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By Haim H. Chiswik, Ralph Hultgren

In recent years considerable attention has been devoted to the development of new commercial uses for silver, chiefly because of lowered prices and large stocks of the metal. This has led to increased interest in the phase diagrams of silver alloys. The silver-lead diagram is reported' to be of the simple eutectie type, but no measurements of the solubility of lead in silver have been made. The solubility of silver in lead has been estimated2 from diffusion experiments and resistance measurements to vary with temperature from 0.09 to 0.18 atomic per cent (0.05 to 0.10 weight per cent). Silver-rich silver-lead alloys have recently been recommended as high-strength bearing metals3 The silver-bismuth diagram is similar.' The solubility of bismuth in silver. has been estimated to be about 5.5 weight per cent on the basis of X-ray work.4 Matthiessen6 found a solubility of silver in bismuth from 0.25 to 0.50 per cent by conductivity measurements. Silver and thallium form the same type of diagram,' with no data on their mutual miscibilities. We have studied the first two of these diagrams by X-ray methods, verifying their main features and determining the solubilities of lead and bismuth in silver at several temperatures. We also determined the solubility of thallium in silver at one temperature. The solubilities of silver in lead and in bismuth were found to be too low to be detectable. Materials and Methods Mallinckrodt precipitated silver, analytical reagent, was used. Maximum impurities listed on the label were: chloride, 0.005 per cent; copper, 0.001; iron, 0.002; other heavy metals (as Pb), 0.002; and sulphate (SO³), 0.05. The lattice constant was found to be a0 = 4.0782 $., in good agreement with the value of Jette and Foote,6 a0 = 4.0779 A., for

Jan 1, 1940

By Ralph Hultgren, Haim H. Chiswik

In recent years considerable attention has been devoted to the development of new commercial uses for silver, chiefly because of lowered prices and large stocks of the metal. This has led to increased interest in the phase diagrams of silver alloys. The silver-lead diagram is reported' to be of the simple eutectie type, but no measurements of the solubility of lead in silver have been made. The solubility of silver in lead has been estimated2 from diffusion experiments and resistance measurements to vary with temperature from 0.09 to 0.18 atomic per cent (0.05 to 0.10 weight per cent). Silver-rich silver-lead alloys have recently been recommended as high-strength bearing metals3 The silver-bismuth diagram is similar.' The solubility of bismuth in silver. has been estimated to be about 5.5 weight per cent on the basis of X-ray work.4 Matthiessen6 found a solubility of silver in bismuth from 0.25 to 0.50 per cent by conductivity measurements. Silver and thallium form the same type of diagram,' with no data on their mutual miscibilities. We have studied the first two of these diagrams by X-ray methods, verifying their main features and determining the solubilities of lead and bismuth in silver at several temperatures. We also determined the solubility of thallium in silver at one temperature. The solubilities of silver in lead and in bismuth were found to be too low to be detectable. Materials and Methods Mallinckrodt precipitated silver, analytical reagent, was used. Maximum impurities listed on the label were: chloride, 0.005 per cent; copper, 0.001; iron, 0.002; other heavy metals (as Pb), 0.002; and sulphate (SO³), 0.05. The lattice constant was found to be a0 = 4.0782 $., in good agreement with the value of Jette and Foote,6 a0 = 4.0779 A., for

Jan 1, 1940

By H. Margolin, E. Ence

In order to understand the effect of zirconium on properties of Ti-Cu-A1 alloys, Ti-Zr alloys were examined for the presence of ordering or compounds at the following compositions in weight percent: 24.1 pct Zr (lZr:GTi), 32.2 pct Zr (lZr:4Ti), 38.8 pct Zr (lZr:3Ti), 49.0 pct Zr(1Zr:ZTi). Alloys were prepared as 15-g buttons by non- consumable arc melting under argon atmosphere from Bureau of Mines titanium (Bhn 63) and Reactor Grade zirconium (Bhn 150). Weight losses during melting did not exceed 1 pct of the initial button weight. Prior to heat treatment, buttons were hot-rolled at 600" to 700°C to rods of about 6 mm diam. Contamination after hot-rolling was found to extend to a depth of less than 0.5 mm. Specimens for heat treatment were wrapped in molybdenum sheet, annealed in argon-filled quartz capsules, and quenched by breaking the capsules under iced brine. Annealing times were as follows: 700°C — 7 days; 600°C— 14 days; 575°C-1 and 2 months; 525°C-2 months; 500°C-2 months. Prior to heat treatment, all Ti-Zr alloys were vacuum annealed at 900°C to remove hydrogen. The reanneal of 575°C specimens for an additional month produced no observable microstructure changes. The results obtained by microstructure and X-ray diffraction are shown in Fig. 1, together with data of Hayes et al.' No other phases than a or P were found. Small amounts of retained P were detected by X-ray in the 49 pct Zr alloy. The data of the present investigation suggests that ß and a transus boundaries are at considerably lower temperatures than those of Hayes et al. The work of Hayes et al. is based on sponge titanium and Bureau of Mines zirconium, both of which contained 0.15 pct 0. Since melting was performed in

Jan 1, 1962

By C. G. Dunn, E. F. Koch, K. T. Aust

Strain-induced grain boundary migration was studied in a series of silicon-iron (3% pct Si) bicrystals of controlled orientations. Each bicrystal was given a 7 pct cold-rolling strain rind annealed at 1100°C. The direction of boundary migration was found to depend on orientation; results for several orientations related by a common [110] axis are given. Analysis of the micrographic and X-ray data is made in terms of the residual strain-energy densities within the crystals (energy per unit volurne) and a driving force on the boundary due to an energy density difference across the boundary. Relative strain energies were obtained for the various orientations investigated. A CHROME-acetic acid electroetching method for revealing dislocation sites in silicon iron was previously applied to clarify the structural features and the energetics involved in strain-induced grain boundary migration.',' The present paper is a continuation of this study, but is primarily concerned with the influence of crystal orientation. Sperry, as reported by Beck,3 attempted to determine the factors that influence the preferred growth of one grain over another in aluminum due to strain-induced boundary migration. He found that the particular grain of a pair which work hardened more was invaded, although exceptions to this correlation were noted. The index of work hardening was determined from microhardness measurements of each grain before and after cold-rolling. In the present study, orientation itself was taken as a useful variable for studying the behavior of individual grains in a bicrystal and the direction of boundary migration, since the extent of work hardening is orientation dePendent." The effect of strain on boundary migration is evident from a consideration of driving forces. Thus, in the absence of inclusions, the driving force (per unit area of boundary) for growth of grain A into grain B when a bicrystal is strained and annealed may be expressed as follows:2

