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By Toshimi Yamane

The internal friction of cold-worked titanium iso-thermally annealed at temperature below the recrystallization temperature was measured. The internal friction was calculated from the half width of a resonance curve of the specimen which was vibrated transversally by the electromagnetic method. The experimental results were as follows: 1) The specimens annealed for a long time at temperature below the re crystallization temperature after cold working have the strain-amplitude dependent internal friction. 2) The internal friction increased by the cold working was decreased during the isothermal annealing. The reason of decrease of the internal friction is considered to be caused by the annihi-lation of lattice defects. 3) There is a linear relation between logQt-1/Q0-1 and (1/T)2/3 below the recrys-tallization temperature, where Q0-1 is the internal friction standing 24 hr at the room temperature after cold rolling, Qt-1 is the internal friction annealed at T°K for t min. 4) The hardness of the cold-worked titanium does not change by the annealing at 300°C for a long time but decreases by annealing at 400ºand 460°C. METALS, when cold worked, show sharp changes in physical and mechanical properties' The internal friction of cold-worked metals increases sharply and has a maximum value1,2 connected with working de- grees. The increased internal friction of cold-worked metals is recovered by annealing. This phenomenon is the well known effect called Köster effect. The recovery of the internal friction occurs earlier than the changes in tensile properties, hardness, or X-ray diffraction, and is very sensitive to the structure of a metal. The mechanism of the recovery at a temperature lower than the recrystallization temperature is being considered variously by many investigators: there are such views as the annihilation of dislocations by smith,' the rearrangement of dislocations mentioned by Nowick,4 and interaction of dislocation with point defects.5 Smith and Nowick also considered the interaction but it is so difficult for them to explain the rearrangement mechanism systematically, it being not considered a special model; therefore, we do not explain it quantitatively. Experiments measuring the recovery of the internal friction of cold-worked metals were performed by Gordon and Nowick6 on NaCl, and by Smith on copper. In addition, there are many studies, particularly those of measurements on copper by other investigators. There are comparatively many investigations on aluminum and iron which are the cubic system,'-' but only a few on metals of the hexagonal system.10 In view of this, I investigated cph titanium at room temperature and measured the internal friction after annealing isothermally at temperature lower than the recrystallization temperature. SAMPLES AND EXPERIMENTAL METHOD samples for the experiment were cut from a 6-mm titanium plate. The long direction of samples was

Jan 1, 1963

By Jack White, Ralph B. Adair

THE Mufulira mine in Northern Rhodesia is 13° south of the Equator and at an altitude of 4100 ft above sea level. The concentrator was planned in 1930 to treat about 10,000 tons of ore per day, but before construction work had gone very far the size of the plant was reduced to 1500 tons daily capacity. Then just as the construction was finished in December 1931, the price of copper did not warrant the commencement of operations and it was not until October 1933 that the mine re-opened. Extensions have been made to the plant in 1034, 1935, 1936 1937, 1940 and finally in 1945. The capacity of the plant when the 1945 extension is completed will be 9500 short tons per day. The various extensions have been carried out with the minimum confusion and with great skill on the part of the designers and the erection engineers. In dealing with the plant in this paper it is proposed to give an outline of the present practice and only to refer to past practice when it is considered of particular interest. ORE TREATED The ore consists of fine grained highly siliceous, felspathic and argillaceous quartzites, the latter containing graphitic carbon and locally termed graywacke. These rocks are considerably altered near the surface and on the fringes of the ore body. Despite extensive efforts at mixing, both underground and in the crushing plant, many sudden changes of ore take place in the mill feed. The minerals are chalcocite, bornite and chalcopyrite with relatively unimportant amounts of malachite, native copper, azurite, covellite and chrysocolla. Gold is present at about 1 oz to a thousand tons, and silver at about 2 dwt. per ton. With increasing depth the nonsulphide content or, as commonly termed locally, the oxide content of the ore is decreasing and is now less than 0.25 pct against a high of 0.77 pct. CRUSHING OPERATIONS The first stage of crushing is done underground where the oversize from 12-in. grizzleys is fed to a 56 X 72-in. jaw crusher. At the Selkirk shaft two 10-ton skips deliver the run of mine ore at a rate of 450 tons per hour to the 400-ton capacity shaft bins. One 6 ft wide Ross chain feeder and one locally made air-operated finger feeder feed the two 30-in. McCully crushers. Ahead of each crusher is a 6 X 9-ft spring grizzley spaced at 5 in. on a 35° slope. Neither the Ross chain feeder nor the finger feeder is entirely satisfactory and for the wet, muddy and sticky ore that has to be handled it is planned to replace these with two 6-ft wide apron pan feeders. The McCully crushers deliver a minus 5-in. product, at a rate of over 500 tons per

Jan 1, 1947

By J. H. Lightfoot, Stuart E. Buckley

Deep drilling has led to the development of numerous pools which yield products consisting predominantly of natural gas accompanied by high-gravity water-white or slightly straw-colored liquid. Yields of this "condensate" or "distillate," as it is commonly called, vary from traces to over a hundred barrels per million cubic feet of gas. The fact that this liquid exists in the reservoir as an integral part of the gas phase and is formed by condensation attending simultaneous reduction of pressure and temperature after its entry into the well was apparently first recognized about 1932.l The nature of the physical phenomena involved in this condensation was clarified for the petroleum industry in 1933 by a report by Sage, Schaafsma, and Lacey2 of the results of an experimental investigation of the behavior of mixtures of methane and propane. Search of the literature has revealed that the condensation of liquid from gaseous mixtures by isothermal pressure reduction is not a new discovery. Kuenen was led by theoretical considerations to expect such a phenomenon, and in 1892 reported3 the results of experimental verification of his deductions. This was followed by a considerable amount of work on the phase relations of mixtures by Kuenen 4,5,6 and by 0thers,7,8 mostly in European universities. Since 1930 investigators in this country have reported experimental data on the properties and behavior of a number of hydrocarbon systems."' It is now generally known that in the presence of natural gas the solubility in the gas phase of the heavier and normally liquid hydrocarbons increases rapidly with increasing pressure above 500 to 1000 Ib. per sq. in. Thus, at pressures of 2500 Ib. per sq. in. or higher a gas may contain appreciable quantities of hydrocarbons with normal boiling points as high as 6o0°F., which in turn may be condensed from the gas phase by the reduction of their solubility therein attending pressure reduc-tion. The combined effects of pressure and temperature on condensation and vaporiza-tioi of mixtures are most readily visualized by the study of phase diagrams. Since the construction, application, and interpreta-tion of such diagrams have been described fully in readily available literature, 18-20 this paper will not review the theoretical aspects of this subject. While the behavior of gas-distillate sys tems is now clearly understood, at least in a qualitative way, most of the published work deals with the results of laboratory studies of binary systems or of synthetic mixtures of hydrocarbons, and although several systematic investigations of the effects of separator pressure and temperature on the yields of liquid product from gas-distillate wells have been made21,12z it appears that in all cases the limitations have precluded the construction of even approximately complete phase diagrams for naturally occurring systems. There has 2

