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By A. C. Losekamp, R. M. Fincel, J. B. Conway

TANTALUM like several other metals exhibits a great affinity for or reactivity with certain gases. Tested in atmospheres which are not completely pure this metal becomes contaminated by certain impurities (notably nitrogen, oxygen, and hydrogen) with a resultant change in various properties. Well-known are the drastic changes in hardness, ductility, and electrical resistivity. Also previously recorded are the distortions of the lattice1,2 accompanying the increased content of oxygen and nitrogen in tantalum. This pronounced affinity for certain gases along with the significant property variations thereby produced makes it necessary to observe additional experimental precautions in making various property determinations with tantalum. Some recent measurements of the linear thermal-expansion characteristics of tantalum have made this point quite emphatically. Failure to observe the greatest precautions in reducing the contaminating influence has led to some extremely distorted results. Not only does such operation lead to different heating and cooling curves during the thermal-expansion measurements, but upon cooling to room temperature the sample is found to have suffered a permanent (actually semipermanent since the specimen can be returned to its original length by a 3-hr degassing treatment in vacuum at 2300°C) elongation. In addition, subsequent heatings will not follow the initial heating curve unless the expansion measurements are based on the actual specimen length at the beginning of the heating cycle. These thermal-expansion measurements were made by positioning the specimen horizontally at the longitudinal midpoint of a 20-in.-long, 4-in.-diam resistively heated tungsten tube furnace. The specimens were in the form of 20-mil sheet formed into a sharp U-shape about 0.3 in. in width and 0.3 in. in depth. Fiducial marks in the form of 0.010-in. holes drilled at either end of the 2.5-in.-long sheet specimens were viewed by a paired filar micrometer telescope system mounted on an Invar bar on the top of the furnace. Tests were made in helium with temperatures measured by a Pt/Pt-lORh thermocouple to 1000°C; above 1000°C temperature was measured by means of an optical pyrometer sighted into a black-body hole drilled into the specimen-holding fixture in the vicinity of the specimen. Previous tests with black-body holes drilled in a 0.25-in.-diam rod specimen had confirmed the temperature uniformity between specimens and specimen-holding fixture in this furnace. A typical thermal-expansion curve for arc-cast tantalum in helium is shown in Fig. 1 for the case where no attempt is made to remove all the impurities from the cover-gas atmosphere. The initial heating curve appears smooth and has a shape characteristic of all metals. However, it is known that the sample begins absorbing impurities at temperatures above 1000°C which are sufficient to distort the lattice and lead to specimen lengths which are somewhat larger than would be obtained in the absence of contamination. During the cooling cycle the expansion curve is seen to be significantly different from the heating curve. This is due to the impurity content causing a semipermanent (i.e., permanent until the impurities are removed by vacuum degassing) deformation which will not allow the speci-

Jan 1, 1965

By Pol Duwez, H. E. Martens

The high temperatures encountered in the operation of jet engines have imposed most drastic requirements upon the materials used in their construction. There are two different approaches to the materials problem connected with the design of parts in contact with high temperature gases. The first approach is to use a material which will perform satisfactorily at a temperature comparable to that of the gas. The second approach is to use a cooling system so that the material is maintained at a temperature appreciably lower than that of the gas. Besides the conventional method of cooling by means of a liquid in contact with the material exposed to a high rate of heat transfer, a less orthodox method consists of making the part to bc cooled of a porous material', so that the cooling fluid can be forced through the pores, In this scheme, the temperature of the coolant moving in a direction opposite to that of the heat flow increases gradually while passing through the porous material, and the coolant forms a protective layer on the surface exposed to heat, This method, referred to as ((sweat cooling," was pro- posed at the Jet Propulsion Laboratory in September 1944, and the experimental work on the preparation of porous metals was started early in 1945. The sweat cooling method opens new lines of research in powder metallurgy by extending the field of application of porous metals. The porous metals available at the present time are used mostly as bearings or filters, and a rather limited number of alloys are made for these applications. In addition, the fabrication of bearings or filters does not require a very close control of the permeability, while in the case of sweat cooling such a control is of primary importance. In designing a sweat cooled part it is imperative to assure a given rate of flow of coolant under certain conditions of Pressure drop. Generally, the Proper pressure drop and the rate of flow of coolant are deduced from heat transfer and design considerations, and consequelltl~ the Permeability of the Porous metal to be used is also determined. It is therefore necessary for the designer to have available a continuous series of porous metals covering a range of permeability as wide as possible. Contrary to the requirements established in the fabrication of filters, the actual pore size of a porous metal intended for sweat cooling is of little consequence, except for its effect on permeability. The tensile strength is likely to be of great importance for some applications. Since the tensile strength of a porous alloy decreases with increasing porosity, an important problem is to develop porous alloys having the maximum permeability with minimum porosity.