Jan 1, 1960

By R. J. Wasilewski

Elastic constants have been determined on single crystals of maximum-melting-temperature NiAl compound (50.6 at. pct Al) at 25°C. Temperature variations of Young&apos;s modulus in the three principal crystal directions between -150°C and +800°C exhibit no anomalies similar to those repovted for the isomor-phous compounds brass and AuCd. It is concluded that the ordered CsCl structure is stable throughout the temperuture range investigated NICKEL aluminide is a congruently melting inter-metallic compound of CsCl (B2) structure, stable over a rather wide composition range (40 to 54 pct Al). It exhibits a lattice-parameter maximum of a. = 2.883A at 50.6 pct 1,&apos; at which composition the excess aluminum atoms are randomly distributed on the vacant nickel sites;&apos; at higher nickel compositions the excess nickel atoms replace substitutionally in aluminum sites, while at higher aluminum compositions vacancies are present in the nickel sublattice.&apos; For compositions close to NiAl no significant variation in order has been observed at temperatures up to 900°C.3 At high nickel (65 pct) compositions the existence of a martensitic structural transformation has been reported.4 NiAl is isomorphous with the ordered B-brass structure and with the high-temperature structures of AuCd and TiNi alloys close to equiatomic composition. All of these exhibit anomalous elastic behavior as the temperature of their diffusionless transformation to lower-symmetry structures is approached.&apos;-&apos; This behavior has been explained as indicative of low stability of the CsCl structure in these compounds.8 The present paper reports the experimental determination of the elastic compliances of single-crystal NiA1. EXPERIMENTAL METHOD 1) Specimens. Polycrystalline NiAl was prepared by induction melting of carbonyl nickel and high-purity aluminum and casting into solid copper molds in gettered helium atmosphere. The castings thus produced were canned in mild steel and impact-extruded at 1100 to 1200°C to 38-in.diam rod. After the steel sheath was pickled off, the rods were converted to single crystals by repeated high-frequency satisfactorily produced the desired orientations in the form of crystals 38 in. diam by 8-12 in. long. These were subsequently center less-ground to 7 to 8 mm diam by 12 cm long, electropolished (in 80 pct methanol, 20 pct HzSO, at 25°C and 15 v), and their axial orientation determined to 1 deg by the Laue back-reflection technique. The rod dimensions were determined to 0.01 mm and the densities determined from geometrical dimensions and the weight of every specimen. The average density was 5.905 0.005 g per cu cm. 2) Elastic Data Measurements. Room-temperature elastic compliances Sii were obtained by determining to 0.1 cps the fundameGtal resonance frequencies in the longitudinal and torsional vibration modes. At these frequencies the following relations hold: E =p(2lfif =pvl= Sn- 2r[Sll- S12- -£„«] g -P(2iftf = pvf = (s<« - fr(sii - sw - ±s»y where vl and vt are the velocities, and f andft the resonance frequencies of the longitudinal and torsional waves, respectively; 1 is the length of the specimen, and r is the direction cosine factor—{cos2 a • cos2 0 + cos2 a . cos2 y + cos2 0 ¦ cos2 Y}. Given three crystals of orientations (loo), (110), and (111)) i.e., F = 0, 14, and 13, we can obtain six equations for the three unknown compliances, thus providing adequate internal check. Mode mixing can readily occur in the relatively long wavelength resonance utilized here. This could cause a significant error in the torsion wave velocities calculated from the apparent resonance frequenies. Therefore, throughout the present work, a method, described previosl,&apos; was used to ensure that no significant mode mixing took place at resonance. The apparatus used was originally designed for the Elastomat, Magnaflux Corp.. Chicago, 111. determination of flexural vibration resonance frequencies. At room temperature torsional vibration mode could be established by suitable positioning of the thin wires from the input and pick-up transducers, and longitudinal mode by cementing thin magnetic foils at the ends of the specimen, and inducing the vibration by means of electromagnetic transducers. Only flex-ural resonance frequencies could, however, be obtained reproducibly over the temperature range of -150 to 800°C. These data are considerably less accurate, the error in the modulus being estimated at -0.6 pct from the specimen dimensions and the room-temperature Poisson&apos;s ratio. The reproducibility of the resonance frequencies in repeat runs was, however, to better than l in 15,000, hence the relative elastic modulus error less than 0.02 pct. Therefore, the temperature variation of the principal Young&apos;s moduli obtained by flexural resonance, relative to room-temperature values, is believed to be satisfactorily accurate.

