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By S. E. Maddigan

MANY experimental and theoretical investigations have been made on the processes involved in annealing and recrystallization of metals. Most of these, however, have treated the time element as constant and heat-treatments used have been for relatively short times. Aside from the early work by Carpenter and Elam,1 the few that have investigated the effect of time on the processes have usually done so for fairly short time periods. During recent years the growing interest in long-time creep properties of metals and alloys under stress has made increasingly important a better knowledge of the recrystallization during prolonged heating. The recrystallization temperature of 70-30 brass given by Clark and White2 in 1932 was somewhat above 400°F. (204°C.) but under 500° (260°C.), whereas in our laboratory recrystallization has been observed in creep specimens at 204°C, the lowest temperature of Clark and White's range. Since the creep properties are quite different above and below the recrystallization temperature, erroneous conclusions can readily be drawn by the application of short-time recrystallization data to creep problems. It was thus considered of both practical and theoretical value to make long-time annealing studies near the minimum recrystallization temperature. In this way useful additions could be made to data on recrystallization temperatures and, since the reactions in this range are relatively slow, additional insight could be obtained into the factors involved in annealing. Several comprehensive reviews of recrystallization processes have been written,3-5 therefore only a brief review of the generally accepted facts will be given here.

Jan 1, 1940

By Robert H. Weber

INCREASING acceptance of perlite products, chiefly in the fields of lightweight structural aggregates and thermal and acoustic insulation, has led to expanding market demands that have encouraged many new producers to enter the field. In some instances, however, the failure of these producers to anticipate the variable response of perlite to conventional processing methods has led to difficulty in establishing an economical flowsheet by which a predictable specification product could be obtained. It is not the writer's intent to provide a solution to these problems, but rather to summarize their nature. It is to be hoped that members of the industry who have hurdled some of these obstacles will document solutions arising from their experience. In this treatment the term perlite will not be restricted to the petrographic definition but will apply to all volcanic glasses. Expansible obsidians and pitchstones are accordingly included in this broader industrial classification. Chemical Properties: Although perlite has been reported to range in composition from that of rhyolite to that of andesite, it is probable that most of the glasses have the composition of rhyolite. When recalculated to an anhydrous basis, the five analyzed glasses from New Mexico, representing five distinct physical types from widely separated deposits, show an amazingly uniform oxide composition. Water content is the only major compositional variable; total water ranges from a low of 0.37 pct (non-expansible obsidian) to a high of 8.95 pct (expansible pitchstone). The wide range in expansion characteristics exhibited by these samples cannot be related to significant variations in the composition of the nonvolatile fraction and has been only partially correlated with variations in water content.

Jan 1, 1956

By John C. McDonald

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

Jan 1, 1941

By John C. McDonald

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

Jan 1, 1941

By 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 10'3. 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.' 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.' 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,4'5 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,' 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'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'0'" it should be possible to test for a relationship between the SFE and textures.

Jan 1, 1970

By Lewis T. Wright

IT is commonly believed by metallurgists that in copper-smelting, the copper in the slags, which is irreducible by continued smelting, is retained in the form of "prills" of matte. I have frequently held well-settled slag in a molten condition for a long period without being able thereby to reduce the copper-content. The slag acted as though it contained a minimum of dissolved or combined copper that could not be settled out by gravity. I have used reagents, but without satisfying myself in what form this copper existed. The same slags, by fine grinding and elutriation, could not be separated into portions containing more or less copper than the average content. By treating copper-slags in an electric furnace an impure button of copper. was produced, but the high temperature and the strong reducing-action of the furnace were influences that suggest an explanation of a result not obtainable with ordinary smelting-temperatures. If all the copper in the slag were in the form of copper-matte, and not existing as a dissolved compound with some of the elements of the slag, then the other metals in the matte, such as gold and silver, should occur in the slag in the same ratio to the copper as to the copper in the accompanying matte. This reasoning led me to study the ratio of metals in the products of smelting, and, apart from the issues discussed in this paper, the research has proved both interesting and illuminative. On the assumption of a similar ratio of metals in matte and slag, if the percentage of copper in the slag accompanying; a matte containing 50 oz. of silver and 1 oz. of gold per ton of copper was 0.3 per cent., or 96 oz. per ton of slag, there should be found 0.15 oz. of silver and 0.003 oz. of gold per ton of slag:; but, in my experience, there is less silver and much