Jan 1, 1941

By H. F. Silliman, Daniel R. Hull, John R. Freeman

In the normal operation of a brass-rolling mill, sheet and strip has, for the most part, been finished in comparatively thin gauges, involving a substantial amount of cold-work and a considerable number of anneals. This condition has been disturbed by the preponderance of cartridge brass, which is not rolled to thin gauges, and particularly by brass for artillery cartridge cases, on which the mill may finish its work at a thickness between 0.400 and 0.900 in. Obviously, the amount of rolling and the number of anneals to which such a product can be subjected are small compared with strip that is carried to a thickness of a few hundredths of an inch. As a result, critical examination into the internal condition of metal has been made on an extensive scale at a stage of manufacture that would not, in normal times, have been chosen for complete inspection. Under these conditions, a type of defect has been recognized that is not seen at thinner gauges. It might be more accurate to call it the appearance of a defect, since it refers to an apparently laminated, discontinuous structure, which, in fact, does not exist as such, and disappears after suitable treatment. For this reason it has been called a phantom lamination, which the authors consider an appropriate term. It is the purpose of this paper to describe the phenomenon and the conditions of its occurrence and, at least tentatively, to discuss its nature and cause. Great numbers of phantoms may be found in 2:r brass, either hot-rolled or cold-rolled. They are also found in 70-30 brass, sometimes when hot-rolled and generally when cold-rolled. It is not believed that phantoms are confined to these alloys but this paper is limited to them for the purpose of description. Hot-rolled 2:1 Brass For illustration, therefore, a typical cake of hot-rolled 2:I brass has been chosen. This was rolled to a slab 36 in. thick, from a casting 5 in. thick by 24 in. wide by 18 in. high, which was believed to have been sound. After hot-rolling and cooling, the slab was sheared and a portion of such a shear cut is shown in Fig. I. It would be difficult to convince anyone viewing this specimen that the metal was not unsound. The impression would be confirmed by the appearance of a tensile break, as shown in Fig. 2. This is an ordinary tensile-test piece from metal just described. Although there was nothing in its tensile strength or elongation that suggested unsoundness, it appeared run through with pipes and laminations. To question the reality of such a condition would imply questioning the obvious. But, considering the history of the metal, it would be difficult to believe that it could be so bad as it appeared. It seemed reasonable, though, that if the defects were what they appeared to be, they could be traced back from the sheared or broken face.

Jan 1, 1945

By P. Rama Rao, D. H. Sastry, T. R. Anantharaman

Deformation (a) and twin (a') stacking-fault densities in cold - wor ked filings of fcc silver alloys containing 2, 4, and 6 wt pct Sb have been estimated from Debye-Scherrer peak shifts and asymmetries, respectively. Evidence has been obtained for a possible strain-induced transformation in a two-phase alloy containing 9.0 zut pct Sb. Using Fourier analysis of X-ray line profiles, the effective particle sizes and root mean square strains have been determined for the three fcc alloys in the cold-worked condition. The values of the compound fault probability 0.5a + a') evaluated from peak shifts and asymmetries are in reasonable apeement with those derived from peak broadening. COLD work of fcc metals may produce both deformation and twin (also called growth) stacking faults, which can be detected and quantitatively estimated by X-ray diffraction techniques.' In addition to peak broadening, deformation faults produce a shift in peak positions and twin faults an asymmetry of the Debye-Scherrer reflections. Besides stacking faults, a reduction in the size of coherently diffracting domains and distortion within these also broaden the powder reflections of deformed fcc metals and alloys. Fourier analysis' of peak shapes provides quantitative infor- mation about the effective domain sizes, lattice strains, and also the compound fault probability (1.5a + a'), where a and a' represent deformation-and growth-fault density, respectively. The Paterson method2 for determination of a from peak shifts, the warren3 or wagner4 method for evaluation of a' from peak asymmetries, and the Fourier analysis for quantitative estimates of all the contributory causes of peak broadening have, in the course of the last decade, been extensively applied to obtain data for a number of deformed fcc metals and alloys. One of the useful results of earlier measurements of a in several solid solutions is a correlation between a and the solute valence as well as electron concentration per atom (p) in alloy systems based on a particular solvent. The work of Smallman and westmacott5 on Cu-Zn, Cu-A1, and Cu-Sn, of Foley, Cahn, and ~aynor' on Cu-Si and Cu-Ge, and of Rama Rao and Anantharaman7 on Cu-Si and Cu-Sb has revealed a common trend in the increase of a with p and also a with valency of the solute. Cahn and Davies' and Ad-ler and wagnerg have observed similar trends for silver alloys containing cadmium, indium, and tin. Data on a for silver alloys with a pentavalent solute element are not, however, available. It is primarily to fill this need that the present investigation on Ag-Sb alloys was undertaken. Utilizing the Patersonand Warren methods, values of a and a', respectively, have been determined in three silver alloys containing 2, 4, and 6 wt pct Sb. By Fourier analysis of the broadening of Debye-Scherrer peaks, effective particle sizes, lattice strains, and the compound fault probability (1.5a +a') have also been evaluated.