Jan 1, 1949

By H. Bloom, H. E. Hawkes

STREAMS and rivers are the principal channels into which the weathering products of rocks and their contained ores are funneled. The inorganic load of a stream system is a crude sample of all the earth materials in the drainage basin of the stream, and the heavy mineral assemblage of sediments is one of the oldest and most successful guides to certain kinds of bedrock ore in unexplored terrain. Early application of this method was made possible by the ease of separation and identification of heavy minerals in the field with the simplest equipment. Water analysis for traces of base metals became a practical possibility about eight years ago with the development of rapid chemical tests that could be carried out at the field site.' , Since that time the water method has been widely used in mineral reconnaissance, and a substantial number of discoveries have been reported. Here again, the techniques developed for this work were relatively simple and could be performed easily at the field site. Sediment analysis by chemical methods, as distinguished from mineralogical, has received less at- tention. Some experimental work was done by Lovering and others," but to the authors' knowledge, chemical analysis of sediment samples has not been used in routine exploration programs until very recently. In spite of the obvious promise of this method, it was not pursued vigorously because of the lack of a simple and portable chemical test that could be used conveniently at the field site or in a field camp. Procedures that had been developed for trace analysis of soils all called for a rigorous chemical attack with hot acids—tests more conveniently applied in processing large volumes of routine soil samples at an established field headquarters. Recently an extremely rapid and simple test was developed by Bloom.4,5 The extractant used in this procedure is a cold solution of ammonium citrate. Elements measured are the heavy metals, principally zinc, lead, and copper. This method differs from the established procedures for soil analysis in that it measures only a small fraction, about 5 pct, of the total metal content of the sample. It has been found, however, that the significant pattern of metals in the sediments of streams below a base-metal deposit can be brought out as well and sometimes better by this simple cold-extraction procedure than by the more tedious methods requiring hot acids. To understand fully the significance of the relation between the readily extractable and the total

Jan 1, 1957

G. K. BURGESS, ? Washington, D. C.-At the Bureau of Standards it was decided, in order to study the high-aluminum end of these curves, that efforts should be made to prepare pure aluminum, and the promise of getting aluminum, practically free from the two elements that have such great effect in very small quantities, namely, silicon and iron, and which

Jan 12, 1919

By J. A. SINGMASTERN

THE New Jersey Zinc Co.'s vertical retort plants are believed to have been in continuous operation through the whole year. At Palmerton metal purer than that made from the same ore in the old plant has been produced and has been able to compete successfully with very pure electrolytic metal in die castings and other special uses where extreme purity is worth money. A new plant using this process was put in production by the Grasselli Chemical Co. at Meadowbrook, W. Va., early in the summer. It is said to be working very satisfactorily. It is understood that this plant will not produce high-grade metal. Two patents issued to Bunce and Mahler (Nos. 1,749,126 and 1,749,127) describe a method of operating the vertical retort so that practically lead-free metal can be obtained from ores containing consider- able lead. The zinc vapors and other gases leaving the reaction zone are filtered through a column of material maintained at a temperature high enough to prevent much zinc from condensing. The filtering medium is either periodically or continuously changed.

Jan 1, 1931

By T. E. Harper, Gustave Reinberg

Electrolytic refining of all lead bullion produced at the Oroya smelter of the Cerro de Pasco Copper Corporation has been adopted as standard practice. A pilot refinery with a capacity of 25 metric tons daily has been in operation since June, 1934, and a new refining unit having an initial capacity of 100 tons per day is under construction. This program has been made possible by certain modifications of the usual Betts refining process1, developed at Oroya, which have the effect of making the purity of the lead produced, and the acid loss incurred in operating the process, entirely independent of the amount of impurities in the original bullion. The modified process, as developed and at present used, treats impure bullion direct, without presoftening or other prerefining step, except that if the bullion carries tin it is desirable to detin before casting into anodes, since tin carries over to some extent to the cathodes. The refining process developed differs from usual Betts practice in two essential particulars: the anodes are cast thinner and replaced at more frequent intervals, and anode slimes are washed by a system of counter-current dipping, prior to their removal from the surface of the anode scrap. Limiting the period of anode corrosion insures a cathode of high purity, since solution of impurities at the anode can occur only if the thickness of the anode slime blanket, and hence the voltage drop across it, becomes greater than a certain critical value. The dip washing system operates to prevent acid losses, by recovering the highly concentrated, nearly neutral lead fluosilicate solution present in the pores of the slime blanket on the corroded anode, and doing this in such a way that there is no opportunity for chemical decomposition to occur. The best illustration of the efficacy of these two expedients may be secured from records of more than a year's operation of the 25-ton pilot plant, during which period the acid losses were less than 2 Ib. of 100 per cent hydrofluosilic acid (H2SiF6) per ton of lead produced, and typical assays of bullion and refined lead were as shown in Table 1.