Jan 1, 1967

By E. T. Turkdogan, M. T. Hepworth, R. P. Smith

The permeability of oxygen in 0 iron in the tempera-ture range 700" to 900 C and in 6 iron at 1450°C was determined by the rate of internal oxidation of iron, containing -0.1 pct Al. The solubility of oxygen in zone-refined iron was determined by equilibration with hydrogen-water vapor gas mixtures at 1450" and 1510°C; oxygen solubilities , for iron in equi1ibriu.rn with molten oxide, are found to be 66 and 83 ppm for these two temperatures, respectively. The diffusivity of oxygen in iron at 14500C3 as calculated from the permeability and solubility data, is (4.1 * 0.6) x 10 "B sq cm per sec. OXYGEN is one of the most common impurities present in iron or steel, mainly in the form of oxide inclusions. In the study of many metallurgical problems concerning solid iron, it is often desirable to know with a reasonable accuracy the solubility and diffusivity of oxygen over a wide temperature range. The solubility of oxygen in solid iron has been the subject of numerous studies yielding highly discordant results as seen for example from the literature surveys made by Meijering &apos; and Schenck et a1.&apos; As shown by Kitchener et aL3 and by Sifferlen, the high oxygen solubilities reported by many investigators are the result of oxidizable impurities which are often present in iron. In addition, there have been experimental problems associated with icaccuracy of oxygen analysis of iron containing less than 100 ppm 0. A number of studies have been made on the permeability of oxygen in a and y iron using Fe-Si, Fe-Mn, and Fe-A1 alloys in the internal-oxidation experiments.1&apos;2&apos;5&apos;6 However, no direct measurements have been made of the diffusivity of oxygen in iron. In the present work two sets of experimental measurements were made: permeability and solubility studies at 1450" and 1510°C and permeability studies only in the range 700 to 900°C. In both sets of permeability measurements slab-shaped specimens containing small predetermined amounts of aluminum in solution were exposed at constant temperature to gas mixtures of hydrogen, water vapor, and argon for varying times. These specimens were quenched, sectioned, and examined for oxygen penetration by metallographic observation of aluminum oxide particles which formed. From these data, it is possible to calculate the ratio of the diffusivity of oxygen in iron, D, to the equilibrium constant K for the reaction Hz(g) * O (dissolved in iron) = H,O(g). EXPERIMENTAL Permeability Measurements at 1450°C. An ingot of vacuum-carbon deoxidized iron containing 0.086 pct A1 was prepared, using commercial "Type lO4A Plas-tiron"; after hot rolling, specimens were machined into slabs a by 2 by 2 in. The impurity contents were: S, P < 0.002 pct; C, Mn < 0.01 pct; each of all other Usual impurities < 0.004 pet. The amount of oxide inclusions in this material, determined by a bromine-methyl acetate extraction, corresponded to about 20 ppm 0 in the iron which agreed well with the results of vacuum-fusion analysis. Each specimen was annealed at 1450°C for 1 hr in purified hydrogen, polished to a smooth surface, and then introduced into a controlled oxidizing atmosphere in a recrystallized alumina tube at 1450°C. The constant temperature zone (*3"C) was about 3 in. in length. The gas composition was controlled by mixing argon with hydrogen (using calibrated constant-head flow meters) and passing the mixture through a column of a mixture of oxalic acid dihydrate and 10 pct anhydrous oxalic acid, to establish a required water-vapor content in the gas mixture. The temperature of the oxalic acid dihydrate column was controlled by a thermostat. The total gas flow was in the range 800 to 1000 cu cm per min. The exit gas from the reaction tube was passed through a weighing bottle containing a desiccant, to cross-check the degree of water-vapor saturation, which for all experiments was about 97 pct of those derived from the data of Baxter and Lansing.1 For a typical experiment, a specimen was introduced into the furnace in a stream of dry argon and hydrogen. The specimen was then rapidly raised by a Pt-Rh alloy wire into the hot zone and allowed to reach the reaction temperature, at which time the oxidizing gas mixture was introduced. The oxygen potentials employed were sufficient to oxidize aluminum but not to cause liquid iron oxide to form. After a specified time, the experiment was ended by dropping the specimen onto a water-cooled copper block at the bottom of the reaction tube. The depth of the internally oxidized zone, hereafter called the "case", was determined by sectioning the specimen at right angles to the long direction. The section was then examined under a microscope equipped with a micrometer stage. In general, the oxide particles were fairly uniform in size and distribution, forming a reasonably well-defined interface between the oxidized and unoxidized region. A typical cross section as observed at X30 is shown in Fig. 1. A thermal macroetch was used in one selected specimen to delineate the case. A cross section of a previously oxidized slab was polished and reheated at 1450°C in a hydrogen atmosphere for about 10 min. Upon quenching, the surface relief shown in Fig. 2 was produced; causes of this effect are unknown. Permeability Measurements Below 900°C. A slightly

Jan 1, 1967

By B. J. Nelson, F. N. Rhinos

Studies upon the rates of oxidation of copper alloys containing small quantities of the alloying elementsl,2 have shown that steady growth of the scales at predictable rates is limited to a small concentration range and to oxidation at temperatures above 600°C., whereas unpredictable and erratic oxidation behavior is found with alloys containing larger additions and at low temperatures. The latter effect appears to be associated with modifications in the geometric disposition of the oxides. At low concentrations of the baser elements in copper, simple oxidation behavior is typified by the formation of two distinguishable zones of oxidation: (I) a subscale composed of discrete particles of the oxide of the alloying element embedded in substantially pure copper and (2) an external scale composed of cuprous oxide (with a very thin layer of cupric oxide on the outside) containing particles of the alloying element distributed throughout, but most profusely near the metal surface (see Fig. 2, top). Where this type of structure obtains, the process of oxidation is believed to be implemented, and its rate controlled, by the diffusion of the reacting elements through a&apos; continuous matrix phase; i.e., through the alpha (metallic) phase of the subscale and alloy and through the cuprous oxide of the external scale. Copper is presumed to diffuse outward through the cuprous oxide layer to the external surface, where it reacts to form more cuprous oxide.3 Oxygen is delivered at the oxide-metal interface in the form of cuprous oxide, which may either react with the alloying element to deposit its oxide at the inner limit of the external scale or dissolve in the pure copper that remains at the surface of the metal after it has become depleted in its oxidiza-ble alloying elements. Both oxygen and the alloying element are pictured as diffusing through the metal, the oxygen inward and the alloying element outward. Where the two diffusion streams meet in sufficient concentration the oxide of the subscale is precipitated. If the oxygen pressure in the surrounding atmosphere is just below the pressure necessary to maintain cuprous oxide undecomposed, no cuprous oxide can be formed; some of the oxide of the alloying element may form upon the external surface, if its decomposition pressure is below that of cuprous oxide, and a normal sub-scale appears. This condition is achieved experimentally by enclosing the alloy with cuprous oxide together with an excess of copper. At temperatures from 600°C. downward, the precipitated oxides tend to accumulate at the grain boundaries of the alpha phase where a relatively small volume establishes a partial barrier to the diffusion of the reactants- Similarly, large volumes of Precipitated oxides tend to deposit in various patterns that may be expected to