Jan 1, 1967

By N. J. Grant, Hans Brunner

ThE materials used in this investigation were furnished by the Aluminum Co. of America and consisted of high-purity alurhinum (99.995 pct) and two aluminum-magnesium alloys containing approximately 2 and 5 pct Mg. The compositions of these alloys are listed in Table I. The materials were received as hot rolled 3/8-in. diam rods and were made from the same heats as the materials which were previously used in this laboratory.'j3 The rods were cold swaged to 1/4-in. diam by 1 in. long, and then had two parallel flats machined over the gage length 0.085 in. apart. The test bars were annealed for 10 min at 700° F, and strained 1 pct in tension at room temperature. They were electropolished (80 pct acetic acid; 20 pct perchloric acid, 70 pct concentration) at a temperature of 60°F at approximately 20 v. A grid, transverse or square, spaced 0.2 mm apart, was impressed by rolling a fine threaded screw (128 threads per in.) across the flat surfaces. The depth of the grooves was less than 5 p. For final annealing and grain size control the specimens were enclosed in aluminum foil and sealed in Vycor tubes. Annealing conditions varied from 1 hr at 700° F to 5 days at 1050° F, depending on the alloy content, to give for most of the specimens a final grain size of about 1 mm. This treatment was followed by electropol-ishing as described above. For the test series presented in Figs. 4 and 5 round specimens were used instead of flat ones, and fine machining marks served as marker lines instead of the impressed grid lines. Electropolishing was omitted. The major advantage is that the spacing of the machining marks is only about 1 u as compared to the 200 u of the impressed grid lines, permitting higher precision in strain measurements. Unfortunately the strain annealing necessary for grain size control also resulted in some preferred orientation of the grains. The preferred orientation of three arbitrary specimens was measured by X-ray diffraction methods and the averaged results are shown in Fig. 1. The possible effects of the preferred orientation on the test results will be discussed later. The testing temperatures were 410°, 515", 725", and 940° F, with one exception in the case of the 5.1 pct Mg alloy. Since the solubility limit of this alloy is 520°F, a test temperature of 545°F was cho-se sen instead of 515°F. The selection of the test temperature was based on two considerations: 1) at 900°F and above, extensive grain boundary migration made it more difficult to measure grain boundary sliding; 2) at 400°F and below, there was so little grain boundary sliding that it was again difficult to make precise measurements. The stress was chosen to give a creep rate of approximately 2.7 pct per hr in connection with Figs. 2

Jan 1, 1961

By H. E. Cline, D. F. Stein

A fine lamellar structure with interlamellar spacings ranging from 0.I to 3.7 was Woduced by high-speed directional solidification and used to study the interaction of dislocations with an array of bimetallic bound-am.es. The tensile flow properties were measured at elevated temperatures and the results interpreted in terms of an image force model. As the width of the plates decreases the strength increases according to a Hall-Petch relation, suggesting pile -ups. Considerable strengthening was also observed at elevated temperatures. In recent years composites containing a strong but brittle phase and a ductile but weak phase have been studied extensively in the search for a high-strength material with adequate ductility.' However, the strength of these composites has been limited to a volumetric average of the strengths of the component phases. In this paper we will show that a composite made by directional solidification of a Cu-Ag eutectic has strength properties that substantially exceed the strength of either of the metals in the composite, and an explanation for this increased strength will be presented. The Cu-Ag eutectic is a near ideal material to study for several reasons. The eutectic structure is made up of alternate plates of silver-rich and copper-rich phases with the same crystal structure.2'3 In addition, the mechanical and elastic properties of silver4 and copper5 are known over a wide range of temperatures and the eutectic microstructure is stable to nearly the melting point.6'7 Therefore, the properties of the eu-tectic are readily comparable to various theories involving the mechanical properties of copper and silver. The experiments consisted of producing directionally solidified Ag-Cu eutectic material, determining the structure and performing tensile tests at different temperatures and strain rates. EXPERIMENTAL A) Solidification and structure. A cylindrical ingot 2.2 cm in diam and 15 cm long was prepared from 99.999 pct pure materials and cast in argon. The ingot was placed in an alumina crucible and was direc-tionally solidified at 7 x 10"4 cm per sec in a Bridg-man apparatus in argon. Metallographic examination at both ends and along the length of the ingot showed a uniform structure that consisted of fine alternate plates of silver- and copper-rich phases. The plates were aligned parallel to the growth direction, as shown in the longitudinal section, Fig. 1, and were in small randomly oriented domains of parallel plates as viewed in a transverse section, Fig. 2. Four smaller ingots 0.175 in. in diam were solidified at speeds of 2Xlo-', 4.4 xlo-', 4.4 x 10-3, and4.4x10-4 cm per sec to produce a range of lamellar spacings. Replica electron micrographs were taken to resolve the individual plates as shown in Fig. 3. The copper-and silver-rich plates in the larger ingot were about

