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By Mark C. Malamphy, Irnack C. Do Amaral

Four magnetic fleld balances and several spare magnetic systems were purchased by the Brazilian National Department of Mineral Production from the Askania Werke A. G., of Berlin, in 1932. Preliminary field tests on this new equipment showed one of the vertical component magnetic systems to be defective. A series of measurements designed to investigate the functioning of these instruments, and particularly the defective system, showed it to have an abnormally low magnetic moment, as compared to the satisfactory systems, and a high-temperature correction that was opposite in sign to that which would be expected for a noncompensated magnetic system. Since these systems were of the "temperature compensated" type, this condition indicated an accidental overcompensation. Attempts to correct for this overcompensation by readjustment of the compensating masses on the aluminum and Invar spindles failed because the distance by which the position of the masses could be shifted was insufficient. The temperature effect was reduced by this readjustment but was not entirely eliminated, as was to be desired. Theoretical deductions indicated that the defective condition of the system could be explained as due to three possible causes: (1) considerable loss of magnetic moment of the system; (2) increase in the magnetic temperature coefficient of the laminas; (3) dislocation of the component parts of the system caused by a shock experienced after it left the factory and before it was tested in Brazil. Later information received from the factory after examination of the returned system indicated that the third cause probably played the most important role. Temperature calibrations of the defective system for various positions of the counterweights brought out an important point, which it is believed

Jan 1, 1940

By Irnack C. Do Amaral, Mark C. Malamphy

Four magnetic fleld balances and several spare magnetic systems were purchased by the Brazilian National Department of Mineral Production from the Askania Werke A. G., of Berlin, in 1932. Preliminary field tests on this new equipment showed one of the vertical component magnetic systems to be defective. A series of measurements designed to investigate the functioning of these instruments, and particularly the defective system, showed it to have an abnormally low magnetic moment, as compared to the satisfactory systems, and a high-temperature correction that was opposite in sign to that which would be expected for a noncompensated magnetic system. Since these systems were of the "temperature compensated" type, this condition indicated an accidental overcompensation. Attempts to correct for this overcompensation by readjustment of the compensating masses on the aluminum and Invar spindles failed because the distance by which the position of the masses could be shifted was insufficient. The temperature effect was reduced by this readjustment but was not entirely eliminated, as was to be desired. Theoretical deductions indicated that the defective condition of the system could be explained as due to three possible causes: (1) considerable loss of magnetic moment of the system; (2) increase in the magnetic temperature coefficient of the laminas; (3) dislocation of the component parts of the system caused by a shock experienced after it left the factory and before it was tested in Brazil. Later information received from the factory after examination of the returned system indicated that the third cause probably played the most important role. Temperature calibrations of the defective system for various positions of the counterweights brought out an important point, which it is believed

Jan 1, 1940

By C. M. Wayman, R. Bullough

The selection rules fir twinning in fcc, bcc, and hcp lattices as established in Part I are used to predict the positions, relative to the matrix (untwinned) reciprocal lattice, of reflections due to double diffraction from the twins. These doubly diffracted reciprocal lattice points, which often coincide with ordinary matrix reciprocal lattice points, are deduced from kinematical considerations. 1. INTRODUCTION. A Bragg diffracted beam under certain conditions may be rediffracted to produce a third beam i .e., the incident beam, the first diffracted beam, and the rediffracted beam). In such a case an initial incident beam is diffracted by a set of planes; the diffracted beam may then be rediffracted by a second set of crystallographically different planes. The initially diffracted beam acts as an incident beam for the second set of planes, thus resulting in a twice-diffracted beam. This twice-diffracted beam may be regarded as a singly diffracted beam from a set of lattice planes whose structure factor is zero. In order to find the reciprocal lattice point corresponding to the doubly diffracted beam, it is customary1,2 to combine vectorially the component reciprocal lattice vectors which head to the extra reflections. For example, hcp metals may exhibit the forbidden (0001) reflections.* As Fig. 1 shows, the (0001) reciprocal lattice point results from: (1010) + (1011) = (0001) Similarly, combination of the beams (1011) and (1010) gives rise to: (1011)- (1010) = (0001) As Pashley and stowell2 have pointed out, even if in fact the double diffraction points lie on the Ewald sphere, they may not actually represent observed doubly diffracted beams because the initially diffracted primary beam, i.e., the source, must also correspond to a reciprocal lattice point which lies on the sphere of reflection; however, the reciprocal lattice point corresponding to the planes causing the rediffraction need not lie on the sphere. A little consideration of the Ewald construction in Fig. 2 makes this argument clear. In Fig. 2 the incident beam is represented by the wave vector ko. This beam is initially diffracted by the lattice planes (hkl) which are represented by the reciprocal lattice vector r(hk1) The reciprocal lattice point (hkl) of course lies on the Ewald sphere in order that the Bragg condition be satisfied. The initially diffracted beam is represented by the wave vector kl. If now kl is rediffracted by a second set of planes (h'k'l') resulting in k2 the lattice point (h"k"l") must lie on the Ewald sphere if the double diffracted beam k2 is to be observed. It is clear that (h"k"l") is the vector sum of (hkl) and (h'k'l'), and that (h'k'l') need not in fact lie on the Ewald sphere. In the usual1,2 analysis the origin (000) of the reciprocal lattice is shifted to the point (hkl). However the translation (000)— (hkl) automatically shifts the point (h'k'l') to the Ewald sphere, i.e., (h'k'l')— (h"k"1"). It is to be seen that (hkl), the source reflection, must lie on the Ewald sphere; if it does not the translation (000) — (hkl) places the "new" origin off the sphere, not satisfying the Ewald construction and hence the Bragg condition. The point (h"k"1") of course must lie on the sphere if it corresponds to an observed doubly diffracted beam. It is to be noted that crystals having the hcp structure, as just discussed, are intrinsically capable (i.e., without lattice defects such as twins) of double diffraction, as contrasted to fcc and bcc crystals which are extrinsically capable (requiring lattice defects or reoriented lattice regions). The "allowed" bcc reciprocal lattice points (which comprise an fcc lattice) are (110), (2001, (211), (220), (310), (2221, (321), (4001, and so forth. The combination