Sep 1, 1909

By R. F. Mehl, J. K. Stanley

THE recrystallization of cold-worked metals is studied ordinarily by determining the temperatures required for complete recrystallization to occur within a given arbitrary time period, usually within 15 min. to 2 hr. The results obtained are conventionally assembled in a three-dimensional diagram relating this temperature to the amount of cold-work (percentage deformation) and the resultant grain size, though sometimes other modes of representation are employed.1 Such three-dimensional diagrams are not complete, for the number of variables exceeds the number represented. The process of recrystallization is characterized by a time-rate, a fact that is not portrayed upon ordinary recrystallization diagrams. It is known that recrystallization consists in the formation of new nuclei and the growth of these nuclei, a process that continues until the matrix is completely consumed and the original set of grains entirely replaced by the new. This knowledge is old.2 Truly heterogeneous reactions invariably proceed by nucleation and growth; the decomposition of eutectoid solid solutions provides an example about which much is known,3 and freezing, originally studied by Tammann, provides the classic example. Although recrystallization is not a heterogeneous reaction .within the orthodox meaning of the term, the mechanism of the process is the same. As in eutectoid inversion and freezing, it should be possible to study the rate of isothermal recrystallization as a function of time, and it should also be possible to analyze the isothermal reaction curve into the component rates of nucleation and growth that determine them.* Other methods, not employing the rates of nucleation and growth, have been used to represent the rates of such reactions, but these in general have been artificial and have not led to progress.4,5? The theory of recrystallization is not in advanced state; if recrystallization data were obtained, in terms of the rate of isothermal recrystallization, and in terms of the rate of nucleation and the rate of growth of recrystallized grains, and in particular if the temperature coefficients of these rates were measured accurately, an adequate theory should be more readily developed.27 Such an effort requires proper experimental technique, but especially requires suitable methods of mathematical analysis to convert measurements made upon a surface of polish into values for the rate of nucleation and the rate of growth and to combine these into a rate of isothermal recrystallization. These methods are now

Jan 1, 1942

By Casimir Constable

DURING the years 1875 to 1879 I had charge of the Rockwood furnaces and mines, situated forty miles from the nearest railway communication at that time, and one hundred miles north of Chap tanooga, Tenn., by the Tennessee River. The small furnace with old-fashioned stoves, then in blast, was built under great difficulties by General Wilder. The early conditions were somewhat as follows: The ore was fossil ore of the Clinton group ; very fine and generally wet, without other admixture. The coke had a large amount of ash, and the fur" nace appeared to be badly scaffolded at times. On many days only a few tons of iron could be obtained. The founder generally id creased the revolutions of the engine when signs of chilling appeared,. The cinder at such times was black, very scoriatious, often closely resembling mill cinder. When the pressure was increased (the joints being the old-fashioned rust joints), leaks in the blast-pipe occurred It was noted that when the blast was stopped, and the leak bolt imperfectly remedied, the furnace improved a little. This set me thinking on the right track; and I took the responsibility of be coming my own founder for a time. A scaffolded condition had existed, and the situation was a trying one. Strange to say the negroes proved excellent furnace-men. Conceiving the hearth of the furnace to be similar to the grate area of a steam-boiler, capable of disposing of but so much fuel per hour, and requiring only a corresponding amount of air, it follows that an excess of air will burn the fuel not yet arrived at the hearth!, and raise the melting-point far above the tuyeres. This might pro duce scaffolding or at any rate choke the boshes, and leave less fuel to be consumed in the hearth. Thus for the time being less ail;. would be needed, as the continued burning of fuel in and above the boshes, would only aggravate the trouble. This condition of affairs accounted for the black cinder; the heat above having melted ore not yet perfectly reduced. This view decided me to reduce the revolutions of the engine; thefurnace finally became gray, as might have been expected. Any attempt to increase the speed produced black cinder and hard iron ;