Jan 1, 1970

By Jack White, Ralph B. Adair

The Mufulira mine in Northern Rhodesia is 13° south of the Equator and at an altitude of 4100 ft above sea level. The concentrator was planned in 1930 to treat about 10,000 tons of ore per day, but before construction work had gone very far the size of the plant was reduced to 1500 tons daily capacity. Then just as the construction was finished in December 1931, the price of copper did not warrant the commencement of operations and it was not until October 1933 that the mine re-opened. Extensions have been made to the plant in 1934, 1935, 1936, 1937, 1940 and finally in 1945. The capacity of the plant when the 1945 extension is completed will be 9500 short tons per day. The various extensions have been carried out with the minimum confusion and with great skill on the part of the designers and the erection engineers. In dealing with the plant in this paper it is proposed to give an outline of the present practice and only to refer to past practice when it is considered of particular interest. Ore Treated The ore consists of fine grained highly siliceous, felspathic and argillaceous quartz- ites, the latter containing graphitic carbon and locally termed graywacke. These rocks are considerably altered near the surface and on the fringes of the ore body. Despite extensive efforts at mixing, both underground and in the crushing plant, many sudden changes of ore take place in the mill feed. The minerals are chalcocite, bornite and chalcopyrite with relatively unimportant amounts of malachite, native copper, azurite, covellite and chrysocolla. Gold is present at about I oz to a thousand tons, and silver at about 2 dwt. per ton. With increasing depth the nonsulphide content or,, as commonly termed locally, the oxide content of the ore is decreasing and is now less than 0.25 pct against a high of 0.77 pct- Crushing Operations The first stage of crushing is done under. ground where the oversize from I2-in. grizzlies is fed to a 56 X 72-in. jaw crusher. At the Selkirk shaft two 10-ton skips deliver the run of mine ore at a rate of 450 tons per hour to the 400-ton capacity shaft bins. One 6 ft wide Ross chain feeder and one locally made air-operated finger feeder feed the two 30-in. McCully crushers. Ahead of each crusher is a 6 X 9-ft spring grizzley spaced at 5 in. on a 35O slope. Neither the Ross chain feeder nor the finger feeder is entirely satisfactory and for the wet, muddy and sticky ore that has to be handled it is planned to replace these with two 6-ft wide apron pan feeders. The McCully crushers deliver a minus 5-in. product, at a.rate of over 500 tons per

Jan 1, 1949

By R. Taggart, D. H. Polonis, J. C. McMillan

Thin foil electron microscopy techniques have been used to study the micros tructure of a Ti- 7.5 wt pct vanadium alloy in the quenched and aged cond_itions. Selected area diffraction has identified a (1011) twinning mode accompanying the martens ite t9.an.sfo?rn~ation. Precipitation of the 0 phase during the aging of quenched alloys has been obsevced to occuv in the form of plates and needles with preferential growth along the (1120) direction in the a' matrix. In the present work, the micro structures of quenched and aged alloys of the 0 isomorphous Ti-V system have been investigated by means of thin-foil electron-microscopy techniques. Most of the previous studies of martensitic phases in titanium-base alloys have utilized optical microscopy and X-ray diffraction techniques. The application of transmission electron microscopy is more recent, and only a few such studies have been reported.1-5 This paper is concerned particularly with the crystallographic nature of substructures formed in the martensitic a' plates. The early stages of aging or tempering have also been examined to determine the modes of precipitation from the martensitic solid solutions. Such information is essential in studying strengthening mechanisms and in determining the feasibility of high-strength rnartensitic alloys based on titanium. Liu and Margolin6 reported several types of substructures within the martensitic plates of quenched Ti-Mn alloys. It was later suggested by Liu7 that the structure of martensitic plates might be very complex and not single crystals as normally assumed. The sub-markings could not be identified with the two possible habit-plane orientations {334}ß and {344}ß, and it was not positively determined whether they are associated with mechanical twinning. The recent studies by Armitage5 on titanium martensites in a variety of commercial alloys have indicated that twinning does not generally accompany the transformation. This observation is in accordance with the Mackenzie and Bowles model for the transformation in pure titanium8 which suggests that twinning is not to be expected. However, a number of other recent investigators have reported twinlike substructures in the martensitic plates of several titanium systems including commercia1 titanium,2,3 Ti-Cu,5,9 Ti-Ta,1 and the commercial alloy Ti-8A1-1Mo-1V. Blackburn* has reported that the structure of quenched Ti-8A1-1Mo-1V depends on the prior solution temperature. He identified two types of martensitic structures, one of which is described as a heavily faulted hcp or twinned fcc structure and the other an hcp structure with a high internal dislocation density. The latter type exhibited some twinning with a (1011) twin plane. EXPERIMENTAL PROCEDURES AND RESULTS The alloy used in the present work was a 7.5 wt pct V alloy that was prepared by conventional arc-melting techniques. This alloy composition was selected

Jan 1, 1968

By H. R. Nelson, Martin S. Maier

The diffusion of metals plays an important role in many metallurgical processes,lJ as, for example, the formation of alloys by the annealing of mixed powders, the homogenization of segregated alloys, and the carburization of steel. Other equally important phenomena, such as recrystalli-zation and creep, are based on the movement of like atoms. Although much is known concerning the effects of diffusion in metals, very little is known concerning the details of the physical processes involved. 1,3-5 The data that should give most information concerning the processes involved in diffusion are those on the diffusion of like atoms—self-diffusion. Very little is known concerning the rates of self-diffusion of metals because before the discovery of artificial radioactivity in 1934 there was no means of detecting the movement of the diffusing atoms through the solvent metal except in the elements possessing natural radioactive isotopes—lead, thallium and bismuth. Using the induced radioactivity of the element as an indicator, atoms can now be "tagged" so that the rate of diffusion of the radioactive isotopes of an element (tagged atoms) into the stable isotopes of the same element can be measured. As the radioactive and stable isotopes of an element differ only in nuclear structure, it is quite certain that all isotopes of an element diffuse at the same rate. Two techniques have been used to measure self-diffusion. In one, a thin layer of radioactive metal is deposited on the face of the solvent metal, and the decrease in the surface activity as the radioactive atoms diffuse into the solvent metal is measured. This method has been used to determine the coefficients of self-diffusion of lead6-l0 and bismuth10 using natural radioactive isotopes, and of gold1' and copper12 using artificial radioactive isotopes. In the other technique a thin layer of the radioactive metal is deposited oil one face of the solvent metal, and after diffusion has occurred the specimen is cut in thin sections to obtain the concentration-penetration curve. This method has been used to determine the coefficients of self-diffusion of gold,13 zinc,14-l6 silver," and copper.17 The second method was used for the work described in this paper. Materials The coefficients of self-diffusion were determined in two grades of polycrystalline copper and in single crystals of copper. Commercial OFHC copper was used in the form of disks I in. in diameter by % in. thick. Samples of high-purity copper described by Phillips and Skinnerl9 were supplied through the courtesy of the American Smelting and Refining Co. The high-purity copper rod was used without remelting by cross-rolling to a thickness of 0.075 in., from which disks 7/8 in. in diameter were cut. A good grade of bus-bar copper was used to make the single crystals.