Jan 1, 1967

By T. Rosenqvist

From the chemical, metallurgical, and mineralogical points of view, the importance of thermodynamic data for metal-sulphides and sulphur dissolved in molten metal has long been realized. Such data will give a basis for thermo-dynamic calculations of processes such as roasting and the distribution of sulphur between molten metal and slags. Furthermore, it will help us understand the chemical forces which tie sulphur to the metal and to the melt. Thermodynamic studies of solid sulphides and the equilibria between solid sulphides and metals have been carried out in a rather large number of cases by several investigators. An excellent review of this work is given by Kelley.1 On the other hand, very little is known about the thermodynamic properties of molten sulphides and of sulphur dissolved in molten metal. The only system which previously has been investigated in this respect is the iron/sulphur system. The purpose of the present investigation was primarily to obtain further data for metalisulphur melts and the system silver/sulphur was chosen, not because this system was expected to be of special interest in itself, but because the silver/sulphur system is a typical example of a metal/sulphur system. Because of the low melting temperatures, the work could be carried out without appreciable furnace and refractory difficulties. The sulphur in this system possesses a rather high escaping tendency compared to most other metal/sulphur systems. By the method employed (reaction with hydrogen to form hydrogen sulphide) this gives ratios Ph2s/Ph2 up to 0.30, which may be determined accurately. 'rhermodynamic investigations of the heterogeneous reaction Ag2S +H2 —+ 2Ag + H2S have previously been carried out by Pelabon,2 Keyes and Felsing,3 Jellineb and Zakowski,4 Wat-anabe,6 and Britzke and Kapustinsky.6 Their results are in rather poor agreement. Experimental Part PRINCIPLE In the present invehgation the escaping tendency of sulphur from the condensed phase was determined by the reaction: S + H2 = H2S The ratio Ph2s/Ph2 is at constant temperature, directly proportional to the escaping tendency of sulphur and to its chemical activity in the condensed phase. (This ratio will subsequently be denoted by H2S/H2.) From this ratio and its variation with temperature and with change in the com- position of the condensed phase, thermodyrlamic quantities such as free energy and heat of reaction can be derived. The apparatus used is shown in Fig 1. The silver/sulphur alloy was placed in a crucible inside a refractory tube and mounted inside the furnace to the left. The tube was a part of a closed, gas-tight system in which the gas mixture could circulate until equilibrium was established. Circulation was maintained by the glass propeller to the right, driven by an external magnet, and promoted by the chimney action of the furnace. The gas passed up through the furnace, down into the crucible where it came in contact with the alloy, passed rapidly up through a narrow tube and out of the hot zone. After equilibrium was established between the gas and the condensed phase, the composition of the gas mixture was determined from its density. In its circulation, the gas mixture passed through a chamber (lower right on Fig 1) containing a buoyancy-balance, where the density of the gas was determined by magnetic balancing. From the measured density,

Jan 1, 1950

By Donald D. Carr, Lawrence F. Rooney

Perhaps no other mineral commodity in this volume has as many uses as limestone and dolomite. These carbonate rocks are the basic building blocks of the construction industry, the material from which aggregate, cement, lime, and building stone are made. Carbonate rocks, and their derived products, are used as fluxes, glass raw material, refractories, fillers, abrasives, soil conditioners, ingredients in a host of chemical processes, and much more. Although the use of limestone and dolomite goes back before recorded history, new uses and products are continually being found. Carbonate rocks form about 15% of the earth's sedimentary crust and are widely available for exploitation. Found extensively on all continents, they are quarried and mined from formations that range in age from Precambrian to Recent. Reserves of carbonate rock are large and will last indefinitely, although high-purity deposits may be absent or have limited availability in certain areas. Limestone and dolomite are so useful and so abundant that in 1981 about 644 million tons were produced in the United States. In fact, about 75% of all stone quarried or mined in the United States was carbonate rock. Sand and gravel was the only mineral commodity produced in greater quantity. In this chapter we have sought to provide the general reader an overview of carbonate rocks, their composition, distribution, production, and uses, with emphasis on developments since 1960. In doing so we borrowed extensively from our report on the applied geology of limestone and dolomite (Rooney and Carr, 1971). The literature on the limestone and dolomite resources of the United States and Canada is so vast and diverse that one can easily become mired down in print. We tried to list those references that are easily accessible and that provide the economic geologist with a starting point for more intensive study. The table listing selected references on limestone and dolomite resources in Canada and the United States reflects our attempt to be selective rather than exhaustive and to direct the reader to the best sources of detailed information. Geology Mineralogy The principal carbonate rocks used by industry are limestone and dolomite. Limestones are sedimentary rocks composed mostly of the mineral calcite (CaCO3) and dolomites are sedimentary rocks composed mostly of the mineral dolomite (CaCO3 • MgCO3). Aragonite (CaCO3), which has the same chemical composition as calcite but a different crystal structure, is economically important only in modern deposits, such as oyster shells and oolites. Aragonite is metastable and alters to calcite in time. Some other carbonate minerals, notably siderite (FeCO3), ankerite (Ca2MgFe (CO3)4), and magnesite (MgCO3), are commonly found associated with limestones and dolomites but generally in minor amounts. Because of their similar physical properties, the carbonate minerals are not easily distinguished one from the other. Specific gravity,