Jan 1, 1883

By Ivan Simon, R. K. McConnell

Anticipating the availability of tiltmeters suitable for use in boreholes, this article proposes a method of using one or more of these meters to determine in situ stress distribution before and after mining operations. Several ways of using relief techniques to measure in situ stresses in rocks have been developed. These techniques, summarized by Merrill,1 involve measuring deformations which take place when a specimen of rock is wholly or partially isolated from the stress field in the surrounding rock. Measurements of rock deformation caused by stress relief from mining operations can, in principle, also be used to estimate in situ stress distributions. Müller2 has mentioned experiments being carried on in Austria with a "deformation indicator" to determine the tilting of holes drilled before a mine opening is made. Similar work using borehole extensometers has been reported by Potts? and Duvall4 has called attention to the possible use of tiltmeters in making these measurements. Considerable attention is now being paid to the use of tiltmeters in detecting rock deformation associated with fault movements, earthquakes, earth tides, etc. The instruments used for these measurements have usually been of the mercury tube, water tube, or quartz fiber type, but because of their large size, and/or fragile nature, such instruments would not be suitable for use in mining stress measurements. Recent instrumentation developments, however, give promise that rugged, sensitive tiltmeters small enough for use in boreholes may soon be available.' In anticipation of these developments, this article presents a number of calculations of the possibility of using one or more tiltmeters emplaced in a drill hole prior to mining operations to determine the in situ stress distribution both before and after a mining operation. Consider point p (x, z) near a tunnel of radius a

Jan 1, 1969

By NATHANIEI HERZ

(Cleveland Meeting, October, 1912.) THE formula very frequently used for computing the economical size of pipe to transmit compressed air is that of D'Arcy, as follows: d5(p1-p2)/w1l D-c w11 Where, D = the volume of compressed air delivered in cubic feet per minute,-at the final pressure. c = an experimental coefficient determined for the various sizes of pipe. d = the diameter of the pipe in inches. 1 = the length of the pipe in feet. P1 = the initial gauge-pressure in pounds per square inch. p2= the final gauge-pressure in pounds per square inch. W1 = the density of the air, or the weight in pounds per cubic foot at the initial pressure, p,. The most common case is that in which the given quantities are: the quantity of air required, the length of the pipe, and the initial pressure. The method of solution is to assume a pressure-loss and to compute the remaining factor, c/d5, thus giving the size of pipe corresponding to the assumed loss of pressure. It is always desirable to try two or more pressure-drops, in order to find the combination that is most satisfactory, since often a small change in the size of pipe will reduce or increase the loss of pressure several pounds. An alternative method is to assume a size of pipe and calculate the corresponding pressure-drop. Each method involves a series of tedious calculations to arrive at the most economical solution, and also requires the use of tables giving the constant, c, the actual diameters corresponding to the nominal pipe-sizes, the density of the air, w1, and often, for convenience, a table giving the

Dec 1, 1912

By A. K. Schellinger, R. D. Lalkaka

IF the ball mill is considered only from an energy standpoint, it can be thought of as a converter of kinetic energy into heat energy and surface energy. The law of the conservation of energy must apply to the ball mill as it does to any machine or process in nature. The heat energy output of the ball mill is apparent to any casual observer of the operating mill since the outflow pulp will be appreciably warmer than the inflow water and rock. The rock in the ball mill is crushed by shearing of its ionic bonding caused by some impact-induced stresses beyond the elastic limit. As the bonds holding the mineral crystal lattices together are ruptured, new surface area is created on each unit of which a definite number of unsaturated bonds exist. Such unsaturated energy of bonding may be termed the "surface energy," and is a potential energy figure. This created energy was withdrawn from the ball mill system and represents an absorption, or disappearance of heat. To reduce the size of the rock, surface area must be created and with it the at- tendant characteristic surface energies of the minerals concerned. Thus the creation of surface energy, from an energy viewpoint, is the creation of useful work by the ball mill. Because of the controversial nature of the energy efficiency figures for modern operating ball mills, it seemed worthwhile to approximate the ordinary magnitude of such efficiencies from the above viewpoint. This was done by an energy balance of the three aforementioned forms of energy, kinetic, heat, and surface energy, for two 9Y2x10-ft grate-type ball mills grinding cement raw materials. Kinetic energy input to the balls was approximated as closely as possible while the heat energy output was measured by means of a thermometer and water and rock flow rates. The assumption was made