Jan 1, 1942

By E. O. Kirkendall

THE investigation reported herein was undertaken to obtain data to supplement those presented in an earlier paper,' particularly for longer times at a higher temperature. This information may further develop our knowledge of the mechanism of diffusion in substitutional solid solutions. Diffusion of solute atoms interstitially dissolved is not difficult to visualize; it can take place without much disturbance of the solvent atoms. The mechanism of diffusion of solute atoms substitutionally dissolved is not so easily understood. Many theories have been advanced. Rosenhain,2.3 Frenkel,4 Smekal,5 Langmuir,3,6 Steigman, Shockley and Nix,7 and Johnson8 all proposed theories to explain diffusion. Langmuir's proposed mechanism consisted of a simple cyclic interchange of atoms involving an interchange in lattice positions of four or more atoms. This mechanism, accepted by the author at the time of his previous publication,' and apparently quite generally accepted, required a net exchange in positions of both solute and solvent atoms in equal numbers. In other words, the rate of diffusion of the solvent and solute atoms would be the same. That this cyclic interchange in lattice positions of solute and solvent atoms in equal numbers is the only true mechanism of diffusion is denied by the evidence presented in this paper. EXPERIMENTAL PROCEDURE This modification of similar procedure1 will be outlined briefly. The method consisted of the following steps: I. A pure Muntz metal (60.6 per cent Cu, 0.1 per cent total impurities) that was almost all beta brass at 780°C. was chosen. 2. The brass was turned between centers in a lathe to a diameter of 0.5965 inches. 3. After the brass was cleaned, it was electroplated with pure copper to a diameter of about one inch. 4. The sample was heated slowly to 400°C. under reduced pressure and held at that temperature for 4 hr. to remove occluded gases. It was then cooled to room temperature. 5. The sample was heated to 780°C. ±3°C. and held at that temperature for different lengths of time; then quenched. Samples were cut off each time after quenching. Metallographic samples 34 in. thick were removed at I hr., 6 hr., 24 hr., 96 hr. and 701 hr. After 96 and 701 hr. samples of about I in. were removed for X-ray analysis. 6. The metallographic samples were polished on the cross section and photo-micrographs were taken. 7. The I-in. samples were polished and etched on both ends. With the aid of a microscope each was carefully mounted in a four-jaw chuck in a lathe, so that they could be accurately bored for an arbor. 8. Turnings were taken for each X-ray sample. After each set of turnings, the sample was heated in an oil bath for about 3a hr. at 300°C. It was then etched in 25

Jan 1, 1942

By Martin S. Maier, H. R. Nelson

The diffusion of metals plays an important role in many metallurgical processes,lJ as, for example, the formation of alloys by the annealing of mixed powders, the homogenization of segregated alloys, and the carburization of steel. Other equally important phenomena, such as recrystalli-zation and creep, are based on the movement of like atoms. Although much is known concerning the effects of diffusion in metals, very little is known concerning the details of the physical processes involved. 1,3-5 The data that should give most information concerning the processes involved in diffusion are those on the diffusion of like atoms—self-diffusion. Very little is known concerning the rates of self-diffusion of metals because before the discovery of artificial radioactivity in 1934 there was no means of detecting the movement of the diffusing atoms through the solvent metal except in the elements possessing natural radioactive isotopes—lead, thallium and bismuth. Using the induced radioactivity of the element as an indicator, atoms can now be "tagged" so that the rate of diffusion of the radioactive isotopes of an element (tagged atoms) into the stable isotopes of the same element can be measured. As the radioactive and stable isotopes of an element differ only in nuclear structure, it is quite certain that all isotopes of an element diffuse at the same rate. Two techniques have been used to measure self-diffusion. In one, a thin layer of radioactive metal is deposited on the face of the solvent metal, and the decrease in the surface activity as the radioactive atoms diffuse into the solvent metal is measured. This method has been used to determine the coefficients of self-diffusion of lead6-l0 and bismuth10 using natural radioactive isotopes, and of gold1' and copper12 using artificial radioactive isotopes. In the other technique a thin layer of the radioactive metal is deposited oil one face of the solvent metal, and after diffusion has occurred the specimen is cut in thin sections to obtain the concentration-penetration curve. This method has been used to determine the coefficients of self-diffusion of gold,13 zinc,14-l6 silver," and copper.17 The second method was used for the work described in this paper. Materials The coefficients of self-diffusion were determined in two grades of polycrystalline copper and in single crystals of copper. Commercial OFHC copper was used in the form of disks I in. in diameter by % in. thick. Samples of high-purity copper described by Phillips and Skinnerl9 were supplied through the courtesy of the American Smelting and Refining Co. The high-purity copper rod was used without remelting by cross-rolling to a thickness of 0.075 in., from which disks 7/8 in. in diameter were cut. A good grade of bus-bar copper was used to make the single crystals.