Jan 1, 1944

By F. N. Rhinos, B. J. Nelson

Studies upon the rates of oxidation of copper alloys containing small quantities of the alloying elementsl,2 have shown that steady growth of the scales at predictable rates is limited to a small concentration range and to oxidation at temperatures above 600°C., whereas unpredictable and erratic oxidation behavior is found with alloys containing larger additions and at low temperatures. The latter effect appears to be associated with modifications in the geometric disposition of the oxides. At low concentrations of the baser elements in copper, simple oxidation behavior is typified by the formation of two distinguishable zones of oxidation: (I) a subscale composed of discrete particles of the oxide of the alloying element embedded in substantially pure copper and (2) an external scale composed of cuprous oxide (with a very thin layer of cupric oxide on the outside) containing particles of the alloying element distributed throughout, but most profusely near the metal surface (see Fig. 2, top). Where this type of structure obtains, the process of oxidation is believed to be implemented, and its rate controlled, by the diffusion of the reacting elements through a&apos; continuous matrix phase; i.e., through the alpha (metallic) phase of the subscale and alloy and through the cuprous oxide of the external scale. Copper is presumed to diffuse outward through the cuprous oxide layer to the external surface, where it reacts to form more cuprous oxide.3 Oxygen is delivered at the oxide-metal interface in the form of cuprous oxide, which may either react with the alloying element to deposit its oxide at the inner limit of the external scale or dissolve in the pure copper that remains at the surface of the metal after it has become depleted in its oxidiza-ble alloying elements. Both oxygen and the alloying element are pictured as diffusing through the metal, the oxygen inward and the alloying element outward. Where the two diffusion streams meet in sufficient concentration the oxide of the subscale is precipitated. If the oxygen pressure in the surrounding atmosphere is just below the pressure necessary to maintain cuprous oxide undecomposed, no cuprous oxide can be formed; some of the oxide of the alloying element may form upon the external surface, if its decomposition pressure is below that of cuprous oxide, and a normal sub-scale appears. This condition is achieved experimentally by enclosing the alloy with cuprous oxide together with an excess of copper. At temperatures from 600°C. downward, the precipitated oxides tend to accumulate at the grain boundaries of the alpha phase where a relatively small volume establishes a partial barrier to the diffusion of the reactants- Similarly, large volumes of Precipitated oxides tend to deposit in various patterns that may be expected to

Jan 1, 1944

By Richard Hamburger

Calculating machines permit the use of the more rapid cotangent and semigraphic solutions of plane triangulation. The results of these methods are as accurate as those of other methods. Simple adjustment of the net, and ease of calculation encourage more complete field work. Errors in field work or in computation are easily localized.

Jan 1, 1950

By G. R. Speich

The distribution of carbon and the type of substructure in iron-carbon martensites containing 0.02 to 0.57pct C has been studied in the as-quenched condition and after tempering at 25" to 700°C by using electrical resistivity, internal friction, hardness, and light and electron microscope techniques. in marten-sites containing less than 0.2 pct C, almost 90 pct of the carbon segregates to dislocations and to lath boundaries during quenching; in martensites containing greater than 0.20 pct C, appreciable amounts of carbon enter normal interstitial positions located far from defects. Tempering martensites with carbon contents below 0.20 pct at temperatures below 150°C results in additional carbon segregation to dislocations and to lath boundaries but no carbide precipitation whereas -carbide precipitation occurs in martensites with carbon contents exceeding 0.2 pct. Above 150°C, a rod-shaped carbide (either Fe3C or Hagg) is precipitated in all cases. At 400°C, spheroidal Fe3C precipitates at lath boundaries and at former aus-tenite grain boundaries. At 400" to 600"C, recovery of the martensite defect structure occurs. At 600" to 700°C, recrystallization of the martensite and Ost-waW ripening of the Fe3C occur. The effects of the carbon segregation that occurs during quenching and the subsequent substructural changes that occur during tempering on martensite tetragonality, hardness, and precipitation behavior are discussed. A mathematical analysis of carbon segregation during quenching is presented. RECENT studies of the strength of low-carbon martensitel-4 emphasize the importance of carbon segregation to the martensite lath boundaries and to the dislocations contained between them during quenching. Unfortunately, very few studies of the tempering of low-carbon martensites have been conducted, so the exact nature of this segregation is poorly understood. In fact, most early tempering studies5,6 were restricted to carbon contents greater than 0.20 pct. Moreover, these studies did not determine the amount of carbon segregated to the martensite substructure during quenching so that the initial state of the martensite was not established. Aborn7 studied the precipitation of carbide in low-carbon martensite during quenching but did not establish whether carbon segregation occurs prior to carbide precipitation, nor did he study the subsequent tempering sequence in detail. In the present work we have used electrical resistance and internal friction measurements, supplemented by electron transmission microscopy to establish the carbon distribution in as-quenched specimens. Specimens thin enough to avoid carbide precipitation (but not carbon segregation) were employed. The redistribution of carbon on subsequent tempering below 250°C was followed by measurements of elec- trical resistance. Additional studies were made on specimens tempered at 250" to 700°C to elucidate the overall tempering behavior of low-carbon martensites, including the formation of cementite and recrystalli-zation of the martensite. EXPERIMENTAL PROCEDURE Eight iron-carbon alloys with 0.026, 0.057, 0.097, 0.18, 0.20, 0.29, 0.39, and 0.57 wt pct C were prepared as 8-lb ingots by vacuum melting. Typical impurities in wt ppm were 40 Si, 20 Mn, 30 S, 10 P, and 10 N. These alloys were hot rolled to 3 in. plate at 1095°C) (2000°F). The hot-rolled plates were surface ground to remove scale and the decarburized layer, then cold rolled to 0.010 in. sheet. Specimens cut from the sheet were austenitized for 30 min at 1000°C (1830°F) in a vacuum tube furnace in which the pressure did not exceed 2 x 10-3 torr. Chemical analysis of specimens after austenitization indicated no decarburization at this pressure. Immediately before quenching, the furnace was filled with prepurified helium. The specimen was then pushed rapidly through an aluminum foil gasket, which sealed the bottom of the furnace, into an iced-brine bath (10 pct NaC1, 2 pct NaOH). The quenching rate at the M, temperature is about 104&apos;c per sec for 0.010 in thick specimens, as calculated from Newton&apos;s law of heat flow2 using a heat transfer coefficient of 25 ft-&apos;. This quenching rate is sufficiently high so that all the alloys transformed completely to martensite throughout the entire 0.010 in thickness and no carbide precipitation occurred in the martensite. All specimens were immediately transferred to liquid nitrogen after quenching and stored there until needed. Tempering below 250°C (480°F) was done in silicone oil baths thermostatically controlled to *;"C. Tempering above 250°C was done in circulating air furnaces or lead pots with the specimens contained in evacuated silica capsules. Electrical resistance was determined by measurement of the potential drop across both a standard resistance and the specimen, connected in series. All resistance measurements were made in liquid nitrogen (77K, -196°C) to minimize thermal scattering of electrons and thus maximize the contribution of impurity scattering to the resistance. Specimen dimensions were 5.10 by 0.19 by 0.025 cm. Although the precision in the electrical resistance measurements was +0.1 pct, the electrical resistivities could only be measured with an accuracy of +5 pct because of uncertainty in the specimen dimensions. Internal friction measurements were performed in an inverted pendulum apparatus at vibration frequencies of either 1.9 or 66 Hz. The specimen dimensions were 5.10 by 0.375 by 0.025 cm. Hardness measurements were made with a Leitz-Wetzlar microhardness machine with loads of 100 g. Specimens were examined by light microscopy after etching in 2 pct Nital and by electron transmission microscopy after preparation of thin sections by electrolytic thinning in a chromic-acetic acid solution.