Jan 1, 1952

By C. Chu

A theoretical investigation has been made of the forward combustion process using a one-dimensional linear mathematical model, taking into consideration the effect of the vaporization-condensation which occurs on the leading edge of the heat wave. This work involves the solution of five coupled partial differential equations. Besides the vaporization-condensation phenomenon, these equations account for conduction, convection, combustion, heat loss, diffusion and bulk fluid flow. For the one-dimensional linear model studied, the vaporization-condensation phenomenon does not induce appreciable change in the temperature at the combustion front; and its primary effect is to create a steam plateau and to increase the length of the heated zone ahead of the combustion front. This effect becomes more pronounced at lower pressures, higher porosities or reduced gas saturations. The peak temperature and the temperature profile on the leading edge of the heat wave stabilize after a certain period. The length of the steam bank remains practically constant, although the length of the water bank increases as the heat wave advances. INTRODUCTION The existence of the vaporization-condensation phenomenon in the heat-wave process and the important role played by the phenomenon have been recognized by several investigators. Kuhn and Kochl stated that steam plateaus were frequently observed on the temperature records of their experiments. The steam plateaus were attributed primarily to the vaporization and subsequent condensation of the interstitial water existing in the oil sand. Szasz2 suggested that both lighter hydrocarbons and water are vaporized on the leading edge of the heat wave, carried forward in the gas stream, and then condensed to create banks of oil and water. Martin et al suggested that the vaporization-condensation phenomenon is one of the main mechanisms of the heat-wave process, along with thermal expansion and viscosity reduction. Wilson et al. reported the existence of a steam plateau several inches in length in their small-scale tube-run experiments. However, this important phenomenon has never been taken into consideration in the numerous theoretical analyses by various authors. 5 The purpose of this work was to study the thermal aspects of a linear heat wave, taking into consideration the vaporization-condensation on the leading edge of the wave, to determine the effect of this phenomenon on the temperature profile of the reservoir, and to investigate how this effect varies when other process variables are changed. THEORY We consider a reservoir of porous medium of cross-sectional area A, extending from x = 0 to x = L. This reservoir contains, aside from the solid matrix itself, a gas phase and a "combined liquid phase" which is a combination of two immiscible liquid phases — namely, an oil phase and a water phase. The oil present in the reservoir is assumed to consist of three fractions, a noncondensable gas, a nondistillable residuum, and a vaporizable oil fraction which may be present in both the gas phase and liquid phase. Before the heat-wave process begins, preheating has taken place and has imparted an initial temperature distribution T,(x) to the reservoir. At the start of the process, a stream of oxygen-bearing gas is introduced through the face at x = 0. This gas supports the combustion of the residual fuel and supplies the heat throughout the process. In order to develop a tractable system of equations, the model properties are postulated as follows: (1) the system is isotropic and homogeneous; (2) there is a uniform fuel content throughout the reservoir; (3) combustion takes place in a moving vertical planar region of infinitesimal thickness; (4) the temperatures of the fluids and the solid matrix are identical; (5) radiation is negligible; (6) the gas and liquid saturations are uniform throughout the reservoir and remain unchanged

Jan 1, 1965

By J. Howard Boyce

INTRODUCTION The Tsumeb Mine is situated in the northern part of South West Africa, approximately 335 air miles north-east of the port of Walvis Bay on the Atlantic Coast, and 240 air miles north of Windhoek, the capital of South west Africa. The mine came into operation in the early 1900's and has operated continuously since then except during the two world warm and the depression years of the thirties, Tsumeb Corporation purchased the property in 1947, installed a new plat, and ham built a modern tom. In addition to the concentrator which began operations in 1948, a copper smelter was started in 1962 and a lead smelter in 1963, Tonnage of ore treated in the concentrator has varied through the years, reaching a maximum of 70,000 tons per month with a current mined tonnage of approximately 50,000 tons per month. Copper concentrates, lead concentrates and zinc concentrates are produced, and for a number of years the production of a germanium enriched concentrate was an important feature of the operation, Both copper and lead concentrates are smelted in Tsumeb, while the zinc concentrates are shipped overseas. Ore change, and the installation of the smelters in Tsumeb have necessitated modifications in the concentrator operation. This paper will describe current plant practice in some detail and will touch briefly on the techniques used from 1954 to