Jan 1, 1942

By Fred C. Bond

The Standard method of determining the crushing resistance of rocks consists of crushing prepared shapes under slow compression, and expressing the ultimate crushing resistance at the load causing failure in pounds per square inch of cross-sectional area perpendicular to the crushing force, with the height approximately equal to the diameter. One-inch cubes or cylindrical drill cores are commonly used. Cubes and drill cores are cut by a highspeed steel disk with diamond dust embedded in the edges, and running under a water spray. such a saw will cut one square inch or more of hard stone per minute. An oiled, spherical, swivel compression block of small diameter should be used to equalize the pressure. Each sample is crushed between sheets of cardboard or blotting paper extending about one-half inch beyond the edges of the stone. A cloth is wrapped around it to prevent dangerous explosive shattering. It is probably preferable to place the swivel block below the specimen, with either a rigid head or another swivel block above. Whatever the arrangement, the conditions should be selected that will develop the maximum crushing strength of the specimen, even though its top and bottom planes may not be precisely parallel. The cardboard pads may be dispensed with if the ends of the specimens are polished smooth. The use of lead pads was discontinued because of the observed tendency to split the material. The samples are weighed and measured before breaking, and the density is calculated. Cubes that contain bedding lanes or veinlets are usually placed with these vertical and parallel to the crushing force, in order to develop the maximum resistance possible. A number of compression tests were made on Canadian ores, by Forrest Nagler, of the Allis-Chalmers Manufacturing CO., and are listed alphabetically in Table I. These tests were made on one-inch cubes or on diamond-drill cores approximately one inch in diameter and One inch long. The drill cores represent virgin rock, while the cubes may have been previously weakened by explosives. compression tests have been made in the Allis-Chalmers Milwaukee Laboratory on a number of ores and other materials. These are listed alphabetically in Table 2. In test NO. 1339, on limestone from the Hanna Coal Co., comparison was made between 2 by 2-in. diamond-drill core segments and one-inch cubes cut from the cores in the same strata. Results for the cylinders are tabulated directly below those for the cubes. The bedding planes were normal to the compressive force in breaking the cylinders and parallel in breaking the cubes, which accounts for the lower strength obtained from the cylinders. The percentage of net linear compression at the ultimate pressure was measured in test No. 1055 for Fontana TV A quartzite as 0.30 for cube A, and 0.37 for cube D.

Jan 1, 1947

By Fred C. Bond

COMPRESSION TESTS THE standard method of determining the crushing resistance of rocks consists of crushing prepared shapes under slow compression, and expressing the ultimate crushing resistance at the load causing failure in pounds per square inch of crossectional area perpendicular to the crushing force, with the height approximately equal to the diameter. One-inch cubes or cylindrical drill cores are commonly used. Cubes and drill cores are cut by a high-speed steel disk with diamond dust embedded in the edges, and running under a water spray. Such a saw will cut one square inch or more of hard stone per minute. An oiled, spherical, swivel compression block of small diameter should be used to equalize the pressure. Each sample is crushed between sheets of cardboard or blotting paper extending about one-half inch beyond the edges of the stone. A cloth is wrapped around it to prevent dangerous explosive shattering. It is probably preferable to place the swivel block below the specimen, with either a rigid head or another swivel block above. Whatever the arrangement, the conditions should be selected that will develop the maximum crushing strength of the specimen, even though its top and bottom planes may not be precisely parallel. The cardboard pads may be dispensed with if the ends of the specimens are polished smooth. The use of lead pads was discontinued because of the observed tendency to split the material. The samples are weighed and measured before breaking, and the density is calculated. Cubes that contain bedding planes or veinlets are usually placed with these vertical and parallel to the crushing force, in order to develop the maximum resistance possible. A number of compression tests were made on Canadian ores, by Forrest Nagler, of the Allis-Chalmers Manufacturing Co., and are listed alphabetically in Table 1. These tests were made on one inch cubes or on diamond-drill cores approximately one inch in diameter and one inch long. The drill cores represent virgin rock, while the cubes may have been previously weakened by explosives. Compression tests have been made in the Allis-Chalmers Milwaukee Laboratory on a number of ores and other materials. These are listed alphabetically in Table 2. In test No. 1339, on limestone from the Hanna Coal Co., comparison was made between 2 by 2-in. diamond-drill core segments and one-inch cubes cut from the cores in the same strata. Results for the cylinders are tabulated directly below those for the cubes. The bedding planes were normal to the compressive force in breaking the cylinders and parallel in breaking the cubes, which accounts for the lower strength obtained from the cylinders. The percentage of net linear compression at the ultimate pressure was measured in test No. 1055 for Fontana TVA quartzite as 0.30 for cube A, and 0.37 for cube D.

Jan 1, 1946

By Fred C. Bond

The Standard method of determining the crushing resistance of rocks consists of crushing prepared shapes under slow compression, and expressing the ultimate crushing resistance at the load causing failure in pounds per square inch of cross-sectional area perpendicular to the crushing force, with the height approximately equal to the diameter. One-inch cubes or cylindrical drill cores are commonly used. Cubes and drill cores are cut by a highspeed steel disk with diamond dust embedded in the edges, and running under a water spray. such a saw will cut one square inch or more of hard stone per minute. An oiled, spherical, swivel compression block of small diameter should be used to equalize the pressure. Each sample is crushed between sheets of cardboard or blotting paper extending about one-half inch beyond the edges of the stone. A cloth is wrapped around it to prevent dangerous explosive shattering. It is probably preferable to place the swivel block below the specimen, with either a rigid head or another swivel block above. Whatever the arrangement, the conditions should be selected that will develop the maximum crushing strength of the specimen, even though its top and bottom planes may not be precisely parallel. The cardboard pads may be dispensed with if the ends of the specimens are polished smooth. The use of lead pads was discontinued because of the observed tendency to split the material. The samples are weighed and measured before breaking, and the density is calculated. Cubes that contain bedding lanes or veinlets are usually placed with these vertical and parallel to the crushing force, in order to develop the maximum resistance possible. A number of compression tests were made on Canadian ores, by Forrest Nagler, of the Allis-Chalmers Manufacturing CO., and are listed alphabetically in Table I. These tests were made on one-inch cubes or on diamond-drill cores approximately one inch in diameter and One inch long. The drill cores represent virgin rock, while the cubes may have been previously weakened by explosives. compression tests have been made in the Allis-Chalmers Milwaukee Laboratory on a number of ores and other materials. These are listed alphabetically in Table 2. In test NO. 1339, on limestone from the Hanna Coal Co., comparison was made between 2 by 2-in. diamond-drill core segments and one-inch cubes cut from the cores in the same strata. Results for the cylinders are tabulated directly below those for the cubes. The bedding planes were normal to the compressive force in breaking the cylinders and parallel in breaking the cubes, which accounts for the lower strength obtained from the cylinders. The percentage of net linear compression at the ultimate pressure was measured in test No. 1055 for Fontana TV A quartzite as 0.30 for cube A, and 0.37 for cube D.