Jan 1, 1983

By N. S. Stoloff, J. N. Mushovic

Age hardening response of a Mg-Th-Zr alloy has been studied at temperatures in the range 60° to 450°C. Transmission microscopy revealed clustering of thorium atoms at low aging temperatures, supporting a previous report of GP zone formation. Peak strengthening, which is observed at 325°C, is due to the formation of a coherent, ordered, DO19 type superlattice structure, of Hobable composition Mg3Th, as plates parallel to the matrix prism planes. These plates later reveal a Laves phase structure of composition Mg2Th. The equilibrium Mg4Th phase begins to precipitate in two different forms at an early stage, competitively with the Mg2Th plates. RECENT work on the Mg-Th system indicated that, unlike most magnesium-base alloys, complex precipitation phenomena may be occurring. The partial phase diagram of the Mg-Th system indicates that an equilibrium phase, Mg5Th, is the sole intermediate phase.' sturkey,' however, has reported, using X-ray and electron diffraction techniques, that a metastable fcc Laves phase, Mg2Th, precedes the formation of the equilibrium compound, which he identified as closer in composition to Mg4Th. Murakami et al.3 reported that the equilibrium phase precipitates preferentially on grain boundaries and dislocations in a Mg-1.7 wt pct Th alloy; Kent and Kelly4 aged a more dilute alloy, Mg-0.5 wt pct Th, for 4 days at 220°C and found similar results. In addition, they reported that a platelike phase with a structure close to that of the magnesium matrix forms perpendicular to the basal plane and is probably ordered. Research on a Mg-4 wt pct Th alloy by electrical resistance measurements and transmission electron microscopy has suggested that GP zones may form at low aging temperatures.3 However, the electron micrographs purporting to show this phenomenon were not conclusive. In view of the fragmentary evidence concerning the nature of the precipitation processes in the various Mg-Th alloys, an aging study was undertaken to clarify the characteristics of the various precipitates which form and to correlate the mechanical properties of the system with the direct precipitate-dislocation interactions. The latter results are presented elsewhere.' The purpose of this paper is, therefore, to discuss the precipitation sequence in this system. EXPERIMENTAL PROCEDURE Sheet stock (0.060 and 0.010 in. thick) of a commercial Mg-3.93 wt pct Th-0.42 wt pct Zr alloy (designated HK3lA) similar to that studied by sturkey2 was supplied through the courtesy of Dr. S. L. Couling of Dow Metal Products Co. Zirconium does not enter into any precipitation reactions,' but is present primarily as a grain refiner. The alloy was chill cast, warm rolled to 0.090 in. thick stock, and then finally reduced by a combination of hot and cold rolling. The alloy chemistry is given in Table I. This material was solution treated at 580°C for 4 hr in a dry CO2 atmosphere, and then water quenched. Material in this condition was fairly clear of precipitate particles and was fully recrystallized. Aging at temperatures less than 200°C was accomplished by immersing the alloy in a silicone oil bath; for higher temperatures, aging was done in a salt pot. Age hardening treatments were conducted at 60°, 80°, 105°, 135°, 160°, 250°, 325°, 350°, and 450°C for times ranging from 5 min to 400 hr. Hardness tests were performed on chemically polished 0.060-in.-thick blanks of solution treated material which were aged at the various temperatures for increasing lengths of time. For aging temperatures above 150°C the Rockwell Superficial 30T scale was employed, while samples hardened at temperatures below 150°C were monitored with the 45T scale. Each data point consists of at least three separate readings. Yield stresses also were measured at room temperature on both 0.060 and 0.010 in. sheet specimens aged at 325°C. The aged foils were thinned by the window method in a solution of 80 pct absolute alcohol and 20 pct concentrated perchloric acid (70 pct) maintained at 0°C. A stainless steel cathode was used and the applied voltage was 10 to 15 v. Thinned samples were rinsed in distilled water and pure methanol. After the me-thanol rinse the thin foils were quickly dried between filter paper. Foils prepared by the above method were examined in a Hitachi HU11B electron microscope operating at 100 kv. RESULTS A) Hardness. The hardness data are depicted in Figs. 1 and 2. Peak strengthening occurs at 325°C after aging about 6 min, see Fig. 1. Significant strengthening is achieved also at 350°C, but aging at 450°C produces only softening. The stepped curve at 250°C indicates that a complicated precipitation process may be occurring at that temperature. Fig. 2 suggests that at least two hardening mechanisms exist since the lowest temperature hardness peaks are displaced to the left of the peaks obtained at 135° and 105°C. A great deal of scatter is observed at long times in all cases due to magnesium surface degradation caused by the silicone oil bath. B) Identification of the Strengthening Precipitates. The structure formed atlowagingtemperatures (c10O°C) was not clearly resolvable by transmission microscopy. The only bright-field evidence for a change in structure was a mottled appearance which could be observed at extinction contours, as shown in Fig. 3(a), and the disappearance of this effect when dislocations produced under the influence of the electron beam passed through the matrix, as noted in