Jan 1, 1970

By H. H. Klepfer, M. E. Snyder

UNTIL very recently, the commercial availability of the rare earths as metals has been very limited. Fabrication of mill products from these metals has not been studied in most cases. This note reports the results of the development of fabrication techniques for thulium. Thulium has a melting point of about 1550°C and a hexagonal close-packed crystal structure. It oxidizes in air to give a black oxide (TmzO,). The procedures for producing thin thulium foil were developed on one ingot weighing about 220 g and were subsequently applied in processing about a pound of metal to foil. Several alternates for the various fabrication steps were investigated and will be discussed. The metal fabricated was in the form of commercial chill-cast ingots 1 in. in diam and 2 in. long weighing approximately 220 g. Impurities in the ingots were reported by the vendor to be 4000 ppni tantalum, 2000 ppm calcium, 200 ppm nickel, 100 to 200 ppm iron, 100 ppm europium, and less than 100 ppm copper, lutetium, and ytterbium. In addition to these impurities, several salt-like inclusions as large as l/8 in. in diam were revealed along the center line of the one ingot sectioned. Preliminary tests indicated that small wafers cut from the as-cast ingot would not fabricate readily by rolling. Forging of copper-jacketed wafers was therefore attempted. At 1550"F forging was satisfactory but an apparent reaction of copper with thulium demanded investigation of lower temperatures. Therefore, the remainder of the test ingot was forged at 1450°F—with only minor cracking. All ingots forged were inserted into copper tubes of 1 in. 1D and 0.125-in. wall thickness. The jackets were sealed by flattening the ends of the tubes and welding under helium. Heating time at 1450°F was 30 min. Press forgings of 1/8 in. per pass were used, followed by 10 min reheats. When the ingots had been squared and reduced to 0.250 in. in thickness, the original copper jacket was stripped off and replaced by a new jacket in preparation for hot rolling. Hot rolling at 1450" F without edge cracking was readily accomplished after forging. Excellent results were obtained with 10 pct reductions of thickness followed by 5 to 10 min reheats. After reduction of thickness from 0.250 to 0.100 in. the copper jacket was removed. It was found, in fact, that hot rolling in air was possible. A tenacious black oxide similar to that seen on zirconium was formed during 3 min reheats at 1450°F. Reduction in air to 0.010 in. foil was possible taking 10 pct reductions per pass. The oxide coat formed during hot rolling in air could best be removed by sand blasting and pickling. Common pickling solutions containing polar solvents were found to attack the metal too rapidly and a concentrated nitric-hydrofluoric acid mixture attacked neither the oxide nor the metal. The most satisfactory pickling solution was 52 vol pct concentrated nitric acid-48 vol pct glacial acetic acid. After forging to 0.250 in., vacuum annealing and cold rolling was found to be another satisfactory alternate to hot rolling in copper jackets. After forging. a hardness of Rockwell B76 was found. Annealing in vacuum (2 X l0-5 mm of Hg) for 1 hr at 1200"F did not alter this value. Annealing at 1470"F for 1 hr brought the hardness down to R;]63. With cold rolling (5 pct per pass) the hardness returned to about R,1:76 after 20 pct reduction and edge cracking became noticeable. However, cold rolling to a total of 40 pct reduction in thickness (RI,,83) was possible before edge crack propagation became serious. Good surface finish was obtained, and the metal loss due to oxidation was minimized by cold rolling and vacuum annealing. Using this procedure the yield of 1.25 in. wide by 0.010 in. thick foil from a 1-in. diam ingot was about 40 pct.