Jan 1, 1970

By Charles H. Behre

KEYNOTE of the mining geology sessions was the preparation for an extensive war with all that this implies as to the need for strategic minerals, both metallic and nonmetallic. Nevertheless the sessions also included many papers of less urgent, more theoretical interest. The stress of wartime production had the effect of giving an unusually full and rich program, the longest in recent years, with sessions continuing virtually throughout the meeting. Some papers dealt with geophysical prospecting as applied to mining geology; others were concerned with the grand strategy of mineral reserves and thus involved the industrial minerals; such "borderline" subjects were presented before sessions held jointly with the Geophysics Committee or the Industrial Minerals Division.

Jan 1, 1942

Membership at the end of the year 1951 was 19,711 including 2228 Student Associates. The data in the third column include these Student Associates. 1. This includes all the cash dues income received from new and old members of all grades. 2. All cash initiation fees received. 3. Net income received from advertising in the three journals. The figure was $72,273, for MINING ENGINEERING; $39,844 for the JOURNAL OF METALS; and $31,564 for the JOURNAL OF PETROLEUM TECHNOLOGY. Income in 1950 was $54,572, $30,390, and $18,443 from these sources, respectively. 4. Receipts from individual sales, nonmember subscriptions, and multiple subscriptions of members. 5. Includes Transactions volumes and the Petroleum Statistics volume. 6. Sales of all other printed matter except special volumes sponsored by certain Funds. Includes a considerable sale of preprints and reprints of technical papers. 7. Does not include dividends and interest from certain Funds whose income reverts to those Funds. 8. Miscellaneous income not included in any of the above categories. 9. The total income compares with $493,197 -in 1950, an increase of $29000.

Jan 1, 1952

By J. L. Weeks

THERMAL conductivities of several samples of uranium and uranium alloys were determined using an apparatus previously described.&apos; The value previously reported for uranium,&apos; 0.035 cal per sec per cm per "C at 70°C, is in error due to the failure of a thermocouple during the determination on uranium. The defective thermocouple was detected after a reanalysis of the data obtained during the run and since has been replaced. Subsequently, runs on several samples of uranium show the thermal conductivity of uranium to be 0.069 cal per sec per cm per &apos;C at 70°C. The accuracy of the determinations was checked by measuring a sample of synthetic sapphire whose thermal conductivity was previously reported and found to be in agreement with other values."-" The values given in Table I are believed correct to % 3 pct or 0.003 cal per sec per cm per "C, whichever is larger. The samples were provided by J. H. Kittel of the Argonne National Laboratory, Metallurgy Div. References J. L. Weeks and R. L. Seifert: Apparatus for the Measurement of the Thermal Conductivity of Solids. Review of Scientific Instruments (1953) 24, pp. 1054-1057. J. L. Weeks and R. L. Seifert: Note Regarding the Thermal Conductivity of Synthetic Sapphire. Journal American Ceramic Society (1952) 35, p. 15. :&apos; J. Francl and W. D. Kingery: Thermal Conductivity: IV, Apparatus for Determining Thermal Conductivity by a Comparative Method; Data for Pb, Al2O3, BeO, and MgO. Journal American Ceramic Society (1954) 37, No. 2, Part 11, pp. 80-84. (Part 11: special issue on thermal conductivity.) &apos; W. D. Kingery, J. Francl, R. L. Coble. and T. Vasilos: Thermal Conductivity: X, Data for Several Pure Oxide Materials Corrected to Zero Porosity. Journal American Ceramic Society (1954) 37, No. 2, Part II, pp. 107-110. (Part 11: special issue on thermal conductivity.) Edwin Ruh: New Jersey Ceramic Research Station, Rutgers University. Private communication.