Jan 1, 1970

By Lane Mitchell

A ceramic product or processed material is a solid composed of materials which have been subjected to heat above 468.3°C (875°F). The raw materials, which are blended together (or in some cases used singly), are selected and utilized for various reasons such as ease of fabrication, aid to processing, to yield desired properties after processing, lack or controllable degree of toxicity or hazard, availability, cost, and perhaps other considerations. Almost all solid inorganic, some organic, and some liquid and gaseous materials have the potential to be used individually in some ceramic product. There are several fundamental functions to be fulfilled in every ceramic product and a number of secondary functions are desirable in specified products. These functions are generally met by the most widely occurring minerals and rocks of the earth and their debris. This fact characterizes ceramics as a field utilizing the raw materials most available to man. Of course, specified products utilize synthetics, organics, and rare inorganics to produce desired results. Any solid nonmetallic product processed by subjection to temperature above a red heat may be called a ceramic product. Widely used construction materials and units, domestic utensils and units, industrial parts to facilitate manufacture, technical components, and aesthetic creations are very often of a ceramic nature because of their durability, inertness, hardness, ease of fabrication, cost, and availability of the ingredients. Often, organics or metals cannot meet desired specifications for some of these products. The rocks and minerals and mineral debris of the earth are largely siliceous. Oxygen and silicon comprise roughly 75% of the earth's crust with aluminum, iron, calcium, and the alkalies following in abundance. Silica (SiO2) and silicates can be melted to form glasses. Alumina (A1203), present in a mineral compound, gives greater durability, hardness, and strength, but lessens the glass-forming property. Iron, calcium, and the other alkalies flux silica and reduce melting points. Thus sand, which is generally almost pure SiO2, and clay, which is generally hydrated alumina silicate, are the most widely used of all ceramic raw materials-principally because of the glass-forming propensities of silicates. In ceramic formulations, clay is generally a refractory filler or skeletal material, having in the raw state a plasticity derived from its colloidal grain size and its water-loving nature. On the other hand, silica sand is a glass former or nonplastic filler. Clay and silica sand in pure forms are quite refractory, i.e., not easily melted. Clay, although siliceous, is less of a glass former than pure silica and is more refractory. Natural contaminants, such as iron oxide or limestone, adulterate many clays and some sands. These contaminants act as fluxes and reduce the fusion points of the mineral or blends. Glass is made from silica sand by fluxing the sand with strong bases, usually soda ash and limestone. Red building bricks are hard and durable because the sand and clay have been partially fused with help of natural iron oxide serving as a flux. The iron oxide performs a dual function, serving as a pigment as well as a flux. In a blend of clay and sand and iron oxide, the sand is more susceptible to fusion than is the clay. Although silica sand and clay are the most widely used raw materials in most ceramic products, many other minerals, and some nonminerals are utilized in products where these materials can produce or aid in achieving desired results. Limestone and dolomite, feldspars, pigmentary minerals, refractory oxides or carbides, and special property producers can

Jan 1, 1983

By I. S. Servi, N. W. Marr

TIN markedly increases the softening temperature of pure copper with only a moderate effect on conductivity. Smart and smith' indicated a substantial increase in softening temperature upon addition of different levels of tin up to 0.05 pct in oxygen-free copper. However, after finding no effect of tin in copper containing about 0.025 pct O, they concluded that "the presence of oxygen completely nullifies these changes in properties by precipitation of SnO2.'' Since preliminary tests on Cu-Sn-0 alloys indicated that this conclusion is not valid outside the extremely limited tin range investigated by Smart and Smith, research was primarily directed toward the partition of tin between the copper-base matrix and the oxide phases. Experimental. Material was prepared by sealing an 80 to 100-g charge consisting of oxygen-free copper, tin, and copper oxide into a y-in.-ID quartz capsule which was evacuated and back-filled with tank-grade argon to 3 atm. The sealed vials were heated to 1125ºC, kept at temperature for 30 min, occasionally agitated, and then allowed to air-cool outside the furnace ("as-cast"). The castings were cold-swaged to 0.370 in., annealed 1 hr at 600°C ("as-annealed"), and cold-swaged 16.5 pct ("as-swaged"). Cross sectional wafers were annealed for 1 hr at various temperatures and Rockwell F hardness measured. The "softening temperature" was defined as the interpolated temperature at which the hardness was 50 Rockwell F. Electrical resistance was measured by an ac poten-tiometric method on 0.040-in.-diam wires after a 1 hr anneal at 600°C. Relative accuracy was of the order of 1 pct. Chemical analyses for tin were performed by two methods, identified as "Acid flux" and "HN03 dissolution". The first consisted of fusing the sample with potassium pyrosulfate and leaching the resulting melt with 10 pct sulfuric acid. The spectrophotometric procedure which followed is described in Ref. 2. Oxygen analyses were performed by the vacuum-fusion method with a bath temperature of 1650°C. Tin content of oxides and copper phases was measured with the X-ray microprobe, using a calibration curve based on a series of oxygen-free Cu-Sn alloys. Results. In Fig. 1, the nominal tin composition for alloys containing nominally 400 ppm O was plotted vs the analyzed or the computed tin content—the latter derived from one of the following: 1) "acid flux" chemical analysis; 2) "HN03 dissolution" chemical analysis; 3) X-ray microprobe analysis of the copper matrix; 4) equivalent tin content, based on the measured increase in electrical resistivity (an increase in resistivity of 1.6 microhm-cm is approximately equivalent to 1 wt pct of sn1,3). It is evident from Fig. 1 that the results of the acid flux analysis are consistent with the nominal composition while the HNO3 dissolution method generally yields lower values, consistent with those obtained from electrical resistivity measurements and somewhat higher than those obtained by microprobe analysis. Microprobe and resistivity values are affected only by the tin in solid solution; hence the HN03 method