Jan 1, 1961

By T. Vasilos, J. T. Smith

THE mechanism of pressure sintering, or hot pressing, for ceramic materials, has been investigated by several researchers.1-8 Plastic flow has been suggested as the rate-determining mech-anism1,2 while grain boundary sliding3,4 and fragmentation processess have been found controlling in other studies. Vasilos and Spriggs5,6 have reported that pressure sintering occurs by a diffusion-controlled mechanism. For the pressure sintering of metals, investigations with lead7 and with tin6 have not identified the operative mechanism during consolidation of these powders. This note reports the results of a pressure sintering study initiated to determine the mechanism controlling the densification of spherical copper powder. Temperatures of 300°, 400°, 500°, and 600°C at 2500, 5000, 7500, and 10,000 psi pressures were investigated. The copper powder for this study was obtained from Metals Disintegrating Co., Elizabeth, N.J. The minimum purity was reported to be 99.9 pct. The powder size was -325 mesh and a lineal analysis showed the average size to be less than 1 p. An alumina die body and punches were employed. Graphite spacers were placed between the copper powder and the punches before pressing. It was expected that the graphite would form carbon monoxide with any entrapped air and form a reducing atmosphere within the die cavity. This condition was generally realized during pressing although a minor amount of oxidation occurred at 500" and 600°C. The oxide particles were located randomly in the pressed samples and were not considered to influence the densification process. Calibration tests showed the temperature of the copper pellet to be about 20°C less than the die wall temperature, probably resulting from heat losses through the punches. This difference was compensated during the experimental pressing operations. The hot pressing equipment employed for this work has been described by Spriggs et a1.9 and was calibrated with a Baldwin-Lima-Hamilton load cell. Travel of the punches was monitored with a dial indicator showing increments of travel to 0.0005 in. Relative density was calculated at selected time intervals for a known copper weight, punch travel, and die diameter. The accuracy of this calculation was *1 pct. Average grain size after hot pressing was obtained by lineal analysis. Typical densification curves are presented in Fig. 1 and Fig. 2 where relative density is plotted vs log time as a function of applied pressure for the 300" and 600°C pressure sintering temperatures, respectively. The curves for 400" and 500°C were similar to those at 300°C and consequently are not shown. The curves at 300°C as well as 400" and 500°C do not show an end-point or limiting density for a particular applied pressure. At 600°C, a density in excess of 95 pct of theoretical has been reached such that further densification is extremely slow for the 5000, 7500, and 10,000 psi pressures. It is suggested that further densification at these pressure levels may be retarded or prevented by discontinuous grain growth, by entrapped gases, and by other microstructural limitations as described by Cob1e.10 The curve for 2500 psi hot pressing pressure is a straight line over the time interval although a slight change in slope may be occurring at the last time intervals. The plastic flow models,1,2 derived for hot pressing, predict the existence of an end-point (or limiting) density dependent on the yield point of the material at the temperature of interest. The yield stress of copper at a 0.005 strain level has been

Jan 1, 1965

By J. T. Norton, H. Blumenthal, S. J. Sindeband

The interstitial phases formed by the transition elements with carbon, nitrogen and boron constitute a unique class of substances which are of considerable technical interest because of their well developed metallic properties and their high hardness and melting points. They are also of interest from the point of view of structure. It was pointed out by Hagg1 some years ago that the principal factor determining these structures was the relative sizes of metal and metalloid atoms. He predicted that if the ratio of the radii of metalloid to metal atoms was less than 0.59, the metal atoms would be arranged in a close-packed fashion of relatively simple type. This prediction has been amply confirmed. It appears, however, that this specification applies most generally to those structures in which the metalloid atoms occupy isolated positions in the lattice and there is no tendency for strong binding between the metalloid atoms themselves. The series of borides of the type MeB2 formed from the transition elements of the fourth (Ti, Zr) and fifth (V, Cb, Ta) groups of the periodic table provide an opportunity to investigate this situation further. If one takes as a basis the radius of 0.87 A for the boron radius and the Goldschmidt values for the metal atoms in 12 coordination, then the radius ratio varies from 0.54 for zirconium to 0.64 for vanadium, which latter is considerably greater than Hagg's limit of 0.59. It was of interest, therefore, to see if these five elements would form borides of the MeB2 type and have simple isomorphous structures. When this investigation was initiated, relatively little information had been published on the structure of this group of borides. McKenna2 reported the preparation of ZrB2 by a carbon reduction process. Its structure was hexagonal and the approximate lattice constants were given as a = 3.15 A, c = 3.53 A. Ehrlich3 reported the structure of TiB2 as being of the C 32 type with a = 3.02, c = 3.21 and c/a = 1.06 A. Recently, Kiessling4 published the results on ZrB2, showing it to be one in which the metal atoms are arranged in a simple hexagonal lattice with the boron atoms in flat sheets, midway between the layers of metal atoms. The structure is C 32 type with a = 3.169, c = 3.530 and an axial ratio =1.11 A. He also states that CbB2 and TaB2 are isomorphous with ZrB2. Preparation of Borides The borides of titanium, zirconium, columbium and tantalum were made by the electrolysis of fused salt baths after the method described by Andrieux.5 The bath, totalling about 6500 g in each case had the following general composition: Metal Oxide + B2O3 + CaO + CaF2. The actual proportions of the ingredients were determined for each individual case. Although Andrieux reports the preparation of vanadium boride by the same electrolytic method, several attempts proved unsuccessful. However, it was possible to prepare VB2 by the carbon reduction method used by McKenna to produce ZrB2. The mixture consisted of V2O5 + 6B2O3 + 11C and the reduction was carried out in an induction heated graphite crucible. This method proved satisfactory for ZrB2 and TiB2 and undoubtedly the others could be made in the same way. The borides, which were all in the form of fine gray metallic crystals from the electrolytic bath or gray powders from the reduction process, were carefully separated from other constituents and analyzed chemically for metal and boron content. The densities of the boride powders were measured using a standard 10 cc pyenometer at 18°C and ethyl benzene proved to be the most satisfactory liquid for this purpose. X Ray Technique The boride crystals, as prepared, were too small for single crystal examination so that powder techniques were employed. Patterns of the finely ground borides were prepared, using the Norelco recording X ray spectrometer. The lines on these patterns were indexed with the aid of Hull-Davy charts and the approximate dimensions

