test temperatures was 80° to 1150oF. MATERIALS AND EXPERIMENTAL PROCEDURE The compositions of the 99.99 pct pure A1 and the A1-10 pct Zn alloy are shown in Table I. Button-head specimens, with a liberal fillet, of 0.20 in. diam and of gage length 0.40 in. were machined from wrought bar stock. The ratio of 2:l gage length to diameter was selected after preliminary tests showed that a shorter length gave a shorter life, probably due to end effects, and after evidence of buckling in longer gage length specimens. After machining, the specimens were chemically polished to remove the worked outer layer, and were subsequently heat-treated to stabilize the selected grain sizes. Both the high-purity aluminum and the A1-10 pct Zn alloy were heat-treated to produce grain diameters of approximately 0.5 and 2 mm in each case. These grain sizes are referred to in the text as fine and coarse grain, respectively. One lot of the high-purity aluminum was heat-treated to produce a still coarser grain size in which the cross section was occupied by 2 to 3 grains. This structure is referred to as very coarsegrained. After heat treatment, the specimens were again electropolished. To avoid complications of both stress and strain gradients in the cross section of the specimen, a hydraulic, axial fatigue machine was designed and built. A button-head specimen, 1/2 in. diam at the head, was firmly gripped in a split-type holder free of any play in the grips. The test temperatures varied from 80" to 900°F. The strain amplitude in all of the reported tests was 1 pct for a total strain amplitude of 2 pct. The strain range was set by precision micrometers and measured by a precision dial gage. Constant strain rates of 5 and 150 pct per min were selected so that high-temperature type deformation and fracture would occur in the higher-temperature tests5,6 The strains and strain rates must be regarded as nominal values because they are based on the original specimen dimensions, which changed significantly as a result of necking and crack propagation, as can be observed from Fig. 8. For the elevated-temperature tests, a thermocouple was inserted into a well in the head of the specimen; the selected temperatures could be maintained with less than ± 5oF fluctuation during the entire test. To avoid changes in grain size before the test, specimens were heated to the test temperature in less than 15 min; similarly, they were cooled to room temperature after fracture with an air blast to avoid or minimize recovery or recrystallization. During the fatigue tests, load vs strain curves were recorded by a strain gage load cell for each fatigue cycle. In addition, the maximum values of load amplitude were recorded for the entire test.

Jan 1, 1968