Jan 1, 1970

By G. D. Bengough

CORROSION tests should be designed so as to facilitate as far as possible the interpretation of results, consequently factors which may affect the rate of corrosion should be controlled as far as practicable, and very full data should be given regarding the conditions of the test. Among the most important factors affecting the rate of corrosion is often the rate of supply f oxygen to the metal surface. It is essential therefore to understand the mechanism by which oxygen is transferred from the liquid surface to the surface of the metal. The work of Adeney and his coworkers has thrown much light on this mechanism. They have shown1 that the aeration of deaerated water and salt solutions proceeds much more rapidly than can be accounted for by mere diffusion, and have suggested that downward "streaming" takes place from the surface of the water, due mainly to an increase of density brought about by evaporation. The evaporation reduces the temperature of the surface layer, and also increases the concentration in the case f salt solutions. The effect of evaporation in facilitating the transfer of oxygen to a metal and increasing the corrosion f the metal was shown in some experiments due to Friend .2 He tested the corrosion f mild steel plates immersed in water in glass jars, a steady stream f air being drawn over the surface of the water in the jars. The air passing through half the number f jars was saturated with moisture, that passing through the others was dried with calcium chloride. He found that "in every case the water exposed to dry air was approximately twice as corrosive as that exposed to air saturated with water vapor."

Jan 1, 1929

By J. H. Brophy

Experimental evidence in recent years shows that nickel coated hydrogen reduced tungsten powder can be sintered to 98 pct of theoretical density at 1100°C. New data indicate that the sintering rate is the same for nickel contents ranging from 0.125 wt pct (mon-atomic layer) to 5.0 wt pct Ni coated on 0.561. tungsten powder. Nickel tungsten made by coreduction from oxides sinters in a kinetically similar way, but the rate tends to increase with higher nickel contents. The activation of sintering can be accomplished with a minimum amount of nickel if coated powder is used. Transverse rmpture strength was found to increase in specimens containing 0.25 pct Ni as density increased during the initial stage of the carrier-phase sintering process. Upon the onset of grain growth in the final stage, strength was found to decrease. With increasing nickel contents up to 4 pct, strength increased. Maximum strengths in three-point loading were observed at 73,000 psi for 0.25 pct Ni and 93,000 psi for 5 pct Ni. These were comparable to that of massive tungsten recrystal-lized in the presence of nickel and tested in the same way. The results were sensitive to the mode of powder treatment and ductility was negligible in all cases. The study and application of sintered bodies of nickel and tungsten is not new; however, the analysis of the mechanism by which small additions of nickel increase the sintering rate of tungsten promises to Contribute new information regarding sintering theory in general. Initial experimental evidence was presented by the authors showing that nickel-coated hydrogen-reduced tungsten powder may be sintered to 98 pct of theoretical density at 1100°C in 16 hr.' Simultaneously, a kinetic analysis of the process showed that it took place in two distinct stages. In the first stage, nickel evidently served as a carrier phase through which tungsten atoms could move. This stage was kinetically similar to the 'solution-precipitationo step postulated when the carrier phase is liquid3 although in the nickel tungsten case, there is no evidence of the existence of a liquid phase either in equilibrium phase relationships or in mi-crostructures at the temperatures under consideration. In the present work, new data for nickel-coated tungsten powder are offered in support of the proposed mechanism, and a more explicit study of the second stage of densification is presented. Concurrently, the sintering kinetics of these coated powders are compared to Ni-W powder made by coreduction of oxides. In this way the present work can be compared to earlier results in nickel activated sintering of tungsten in which the coreduction process was emplyed. The ultimate utility of such an activated sintering process will be determined to some extent by the mechanical and physical properties of the final prod-

Jan 1, 1962

By A. D. Taylor

In recent years there has been an increasing effort to attract students into engineering. Obviously, the effort is necessary because young people find the image of the engineer unattractive. Some of the things they find unattractive are real, some are not, and part of the problem is too little knowledge of the field. First, I would like to comment on some of the ideas which appear to be justified. Engineering is a difficult course of study. True, and nothing can or should be done to change this. The education is continually being improved, but it is unlikely to be made easier.

Jan 1, 1970

By J. P. Heller

The purpose of this discussion is to comment briefly on one of the points raised in the paper. The topic is that referred to in the Conclusion 2, in which the authors note a "disproportionate increase in mixing rate" as they proceed from a displacement performed at viscosity ratio 0.998 to one at 1.002. The recovery curve of this displacement, Fig.2A, shows a quite noticeable difference between the two runs in which displaced and displacing liquids were interchanged. This difference is ascribed by the authors to the change in viscosity ratio between the two experiments. This interpretation of the experimental results must certainly be based on rather precise measurements of the fluid viscosities or, at least, of the ratio of their viscosities. The ordinary Ostwald viscometer, employed in the usual way, is only just able to distinguish between liquids whose viscosities differ by two or three parts per thousand. The experimental refinements which then must have been necessary to measure with any precision a viscosity ratio of 1.002 would be worthy of mention. Indeed, one would have expected the authors to devote at least a paragraph to the display of this technique. For the same reason - to emphasize that the details of such unusually critical experimental work should be reported and discussed in the literature — I would have liked to see some comment by the authors on the requirements for temperature control during both the viscosity measurements and the displacement experiments. The temperature coefficient of viscosity of Soltrol C at room temperature has been measured in this laboratory at about - 1.9%/1°C. How much did the coefficients for the fluid mixtures used in the experiment differ from this and from each other Even if the two fluids were identical in this respect, it would appear that a temperature difference of .l°C between them in the flow system would produce a viscosity con- trast equal to that imposed by their composition. Reference to the experimental solutions of these problems would render Conclusion 2 more credible. Published theoretical work on the stability problem contains no indication of such extreme sensitivity to the viscosity ratio in the immediate neighborhood of unity. On the contrary, perturbation calculations such as those made by Chuoke1 and Perrine2 lead to initial finger growth rates proportional to the first power of the viscosity difference. The later instability growth calculated by Scheidegger,3 using the assumption of zero pressure gradient perpendicular to the average flow, is also simply proportional to the viscosity difference. The conflict regarding the sensitivity of the dependence of instability growth or mixing rate on the viscosity contrast needs explicit recognition in the literature. In particular, it would seem that the experimental work reported here should be supported by a more detailed description of the viscosity controls. Further discussion of possible alternative interpretations of the data would also be in order. For instance, is it possible that the unconsolidstted bead pack used changed its characteristics between the runs (due, perhaps, to the handling and inverting involved in the injection of the front) Or, are the data points of Fig. 2A averages from several runs performed in a series in which the two liquids alternated as displaced and displacing fluids? To summarize, it seems to me that the relationship asserted by Conclusion 2 in the paper needs the support of more detailed experimental evidence. REFERENCES 1. Chouke, R. L., van Mews, P. and van der Poel, C.: "The Instability of Slow Immiscible Viscous Liquid-Liquid Displacements in Porous Media", Trans., AIME (1959) Vol. 216, 188.