Jan 1, 1947

By John C. McDonald

This report is a continuation of an earlier one with a similar titlell to which the reader is referred for such details of procedure as do not appear here. A brief summary will be given of the objects and methods of the research at this time. It was pointed out in the previous paper that properties of magnesium alloys, as reported by different workers, often differ. This was thought to be due to differences in the preparation of the specimens tested. The ideal way to compare alloys would be to prepare each of them in so many ways that reasonable assurance would exist that the best properties of each alloy had been developed. The alloys would then be compared on the basis of these properties. The treatment actually given the alloys of these studies is necessarily a compromise with completeness. Nevertheless, enough treatments have been given so that a considerable degree of assurance exists that the properties obtained are representative of the alloy as such, and not merely of the manner in which it was worked and heat-treated. Procedure The alloys were cast in the form of cylindrical ingots, which were extruded into bar before being rolled. Some of the ingots were made in 2-in. diameter molds whereas all of the alloys of the previous paper were cast in 4.in. molds. For the larger ingots, the extruded bar was 2 by 0.140 in.; lor the 2-in. ingots, it was I by 0.100 in. Preliminary work indicated that strip rolled from both sizes of the bars would have substantially the same properties. The bar was rolled at some temperature in the range 400' to 800°F., for a total reduction of 50 per cent. The temperature and reduction per pass were so selected that no cold cracking occurred, but were such as to leave the metal in a semihard condition. The hot-rolled metal was annealed at several temperatures in the range 400' to 800°F.; it was also cold-rolled, and given solution and aging treatments. Two standard test bars corresponding to each treatment were pulled in tension, and the average was obtained. Twelve treatments, in all, were given each alloy. The properties of the annealed specimen having the highest percentage of elongation were selected to represent the alloy in the annealed condition. The properties of the cold-rolled specimen having the highest yield strength were selected to represent the alloy in the cold-rolled condition. These properties were then plotted against percentage composition by analysis. Smooth curves were drawn among the points, thus graphically averaging the results over the entire range studied. The percentage of elongation in the cold-rolled state was not plotted, since it was always low, and varied in an irregular manner with composition. Alloys Studied Magnesium-calcium Alloys.—Fig. I presents the results on the alloys of the rnag-

Jan 1, 1941

By John C. McDonald

This report is a continuation of an earlier one with a similar titlell to which the reader is referred for such details of procedure as do not appear here. A brief summary will be given of the objects and methods of the research at this time. It was pointed out in the previous paper that properties of magnesium alloys, as reported by different workers, often differ. This was thought to be due to differences in the preparation of the specimens tested. The ideal way to compare alloys would be to prepare each of them in so many ways that reasonable assurance would exist that the best properties of each alloy had been developed. The alloys would then be compared on the basis of these properties. The treatment actually given the alloys of these studies is necessarily a compromise with completeness. Nevertheless, enough treatments have been given so that a considerable degree of assurance exists that the properties obtained are representative of the alloy as such, and not merely of the manner in which it was worked and heat-treated. Procedure The alloys were cast in the form of cylindrical ingots, which were extruded into bar before being rolled. Some of the ingots were made in 2-in. diameter molds whereas all of the alloys of the previous paper were cast in 4.in. molds. For the larger ingots, the extruded bar was 2 by 0.140 in.; lor the 2-in. ingots, it was I by 0.100 in. Preliminary work indicated that strip rolled from both sizes of the bars would have substantially the same properties. The bar was rolled at some temperature in the range 400' to 800°F., for a total reduction of 50 per cent. The temperature and reduction per pass were so selected that no cold cracking occurred, but were such as to leave the metal in a semihard condition. The hot-rolled metal was annealed at several temperatures in the range 400' to 800°F.; it was also cold-rolled, and given solution and aging treatments. Two standard test bars corresponding to each treatment were pulled in tension, and the average was obtained. Twelve treatments, in all, were given each alloy. The properties of the annealed specimen having the highest percentage of elongation were selected to represent the alloy in the annealed condition. The properties of the cold-rolled specimen having the highest yield strength were selected to represent the alloy in the cold-rolled condition. These properties were then plotted against percentage composition by analysis. Smooth curves were drawn among the points, thus graphically averaging the results over the entire range studied. The percentage of elongation in the cold-rolled state was not plotted, since it was always low, and varied in an irregular manner with composition. Alloys Studied Magnesium-calcium Alloys.—Fig. I presents the results on the alloys of the rnag-

Jan 1, 1941

By D. B. Masson

THE martensitic transformations occurring in ,B AgCd as a result of cold working at room temp.. a-ture and cooling below room ten1erature have been reported by Masson and Barrett.1 These authors found that simple cooling to 127°K caused body-cen-tered-cubic AgCd containing 53.0 at. pct Ag to transform to an orthorhombic structure, while mechanical deformation at room temperature was found to induce a hexagonal structure. Furthermore, they observed that the temperature at which martensite first appeared on cooling, Ms, and that at which the transformation was complete, MI, as well as the corresponding temperatures for the reversion on heating, As and Af, could be ascertained to ± 1°K, although they report these temperatures only for the alloy containing 53.0 at. pct Ag (51.96 wt pct). In the work reported here the temperature range of the transformation on cooling was studied as a function of composition, and further consideration was given to the relationship between the original bcc structure and the transformation-induced hexagonal and orthorhomic structures. EXPERIMENTAL PROCEDURE All samples studied were in the form of annealed 300-mesh powder and were prepared from the constituent metals in the manner described previously.1 The compositions in weight and atomic pct are listed in Columns 1 and 2 of Table I. Method of determination of transformation temperature was the same as utilized previously1—measurement of the intensity of X-rays diffracted by the transformation product. A diagram of the low-temperature sample mount is shown in Fig. 1. This mount was made to fit a GE model XRD-3 X-ray diffraction unit. The powder sample was varnished to a flat surface on a copper sample holder at A. This sample holder was soldered to a brass rod, B, which was in turn soldered to a second copper rod, C. Rod C could be cooled to 78°K by inserting it into a reservoir of liquid nitrogen, D. A heater coil of nichrome wire was wound at E on the sample holder, and by varying the current through the heater a thermal gradient could be maintained along brass rod B. Sample temperatures from 78°K up could be attained and held as long as needed. The sample holder and nitrogen reservoir were insulated by Styrofoam, F, and the sample itself was protected by two radiation shields, G. The X-ray beam entered and left the sample chamber through windoys in the supporting container at H and I. Sample temperatures were measured by a calibrated copper-constantan thermocouple varnished to the sample holder just out of the beam at A. The low-temperature structure had been found to possess orthorhombic symmetry1 and the expected positions of the diffraction maxima were known. Therefore the sample was aligned in the X-ray beam and the Geiger counter of the spectrometer set to receive the most intense orthorhombic reflection without an adjacent interfering cubic reflection. This