Jan 1, 1956

By Albert Sauveur

THE senior author of this paper has expressed the belief that when gamma iron transforms into alpha iron on reaching the A3 point, each gamma grain does not change bodily into one or more alpha grains but that the alpha phase forms first at the boundaries and along the crystallographic planes of the austenite grains.1 To quote: On cooling through the point A, at about 900° C., iron passes from the gamma condition to a. new allotropic form generally designated as alpha. This transforma¬tion, however, is not instantaneous. There are good reasons for believing that it begins at the grain boundaries and along the octahedral planes of the crystals and that it progresses until each grain of gamma iron is changed into a grain of alpha iron, the resulting structure being similar to that of gamma iron. Were it possible to retain at room temperature pure iron but partially transformed, it seems probable that a Widmanstättian structure, or rather, as later explained, a martensitic structure would be observed (Fig. 1), consisting of alpha iron at the boundaries and at the octahedral planes, and of a groundmass of gamma iron. In order to confirm, if possible, the accuracy of that view, a number of experiments were conducted. Polished samples of electrolytic iron were heated in a vacuum, maintained in the gamma range for several hours and quenched in different media. It was hoped by such means to produce and retain on the polished surfaces a pattern which would reveal the mechanism of the allotropic transformation. The samples were placed in evacuated quartz tubes, heated to 1000° C. and held 2 hr. at that temperature. The tubes were then immersed in the quenching bath. Iced brine and liquid air were used first. The polyhedral austenitic structure existing at the time of immersion was very clearly revealed (Fig. 2). This is generally ascribed to iron volatilizing at the grain boundaries.

Jan 1, 1929

By J. L. Tokich, A. R. Troiano

Since 1921, when Hull1 discovered that cobalt can exist in the face-centered cubic and hexagonal close-packed modifications, the transitions that occur in cobalt have been extensively studied. It is generally agreed that on heating the hexagonal lattice changes to the cubic structure at ternperatures ranging from 400° to 500°C although considerable doubt exists as to the exact temperature. Data concerning the temperature of the transformation on cooling are much less concordant and their interpretation has not been satisfactory. The study is further complicated by the fact that many investigators have reported the existence of a high temperature allo-tropic change in the range 850 to 1020°C, at which the cubic lattice reverts to the hexagonal modification. The transition on cooling, which has been reported as Occurring at various temperatures from approximately 400 to 100°C, is of particular interest. Troiano and Greninger2 have recently suggested and considered the possibility Of allotropic transformations occurring in pure metals by a shear-type, diffusionless (martensite) transformation. The case of cobalt was specifically discussed and certain observations of previous investigators evaluated in terms Of this type of Of Table 1 briefly outlines the methods and results Of previous investigators Of the transformation temperatures of cobalt. Materials and Methods The major portion of this investigatioll was performed with cobalt sheet containing a total of 0.2 pet impurities with carbon present to the extent of o,I pct. After melting in an induction furnace under an atmosphere of hydrogen, the carbon con. tent analyzed 0.03 pct. Some observations were repeated with hydrogen reduced cobalt compresses analyzing 99.9 pet pure. No significant variations in results were observed employing the as-received sheet, the remelted stock, or the cobalt compresses. Filings for X ray diffraction analysis were sealed in evacuated glass ampoules. Pyrex glass tubing was used for temperatures below (600°C and for higher temperatures clear fused quartz was satisfactory. After appropriate heat treatment at various ternperatures, the specimen ampoules were furnace cooled, air cooled or quenched by crushing under distilled water. This allowed a range of cooling velocities from less than one degree C per set to greater than 1,0oo°C per sec. X ray diffraction patterns were taken with a Debye camera and filtered characteristic cobalt K-alpha radiation. The of of the existing phases was roughly approximated by visual examina-

Jan 1, 1949

By F. C. Sturges

[CONTENTS PAGE ................. Introduction-Grouting in Mines. By F. C. STURGES. I Use and Technique of Pressure Grouting in the Construction Industry. By V. L. MINEAR . 3 Technique of Pressure Cementing in the Petroleum, Mining, and Construction Industries. By WY. D. OWSLEY and R. E. MOELLER. ..................... 9 An Example of Controlled Pre-grouting in Shaft Sinking. By R. H. ALLEN and J. W. GALPIN. 15 ........ Solidifying Mines and Shafts Areas by Pressure Grouting. By B. H. MOTT 17 .............. Grouting in Southeast Missouri District. By W. W. WEIGEL 20] Introduction-Grouting in Mines By definition the word "grout" means a thin mortar, or a kind of plaster or cement, and "grouting" means to fill up or finish with grout. The words "cement," "plaster" and "mortar" mean a substance that is used in a soft state which subsequently hardens. Thus, grouting is the filling of void space with a substance that hardens. Construction cements are the most common substances used, either by themselves or in mixtures, but the term grouting is applied quite correctly when other substances such as plastics and certain chemicals are used. Also, the use of the term grouting to cover the filling of voids with materials that do not actually become hard, such as the flotation tailings used in grouting in the southeast Missouri lead district, should be considered correct, as some stiffening does take place and, anyway, it is a better descriptive term than any substitute. Engineers are interested in grouting because some of the materials with which they must work contain voids, and certain conditions can be improved if these voids can be filled with something solid and permanent. Grouting is done to accomplish several purposes: I. To stop the passage of fluids and gases, 2. To cement materials together to make them stronger, and 3. To prevent consolidation of materials by filling void space with something solid as a replacement for the air and water that could be forced out under load. The construction industry uses grouting extensively for all three purposes. Grouting is used to stop water percolation under and around dams. It is used to control water flow in tunnel driving and in shaft sinking. It is used to improve foundation conditions under civil engineering structures by permanently filling void space and thereby reducing settlement, or by cementing broken rock together and increasing its supporting strength. The oil and gas industry does a lot of grouting, primarily to stop the passage of gases and fluids. The search for oil at increasingly greater depths has meant greater investment per well, and the oil industry has spent large sums on development of improved drilling methods. This