By D. A. Stevenson, R. A. Burmeister

Single-phase silver antimony telluride has been prepared by zone-melting techniques using initial compositions of A new phase appears upon prolonged annealing of this material, but the reaction does not appear to be a simple eutectoid decomposition. A complete analysis of the phase equilibria is complicated by the slow kinetics involved. The Hall coefficient, magneto -resistance, electrical resistivity, and Seebeck coefficient are all sensitive to the presence of second phases. The low Hall mobilities measured for single-phase material indicate that the usual band theory is inadequate to explain the observed transport properties in the system. Density anomalies of up to 2.5 pet between measured and theoretical density were observed but are not conclusive evidence for a defect structure. COMPOSITIONS in the Ag-Sb-Te system have been studied previously by several investigators.1"18 The interest in this system arises from potential thermoelectric applications of alloys on the Ag2Te-Sb2Tes vertical section. Although the composition corresponding to the formula AgSbTe, has received most attention, it has been found to consist of more than one phase.7'8 A thorough understanding of the properties of this heterogeneous material has been impeded by both lack of knowledge of the properties of the homogeneous phases comprising it and the problem of analysis of transport properties in an inhomogeneous system. The present work describes the preparation of the homogeneous ternary phase and the corresponding electrical properties of both homogeneous and heterogeneous material. MATERIAL PREPARATION Most specimens for this investigation were prepared by encapsulating the elements in evacuated quartz tubes after which they were melted and homogenized in the liquid state. The ambient temperature was then dropped to 500°C and the resulting ingot zone melted. The growth rate, width of zone, stoichiometry, and number of passes have an effect on the resultant microstructure. Grains several centimeters in length were easily produced by this method. Other solidification techniques were also used, including uniform slow cooling of the entire specimen and rapid freezing. The microstructures of specimens produced by these techniques frequently differed appreciably from similar compositions prepared by zoning. A variety of nonequilibrium microstructures characterized by long needlelike particles resulted from the rapid-freeze method. PHASE EQUILIBRIA The lack of information on phase equilibria is a major difficulty associated with a comprehensive study of the Ag-Sb-Te system. Considerable confusion has resulted from the use of the formula AgSbTe, to identify the cubic ternary intermediate phase even though it has been established that material of this stoichiometry normally contains AgzTe as a second phase.798 In this paper, silver antimony telluride will denote the cubic ternary intermediate phase comprising the major portion of AgSbTe,. The term "single phase" will denote material which consists of only the cubic phase (as evidenced by metallographic examination and X-ray diffraction) and the term heterogeneous will describe multiphase material containing AgzTe, SbzTe3, or other phases in addition to the cubic phase. The single-phase material may actually contain a variety of inhomogeneities—gradual changes in composition on a macroscopic scale, localized fluctuations in composition, clusters or other products of early stages of the precipitation process, and a variety of point and line defects—all of which will not be detected by the present techniques for determining homogeneity. Single-phase material has been prepared from compositions close to 59 mole pct SbzTe3 21 (this notation refers to the location on the Ag,Te-Sb2TeS vertical section). Zone widths of =2 cm and growth rates 51.2 cm per hr were used. The single-phase region at elevated temperatures extends off the vertical section to a composition which can be expressed approximately as Ag,,SbzgTes,.9 The latter two compositions as well as AgSbTe, are represented in the conventional Gibbs triangle in Fig. 1. It is not presently possible to ascribe exact values to the limits of the single-phase region on a given isotherm or vertical section due to the extremely

Jan 1, 1964

By Louis Moyd

The Concrete Research Division, U.S. Corps of Engineers, has developed a simple procedure for determining the coefficients of linear thermal expansion of rocks by means of resistance wire (SR-4) strain gauges. Gauges are cemented to the surfaces of specimens, which are then brought alternately to temperatures of 35°F and 135°F. Results are accurate to the seventh decimal place.