Jan 1, 1961

By H. R. Hendricks

The ore of the Iron King mine, being very hard and having a very fine crystalline structure, presents many problems in milling that are not present in ordinary lead-zinc ores. This very fine crystallization causes much interlocking of minerals and is most prevalent between the gold and pyrite and the sphalerite and pyrite. The recovery of gold is extremely important in the economic value of the ore and therefore constitutes a large part of the metallurgical problem to be solved. All of the gold is free but it has not been observed in any of the mill products except under very high magnification. Some of the gold is tarnished, and this condition also makes recovery difficult. The gold values have been determined to be highest in association with chalcopyrite and arsenopyrite. The silver occurs mostly in association with galena and tennantite. A small amount of native silver has also been observed occasionally. The galena, being softer than the other minerals, frees much better in grinding. Some oxidation of galena is present in the ore, as the non-sulphide lead content amounts to approximately 10 pct of the total lead. Some oxidation of sphalerite is also present in the ore. Microscopic examination of the zinc concentrate shows many grains in the minus 325-mesh to be half pyrite, together with the fact that some of the zinc is marmatite, makes production of a high-grade zinc concentrate very difficult unless recovery is sacrificed. In the grinding, it has been determined that the flotation feed must be maintained at 85 pet minus 200-mesh to free the minerals sufficiently to make the best economic recoveries. Table I illustrates the effect of fine grinding. It shows that the bulk of the recovered minerals is in the minus 325-mesh size and is the part of the minerals that is more readily freed. The pyrite concentrate is not given in the table because it contains practically no minus 325-mesh. Development of Present Flowsheet and Milling Practice The first milling operation started in 1938, with a mill capacity of 140 tons daily, producing a bulk gold-silver-lead concentrate. After several stages of expansion and changes of the mill flowsheet, the mill is currently treating 380 tons of ore daily and three separate concentrates are produced. In order of their importance and value, these are: (I) lead concentrate, (2) zinc concentrate and (3) pyrite concentrate. The present average grade of mill heads is: gold 0.11 oz, silver 4.00 oz, lead 2.50 pet, zinc 7.60 pct, copper 0.22 pct, iron 22 pct and 30 pct insolubles. Specific gravity of the ore is 3.8. During the period when bulk flotation mas practiced, the flowsheet was very simple. The ore was ground fine enough to liberate as much gold, silver and lead as possible. Necessary collectors and frothers were added in sufficient quantity

Jan 1, 1949

By David J. Mack, A. H. Kasberg

The transformation characteristics are found to resemble a similar binary alloy. The differences are due to the alpha iron particles. While strength properties of the isothermally transformed alloys are high, ductility is low, resulting in high notch sensitivity. The elastic modulus can be varied widely and correlates with strength. Abnormal grain growth sometimes occurs. A CONSIDERABLE amount of work has been done on the isothermal transformation of high purity aluminum bronzes using the methods pioneered by Davenport and Bain.' The first isothermal study of these alloys was made by Smith and Lind-lief,' but more recently Mack", " and Klier and Grymko5 have continued the work. In commercial aluminum bronzes, one or more elements are always added to refine the ß grain size and to improve the mechanical properties. The effect of these elements on the isothermal transformation has not been reported in the literature. No systematic study of the properties of isother-mally transformed aluminum bronzes has apparently been reported, although adequate information is available on their properties after more conventional heat treatments. The fact that a eutectoid alloy will reject face-centered cubic a during isothermal transformation at appropriate temperatures2'" warrants investigation of the properties of such structures. Another cogent reason for determination of properties is the fact that the modulus of elasticity of the eutectoid alloy varies widely with the nature of the heat treatment." Preliminary experiments7 indicated that a high purity eutectoid alloy would not give reproducible results in property determinations because of ex- cessive ß grain growth during heat treatment, a single ß grain frequently occupying the entire cross-section of a standard test bar. For this reason a commercial aluminum bronze containing iron as a grain growth inhibitor was used. The isothermal transformation diagram of the alloy was first determined. On this basis, the heat treatments necessary to produce representative structures were selected and the properties determined. Material A commercial alloy (Ampco Grade 20) of the following composition was used: Cu, 83.68 pct; Al, 12.31 pct; Fe, 3.68 pct; Ni, 0.28 pct; and Mn, 0.03 pct. This alloy proved to be very close to the eutectoid composition and may be compared with the accepted value of 11.8 pct A1 in the binary Cu-A1 system. Comparison is valid only because of the "negative replacement effect" of the iron? Since traces of excess y² are present, the alloy is slightly hyper-eutectoid. The material was received in the form of 3/4 in. round, hot extruded bars. Specimens of approximately ? in. thickness were cut from this stock and drilled to allow suspension in the salt bath. The structure of the as-received material varied from 5 to 40 pct a + y2* in a matrix of ß. The amount of a + y² present was dependent upon the ß grain size of the extruded material. The coarse grained portions did not form as much a + Y, as did

Jan 1, 1952