Jan 1, 1947

By Luis Elek

DEVELOPMENT of the cement industry in Mexico began some 40 years ago. It has gradually reached great importance in the economic life of the country and has contributed greatly to the technical and economical advances which have been so noteworthy, particularly during the last 15 years. From a modest start, the industry now comprises 18 cement-producing plants having a potential annual capacity of approximately 14 million bbl. About half the plants were built and equipped with second-hand machinery during the last world war when no new machinery could be procured. They will hardly attain full production before being modernized and reconditioned, a job now under way in several of the plants. At present, the yearly consumption is only about 8 to 9 million bbl but is steadily increasing. This is only a fraction of the cement consumed in the U.S.A., which is about 250 million bbl per year, although on the basis of consumption per capita per year, the figure is 1/3 bbl for Mexico and 1 2/3 bbl for the U.S.A. Cement consumption in Mexico is well above the average of all other Latin American countries, with the exception of the Argentine, and considering the potentialities and undeveloped riches of Mexico, the road construction and irrigation works, it is fair to assume that the Mexican cement industry will still prosper and expand in spite of temporary setbacks in the future caused by-local events of economic or political nature. Portland cement is manufactured by burning a mixture of raw materials, one of which is mainly composed of calcium carbonates and the other of aluminum silicates. The most typical materials answering this description are limestone and clay, both of which occur in Mexico in many varieties. To be usable for cement manufacture limestone should contain at least 77 to 80 pct calcium carbonate. Lower grade limestone can be used for cement manufacture only if the lime content is increased by the beneficiation process, which has not yet been adopted by the Mexican cement industry. Most of the limestone used by Mexican cement plants has a calcium carbonate content of 90 to 95 pct and therefore requires addition of one or several correction materials. A typical composition of raw mix for cement manufacture is 85 pct limestone and 15 pct shale, clay or volcanic materials. Occasionally it is necessary to add a smaller amount of sand or other siliceous material to increase the silica ratio in the raw mix. Likewise, it is sometimes necessary to add 1 or 2 pct iron ore to facilitate fusion in the kiln and to obtain proper relation between alumina and iron oxide. After calcining and

Jan 1, 1952

By Harold Vagtborg

Equilibrium vaporization ratios were obtained for light hydrocarbons, nitrogen, carbon dioxide, and hydrogen sulfide in a reservoir fluid containing 35 mole per cent hydrogen sulfide. The data cover the range from 700 to 2500 psia at 154°F. The results of this study are compared with results obtained by other investigators on systems containing less hydrogen sulfide. When large amounts of hydrogen sulfide are present, the equilibrium vaporization ratios for ethane and heavier hydrocarbons are greater than the ratios for systems containing little or no hydrogen sulfide. Large amounts of hydrogen sulfide have the reverse effect on the ratios for methane. Routine PVT studies were performed on the reservoir fluid including flash and differential liberations of the dissolved gas. The pressure-volume relationships of the saturated fluid were also determined. It is shown that the use of published correlations on physical properties of reservoir .fluids can lead to gross errors when applied to systems containing large amounts of hydrogen sulfide. INTRODUCTION Equilibrium vaporization ratios for various components in naturally occurring crude oil and condensate systems have been reported in the literature.1,2,3,4 Recently, several papers have been published with emphasis on non-hydrocarbon components such as nitro- gen, carbon dioxide and hydrogen sulfide.5,6,7,8,9 The increased discovery of reservoir fluids having high concentrations of these non-hydrocarbon components, particularly hydrogen sulfide, has created a need for a further study of their phase behavior. Equilibrium vaporization ratios are known to vary with pressure, temperature, and overall composition of the system.&apos;" It was anticipated that ratios for systems containing large amounts of hydrogen sulfide would differ from the ratios for systems containing small amounts of hydrogen sulfide. Therefore, the present work was undertaken in order to obtain reliable equilibrium vaporization ratios for the reservoir-fluid in question. PROCEDURE The procedure followed was evolved after considerable experimentation on methods of handling the very sour crude. It was found that drying agents (e.g. CaCl2 and CaSO4) absorbed an appreciable amount of hydrogen sulfide from the gas used to prepare the recombined samples. The concentration of hydrogen sulfide dropped as much as 10 mole per cent in a single pass through a 3-ft drying tube. It was also found that when undried gas was agitated with mercury in the PVT cell, a black scum, believed to be mercuric sulfide, was formed and the hydrogen sulfide content of the gas dropped several mole per cent. Because composition changes during a run could not be tolerated, separation of the mercury and sour fluid was necessary. In order to effect this separation, a stainless steel piston, equipped with Teflon O-rings, was placed in the PVT cell between the mercury and the sour fluid. This piston had to be constructed in three parts because