Jan 6, 1950

By H. F. Yancey, O. L. Furse

For several years the Bureau of Mines at its Northwest Experiment Station, in cooperation with the Mines Department. of the University of Washington, has been studying the breakage and degradation of coal. The first phase of the study was devoted to the determination of the friability of many coals of various ranks and comparison of various methods for estimating friability.' A study of the relative ease or difficulty with which various coals are reduced to the fine size required for use as pulverized fuel followed the completion of this work. Baltzer and Hudson2 list twelve research organizations in the United States, two in England, one in Germany and one in Canada that are reported to be engaged on this problem; showing the general appreciation of the need for a simple method of estimating the grindability of different coals. Hardgrove,3 ho has advanced a method for estimating grindability, points out that pulverizer tests of different coals are incomplete and unsatisfactory. He compares such tests to that of a boiler test made without knowledge of the calorific value of the coal. Frisch arid Holder4 also stress the same point. They state that,

Jan 1, 1934

By J. B. Conway

Stress-vuptuve data for several of- the refractory metals are frequently found to yield a linear relationship between the Larson-Miller parameter and the logarithm of the applied stress. In such cases linear stress-rupture isotherms result with slopes bearing a definite relationship to the temperature. It also follows that the stress to produce rupture in a certain period of time will be linear in temperature. Data for several refractory metals have been reviewed and excellent linearity is shown in this type of isochronal plot. In addition, the af ore - mentioned lineavity leads to a linear relation between the log of the stress to produce rupture in a certain time and the homologous temperature. This has been illustrated for the Group VI-A metals, tungsten and molybdenum. EXTENSIVE use has been made of the Larson-Miller' parameter in the interpolation and extrapolation of stress-rupture and creep data. In those cases where this particular parametric approach is applicable a convenient and fairly straightforward procedure is made available for the correlation of experimental stress-rupture data. It is quite common to employ this parameter in the form of a master rupture plot in which the parameter, T(C + log tr), is expressed as a function of log stress. In many cases this functional relationship in log stress is linear within acceptable accuracy and hence the following relation results: where P is the parameter, C is the Larson-Miller constant, T is the absolute temperature, t~ is the rupture time, a is the stress, and a and b are constants. Examples of such a relationship are contained in the work of Green, Smith, and 01son2 dealing with high-temperature rupture behavior of molybdenum and in the work of Green' dealing with the high-temperature behavior of tungsten. In addition, pugh4 has shown a similar linearity for some fairly low-temperature data for molybdenum. It can be shown that when the relationship in Eq. [I] is exhibited certain generalizations can be made concerning the form of the stress-rupture isotherms. For example, rearranging yields: For a given material (constant C) at a given temperature the first term on the right-hand side of Eq. [2] is a constant and hence this equation defines a straight line when log stress is plotted as a function of log-rupture time. This is recognized as the standard form usually employed in this type of data presentation. Such linearity then suggests the linear form of the Larson-Miller parameter. Or, in other words, the linear parametric relationship in Eq. [2] results only when the stress-rupture data are linear on a log-log plot of stress vs rupture time. Another interesting observation can be made in regard to Eq. [2]. It can be noted that the slope of the stress-rupture isotherms is given by - T/b and hence a direct calculation of the constant b is available. It also follows that since the value of b is the same for all temperatures the slopes of the various isotherms on the log-log stress-rupture plot cannot be the same. Indeed, the existence of the relationship in Eq. [2] precludes a system of parallel lines on this common stress-rupture plot. As a matter of fact it further specifies that in addition to being nonparallel the slope of these isotherms must decrease (i.e., become more negative) with increasing temperature. Such a condition is indeed found to exist in the case of the stress-rupture data reported for molybdenum.' As a corollary to the above, it may be stated that stress-rupture data which do not lead to a linear log-log stress-rupture plot or whose isotherms do not exhibit a decrease in slope as the temperature increases will not yield the linear relationship of Eq. [I]. Applying Eq. [2] to two different temperatures and solving for C yields: Eq. [3] affords a simple and rapid method for calculating the Larson-Miller constant from the log-log stress-rupture plot. The slope of a given linear isotherm is measured and the value of "b" calculated based on Eq. [2] as: slope = - -Tb Then at an abscissa value of 1.0 hr (making log tr in Eq. [3] equal to zero) read the stress corresponding to rupture for two different temperatures. Substitution in [3] yields: A value of the Larson-Miller constant can thus be calculated from a few simple mathematical procedures employing data read directly from the log-log plot of the stress-rupture data. Of course, it is not to be overlooked that the above reasoning has been based on the linear relationship of Eq. [I] being applicable. However, if as mentioned above the log-log plot is

Jan 1, 1967

By C. D. Tedmon, D. P. Ferriss

THE yield stress, o of low-carbon steel has been shown to vary with the average grain diameter, d, according to the relation1-3 where o is taken to be the lower yield-point stress Of is the friction stress on an unlocked dislocation, and ky is a constant. The interpretation2,4 of ky in terms of dislocation theory relates this constant to the stress to unlock a source across a grain boundary. cottrel14 predicted that ky would increase with decreasing temperature. This was observed to be the case by Adams and coworkers5 in their investigation of niobium (columbium). However, petch6 and Backofen: both working with low-carbon steel, found ky insensitive to temperature. In his work with high-purity niobium, Johnson' found ky equal to zero. Evansg showed that k, was essentially zero for niobium containing nitrogen in an appreciable concentration range. The present experiments were designed to check this apparent anomaly in the value of ky in another Group V metal. Yield points were determined as a function of grain size at several temperatures for tantalum and a tantalum-tungsten alloy. The material used was double are-melted tantalum and a double are-melted alloy of 90 pct Ta and 10 pct tungsten (by weight), both obtained as unannealed, swaged rod. The impurity content of the materials is given in Table I. The tantalum was annealed at 1325"C. in a vacuum resistance furnace using a tantalum boat. The alloy was similarly annealed at 1660°C. Annealing times varied from 15 min to 2 hr, depending on the desired grain size. Nominal pressure in the furnace was 3 X 10~4 mm of Kg. Metallographic examination showed that the annealing treatment produced grain sizes ranging frorn 0.021 to 0.200 mm in the tantalum, and 0.060 to 0.160 mm in the alloy. Tensile bars were made by centerless grinding the annealed specimen;, and then electropolishing to remove all grinding marks. The specimens were than pulled :it 2 1/2 pct per rnin in an Instron testing machine. The tantalum specimens were tested at 77", 195", and 300°K. The alloy was tested at 300°K only. All specimens exhibited a yield-point phenomenon at all temperatures. Typical load-elongation curves at the three test temperatures are shown in Fig. 1. The lower yield stress is plotted as a function of (grain size) in Figs. 2 and 3 for tantalum and the 90 pct Ta-10 pct W alloy, respectfully. The position and slope of the curves was determined by least-