Jan 1, 1950

By Walter S. Weeks

CONFUSION appears to exist in the discussions of fan testing because engineers do not agree on what energy should be credited to the fan in certain cases, and because certain terms that are used in the discussions seem to have double meanings. The purpose of this paper, therefore, is to discuss the useful energy that should be credited to the fan and the methods of determining this energy, and to suggest changes in nomenclature for the sake of clearness. The instruments commonly used in the measurement of fan pressures are the manometer, the static tube, and the impact tube. The static tube is a tube with small pinholes in it. When connected to one leg of the manometer and placed in the air current with the holes facing at right angles to the direction of the current, this tube causes the manometer to register the static pressure, unaffected by the impact of the air. The impact tube is a tube with an opening that faces the air current. When connected to one leg of the manometer, this tube causes the manometer to register a pressure which is the static pressure modified by the impact of the flowing' air on the end of the tube. If the static tube is connected to one leg of the manometer and the impact tube to the other leg, and both instruments are inserted close together in the air current, the static pressure is eliminated and the manometer registers the impact pressure. The efficiency of a fan is the percentage of the expended power utilized in useful work. The items to be included as useful work are a matter of convention, and as the conventions are not universal I feel that the matter is open to discussion.

Jan 1, 1929

By Paul Tyler

STRATEGICALLY situated in almost the heart of the leading fertilizer-consuming area of the United States, Tennessee long has ranked second only to Florida as a phosphate-producing state. Since 1932 its share of the national output of phosphate rock has increased steadily, and in 1937 its production mounted to an all-time record. More significant even than the increase in tonnage are the forward strides in technology. The Tennessee Valley Authority's research program has led to quasicommer-cial operations using hydroelectric power to manufacture concentrated phosphatic fertilizer that is used to further the farmer education program designed to streamline the fertilizer business and halt the appalling waste of farm land by soil erosion. Even more stimulating to chemically minded imaginations is the production of elemental phosphorus by a private company that not only has succeeded in extracting it from the phosphate rock in electric furnaces but actually has contrived to capture it and to transport it safely in tank cars. New values have been created for low-grade phosphate deposits, and the economic life of reserves has been lengthened while the waste of former years goes back into the mills for recovery of its values by modernized methods. Tennesse's phosphate-mining industry dates from the discovery of blue rock in Lewis County in December 1893. Its known reserves are of the order of 101,500,000 tons, which compares with the production of 825,099 tons in 1937; that is, 21 per cent of the phosphate-rock output of the whole nation. The total output reported from 1894 until July 1, 1938, was approximately 19,000,000 tons. Official estimates of reserves are overly conservative and evidence submitted before a joint Con-gressional committee in November 1938 places "probable" reserves at more than 6,000,000,000 tons.