Jan 1, 1955

By Danforth R. Hale

Minerals for electronic and optical uses divide easily into two sections: (1) quartz and (2) minerals other than quartz. Quartz Quartz, having a great usefulness discovered by the radio communication enthusiasts about 1918, has become a subject of amazingly expanded interest in the U.S. over the past decade as a man-made mineral and a $3 million crystal-growing business. An economic summary of the commercial growing of quartz crystals has a place in a handbook directed to the mineral engineering industry when it is remembered that quartz crystals have long been an important commercial mineral, and that the raw material for “cultured quartz”- that is to say, quartz crystals grown through the ingenuity of man-is still natural quartz. Nearly all the natural crystals come from Brazil. The larger pieces which meet rigorous standards of quality are used for electronic and, to a lesser extent, optical components. Smaller pieces and fragments are used for vitreous silica. The need for high quality material in quantity led to U.S. government-sponsored research programs in the 1940s that have resulted in the factory growing of beautiful crystals of prescribed shape, size, and quality. The development of the cultured quartz crystal is typical of man&apos;s success in adapting the product of the mine to increasingly sophisticated uses. A remarkable achievement perhaps, but foreshadowed by experiments in 1908 by Giorgio Spezia (1908), an Italian geologist studying the relative effects of temperature and alkaline environment on the solubility of quartz. Modern radio equipment is most often controlled as to frequency by the presence in the circuit of a separately added "crystal"-the 1918 discovery responsible for the existence and growth of the quartz industry. The "crystal" is quartz, but this component is a carefully oriented and prepared slice from a crystal, but not a crystal as recognized by a rock hound or seen in a museum. How quartz operates to control frequencies is not a proper subject for a handbook on industrial minerals, and references should be consulted (Cady, 1964; Mason, 1964). Quartz belongs to that class of materials called dielectrics: those that do not conduct an electric current but permit electric fields to exist and act across them. Quartz shows the "piezo-electric effect," which means that when a quartz plate is mechanically deformed against its natural stiffness, one of its surfaces becomes negatively charged, the other, positively charged. When the plate is released from the stress quickly, the charges disappear as the plate regains its original shape, but because of mechanical momentum the plate deforms in the opposite direction (to a lesser amount) and the surfaces correspondingly become charged in the opposite direction. By coating the two surfaces thinly with metal and attaching flexible wires, these charges may be brought into an electronic circuit. If the surfaces are suddenly electrically charged by movement of current through the wires, the "converse piezoelectric effect" occurs -the plate deforms. Carry the thought further and it is realized that an alternating current flowing through the wires responds to the mechanical oscillation of the plate and is keyed to this oscillation. By controlling the thickness of the plate its mechanical vibration frequency can bevaried through a wide range. One type of quartz plate, called the AT-cut, having a precisely defined orientation with respect to the crystallographic axes of the crystal, vibrates on a microscopic scale much as a book would deform when placed flat on a table and the top cover moved parallel back and forth with the hand. There are at least 17 other orientations which have been studied, some of

Jan 1, 1975

By Y. C. Liu, G. A. Alers

The effect of rolling reduction on the textures of Cu-A1 alloys has been investigated both by pole figure and by modulus methods. In alloys which exhibit complete copper or brass types of rolling texture, the rolling reduction has little effect on the texture except to increase the degree of preferred orientation. In alloys which exhibit a transition texture, however, increased rolling reduction increases the amount of brass-type texture at the expense of the copper-type texture. The present experimental results show that there is no one-to-one correspondence between the SFE and the rolling texture of fcc metals. Additional data taken from the literature for fcc metals also support this conclusion. On the other hand, the present and previous experimental results are shown to be in good agreement with the suggestion that the texture transition occurs at a critical value for the separation distance between two partial dislocations—a consequence of the "dislocation interaction" hypothesis for texture. formation. This critical separation occurs when the parameter .r/ub is 3.75 x 10&apos;3. From this, a value for the SFE of 39 ergs per sq cm may be deduced for a Cu-2.85 at. pct A1 alloy. ThE correlation between the rolling texture of fcc metals and the stacking fault energy, SFE, was one of the first attempts to relate atomistic properties with the type of rolling texture.&apos; This correlation gives a qualitative explanation for the experimental observation that the addition of alloying elements, which generally lower the SFE, changes the copper-type texture to a brass-type texture. The simplicity of this correlation had led to its general acceptance and even its quantitative use.&apos; However, it is only a correlation and is largely based on descriptive features of pole figures, and on the poorly known SFE values in dilute alloys. Quantitative verification of this phenomenologi-cal correlation is, in fact, completely lacking. One purpose of the present study is to test this correlation. Another atomistic description for the formation of rolling texture is the "dislocation interaction" hypothesis of texture formation.3 In this hypothesis, the factor controlling the type of rolling texture depends on whether or not the separation distance between two partial dislocations exceeds a critical value. Materials having a separation of less than the critical value are supposed to exhibit a copper-type texture while those with a separation above the critical value are supposed to have a brass-type texture. At the critical value, it is expected that the material should show equal amounts of copper- arid brass-type orientations in their textures, i.e., a 50 pct transition texture. The SFE appears in this hypothesis as only one of several factors which determine the separation distance between partial dislocations. It is possible to test the validity of these two concepts by studying the rolling texture as a function of rolling reduction. Since the SFE per se is an intrinsic property of the metal, it should not, by definition, be influenced by local irregularities, such as variable stress conditions. Thus, no change in texture-type is expected to occur with changes in rolling reduction. On the other hand, according to the "dislocation interaction" hypothesis, any factor that effectively influences the separation distance of partial dislocations would be expected to change the rolling texture. Since the separation distance between partial dislocations is known to depend upon local stresses,4-6 it is anticipated that there would be an effect of the degree of reduction on the texture-type. Also, since applied stresses are more likely to increase, rather than to decrease, the separation between partials,4&apos;5 the overall effect would be to increase the amount of material in the brass-type orientations as rolling reduction is increased. Furthermore, this reduction dependence would be most prominent in alloys exhibiting the transition texture since the distance between partials in those alloys is thought to be close to the critical value. Experimental data in the literature is insufficient to distinguish between these two alternatives. Haessner studied the effect of rolling reduction on textures in a series of Ni-Co alloys by means of the X-ray intensity-ratio technique,&apos; and found that while one texture parameter indicated no reduction dependence the other indicated a slight dependence of the rolling texture on reduction in the range of 96 to 99 pct. As has been noticed previously, the intensity-ratio technique is a convenient but controversial method7 because there is no a priori reason to suggest which intensity-ratio would describe the texture most meaningfully. A more quantitative method of describing textures is found in terms of the orientation dependence of Young&apos;s modulus. Here, the type of modulus aniso-tropy associated with the copper-type texture is sufficiently different from that observed for the brass-type texture to allow the two types to be easily distinguishable and a quantitative measure of the amount of each can be deduced from the numerical results. This ability to provide quantitative data is particularly valuable when the two textures occur simultaneously in one alloy as is the case for the transition textures. In this paper the modulus method, supplemented by pole figure data, is used to look for an effect of roll: ing reduction the texture. Also by combining the texture measurements with recent determinations of the SFE in Cu-A1 alloys&apos;0&apos;" it should be possible to test for a relationship between the SFE and textures.

Jan 1, 1970