Jan 1, 1962

By Ancel St. John

AT THE New York meeting of the Institute of Metals Division in February, 1927, Jeffries and Tarasov presented a paper on Tungsten and Thoria,1 in which the experimental facts were interpreted in accordance with the prevailing point of view that the thorium is present as the oxide, thoria. In discussing that paper the writer of this article stated that his own investigations, which had been unavailable to Messrs. Jeffries and Tarasov, showed that the so-called "thoriated" tungsten filament failed to disclose any sign of the oxide when subjected to X-ray diffraction analysis, but did give plenty of evidence of the presence of metallic thorium and, in certain cases, of a material believed to be an alloy of tungsten in thorium. Since these results were completely at variance with the results reported in the paper under discussion and with other papers which had preceded it from time to time in the past, it was felt that further discussion should be withheld until the new evidence could be presented adequately. Arrangements were therefore made to present that evidence at this meeting. MATERIAL EXAMINED The material examined was high-emission filament such as is used in radio tubes, supposed to contain about 0.75 per cent. thoria. The actual analysis was not stated. SCOPE OF THE INVESTIGATION The investigation was undertaken because of a feeling that the thorium present in filamentary material of this type exists as metallic thorium or as an alloy of thorium and tungsten and not as the oxide. Attention was therefore directed to determining: 1. The minimum amount of thoria detectible in a mechanical mixture of thoria powder and finely divided tungsten. 2. The amount of thoria detectible in the filament. 3. The condition of any thorium present in other form than as thoria. 4. The amount of thorium dissolved in the tungsten.

Jan 1, 1928

By George S. Rice

ARIAL maps of prospective mineral-bearing territory have become almost indispensable in all the branches of exploration, and have proved particularly useful in the great oil area of the Southwest. About nine years ago aerial photographic mapping in this area was begun. The early product was lacking in scale accuracy and other control features, which limited its effective use. Since then, the evolution of the technique of such mapping has been steady, with several mapping companies collaborating with five of the leading oil companies, and aerial maps have been prepared covering practically the entire area.Improvements in cameras, film, and developing equipment and practice have resulted in more uniform and clearer photographs, but the outstanding development has been the accuracy obtained with respect to scale and all other control features. Maps are no

Jan 1, 1936

By J. G. Y. Chow, S. B. McRickard

The tensi1e properties of Ferrovac iron have been studied from 4° to 300°K. The stress required for macroscopic yielding was found to he constant below approximately 50°K. The effect of mechanical twinning on this low -temperature stress plateau was investigated. The onset of twinning occurs in this iron between 130° and 150°K and depending on its previous thermal history the twinning-stress curue may drop below or remain above the vield-stress curves as the temperature is lowered. Twinning has been shown to initiate slip in quenclzed iron at low temperatures. In no instances, however, did the onset of twinning alter the continuity of the yield stress -tempwature curve. Our data shows that carbon inhibits twinning and slip at low tem-peratures. This observation nay be used to explain the ductile-to-brittle transition in iron. The effect of fast neutron irradiation on yielding and embrittlement in iron and Fe-C alloys is offered as supporting evidence for this viewpoint. THE mode of yielding in iron at low temperatures was studied in an attempt to find an expression based on a single mechanism to describe the thermal dependence of the yield stress of iron. There are two types of inflections observed in the variation of the yield stress with temperature in iron and Fe-C alloys. The first is associated with ductile behavior and consists of a region extending 50" to 100°K above absolute zero in which the yield stress is independent of temperature. The second is observed in more brittle materials such as Fe-C alloys and irradiated iron and consists of an abrupt discontinuity in the yield curve as the temperature is lowered through a ductile-to-brittle transition point. The temperature dependence of the yield stress for iron with four grain diameters as found in this study is shown in Fig. 1. To varying degrees all the curves appear to flatten or approach an asymptotic value as the temperature is lowered below 50°K. Several other investigators1,2 have observed a plateau in the yield stress of iron and steel at low temperatures and in 1956 Louat3 presented a theory which contained an explanation for this behavior. In a subsequent exchange with Erickson and Low4'5 who attributed the plateau to the onset of mechanical twinning Louat8 showed that twinning first occurs in iron and steel tested in tension at temperatures as high as 140°K which is well above the observed plateau in yield stress. Furthermore he pointed out that both twinning and slip are basically dislocation processes and that with modified parameters his original theory still applied when deformation is initiated by twinning. Variables which affect the ductile-to-brittle transition in iron are test temperature, strain rate, composition and grain size.7 LOW,8 Hahn et al.,9 and Hull10 have provided evidence which links brittle fracture at a given temperature with the specimen grain size and the onset of twinning. In fact, Hull equates the brittle fracture stress to the twinning stress. On the other hand brittle fracture has been observed in the absence of twinning and priestnerl1 has given a fracture criterion which is valid whether or not fracture is preceded by extensive twinning. The data presented here clarify the role of twinning in the low-temperature deformation of iron. Strong evidence is given that the amount and distribution of interstitial impurities such as carbon are of

Jan 1, 1965