Jan 1, 1939

By J. B. Cohen, B. W. Howlett, M. B. Bever

The partial molar heats of solution at infinite dilution in tin of aluminum at 300° and 350°C and of gallium, indium, and thallium at 240°, 300°, and 350°C have been measured by tin solution calori-metry. Aluminum, gallium, and thallium are endo-thermic on solution; indium is exothermic. Any temperature dependence of the heats of solution lies within the experimental scatter. Over the dilute ranges investigated, only aluminum has a measurable change in its heat of solution with composition. HEATS of solution of one element in another reflect the interaction between them. The investigation of partial molar heats of solution in dilute alloys is of particular interest as the properties of the solvent are altered to only a limited extent by the presence of the solute and also as the interaction between solute atoms is small. When the heats of solution of a related series of elements in a solvent are known, a systematic comparison may be made. In the investigation reported here, the partial molar heats of solution of the Group III elements aluminum, gallium, indium, and thallium in dilute solution in tin were measured. This work follows an investigation of the heats of solution in tin of the Group IB elements.' EXPERIMENTAL PROCEDURES Materials. Samples of gallium, indium, and thallium were obtained from Johnson, Mathey and Co., Ltd. Indium and thallium were supplied as wire, 1.6 mm in diam; gallium was in the form of irregular pieces. The supplier reported the following minimum purities: gallium—99.95 pct; indium—99.99 pct; thallium—99.99 pct. The aluminum, obtained from Alcoa Research Laboratories, was reported to be 99.995 pct pure. The tin was supplied by Baker and Co., Inc.; the reported analysis indicated a tin content of at least 99.96 pct with lead as principal impurity. Calorimeter. this description will cover only the essential features of the calorimeter with special attention to modifications made since an earlier description was published.' A Dewar flask containing the tin bath was held in a constant-temperature bath of a near-eutectic mixture of lithium, sodium, and potassium nitrates. This bath, which was stirred vigorously, was heated by a primary resistance winding in the container wall and by a secondary winding immersed in the salt. The voltage supplied to both windings was stabilized. The temperature of the salt bath was controlled by means of a platinum resistance thermometer in one arm of a Wheatstone bridge. The light from a mirror galvanometer in the bridge circuit fell on a photocell which controlled the current in a saturable reactor in series with the secondary winding. In this manner, the temperature of the salt bath was controlled to ±0.003°C and that of the tin bath to at least ±0.002°C. Each of these temperatures was measured by two iron-constantan thermocouples in series, coiled in a helix to minimize heat loss and immersed in the salt and tin baths in protective sheaths. The temperature of the laboratory was kept constant to ± 1°C during a run. Specimens were dropped into the tin bath from an addition arm held at O°C which was part of the cal-orimetric system. The system was evacuated to about 0.02 1 to minimize oxidation and to reduce transfer of heat. The bath was stirred by a glass stirrer introduced through a double Wilson seal. The samples were scraped clean before weighing, which was carried out as rapidly as possible. Each sample was immediately placed in the evacuated addition arm to minimize contamination. These precautions were especially necessary with aluminum. After the runs with gallium and thallium at all temperatures and with indium at 240° and 350°C (Series I) were completed and before the runs with indium at 300°C and aluminum at 300° and 350°C (Series 11) were begun the following changes were made. The shape of the Dewar flask was changed so as to result in a lower surface to volume ratio of the bath and at the same time the amount of tin was reduced from 500 to 400 g. The paddle type stirrer was replaced by a helical screw and the rate of stirring was increased to about 150 to 200 rpm.

Jan 1, 1962

By George S. Rice

GROUND movement and subsidence is an important matter from several points of view and it is regrettable that more papers have not been written on this subject in the past year. Damage may be done to surface buildings or to the higher workings of a mine, and a study of the subject gives valuable in- formation on hanging-wall or roof control. The latter objective is strikingly shown in a recent paper presented by Jack Spaulding on Oct. 21, 1937, before the Institution of Mining and Metallurgy, of Great Britain, entitled "Theory and Practice of Ground Control in the Kolar Gold Field, India." All may not agree with some of his theories that were deduced from studies of the many violent rock bursts at depths of 5000 to 7000 ft., but the data obtained are of great value. His theories of symmetrical ring stresses and symmetrical domes which are pictured as perfect are rather hard to understand as such uniformity is un- likely in view of the irregularities in the formation due to folds and fractures of various kinds. All will agree in principle with this idea of domal effects, which have been observed in many countries, but they are generally irregular.

Jan 1, 1938