Jan 1, 1937

By M. E. Straumanis, S. M. Riad

The lattice parameter of 99.999 pct pure Ag rtlas redetevnzined and found to be az5 = 4.08626 5 0.000041 with the vefnzctiotz correction included); the expatzsion coejjicient between 10° and 65°C was 18.73 X10-6°C-1. The lattice paratneter increased upon solution indium in silver in good agrement with other authors. The solid-solubility limit around room temperature was at 20.4 wt pct of in, which suggests that the high-temperature solubility (at about 689°C) determined by other authors is too low. The expansion coejficient of si1ver increases with the itzcrease of indium content between 10° and 65° C from, 18.73 (In = 0) to 20.9 x 10-6°C-1 (In = 20.4 pct), being only very slightly influenced by small amounts of indium. The expansion coefficents of all solid solutions increarsed strongly with temperature, reaching values > 27 x 10- 6 800°C. ACCORDING to the Ag-In diagram,' the solubility of indium in silver (the a phase) extends to about 18 pct by weight at room temperature. However, there has been only one investigation of the solubility limit by X-ray methods—that of Weibke and Eggers.2 Hume-Rothery, Lewin, and Reynolds measured only the lattice parameters of Ag-In solid solutions3 as did Owen and Roberts4 and Adler and Wagner.' The thermal expansivity of four solid solutions was determined by Owen and Roberts4 in a temperature range between 25" and 300°C. In view of the limited amount of work on Ag-In solid solutions, it seemed appropriate to redeter-mine the lattice parameters and the room-temperature solid-solubility limit, to find the exact expansion coefficients of the solid solutions at about room temperature (between 10° and 60°C) and the expansivity up to 800°C, and finally to derive the thermal-expansion coefficients for any alloy within the solid-solubility region. THE ALLOYS AND THE DETERMINATION OF LATTICE CONSTANTS The metals used were 99.9991 pet pure, supplied by the ASARCO company. Both silver and indium were weighed accurately on an analytical balance in

Jan 1, 1965

By J. Washburn

Two simple types of dislocation distribution were introduced into zinc crystal specimens and the effect of each on the stress-strain curve was investigated. Quantitative results were obtained for simple edge dislocation arrays and for an array of screw dislocations lying in the slip plane. A CCORDING to present knowledge, the disloca-tions present in large annealed metal crystals can be divided into two somewhat arbitrary groups: 1—single dislocation lines distributed more or less at random or forming elements of a three-dimensional network in which the distance between adjacent dislocations is of the order of 10 2 to lo-' cm and 2— widely separated planar arrays of edge dislocations forming dislocation walls or small angle boundaries within which adjacent dislocation lines are spaced at much smaller distances (lo-' to 10- hm). The former can be considered as a dislocation interpretation of the mosaic crystal proposed by Darwin and Ewaldl, ' 40 years ago to account for anomalously high integrated intensities of X-ray diffraction maxima. Small angle boundaries, although now known to be present in most single crystals used for mechanical testing, were not generally recognized by the early workers. This was partly due to the fact that only recently have improved X-ray and metal-lographic techniques been available for checking the macroscopic perfection of crystals."" It has long been known that changes in growth conditions and in annealing procedure, which might logically be expected to cause variations in the structural details of both the dislocation network and of dislocation boundaries, produce marked variations in some mechanical properties such as yield strength." However, no quantitative experimental correlations between changes in dislocation distribution and changes in mechanical properties have yet been made. Such a correlation has been difficult to obtain because, even when great care is exercised to keep the histories of a number of single crystal specimens identical, it usually has not been possible to avoid considerable variation in macroscopic per- fection.' The number and orientation of dislocation boundaries vary from specimen to specimen. This has probably been an important contributing factor to the large scatter in the results of most mechanical measurements on pure single crystals. Some recent experiments"% ith single crystals of zinc have shown that the presence of dislocation boundaries in a specimen can increase its resistance to deformation by slip. With polycrystalline aluminum and nickel, there is also evidence that dislocation boundaries within the individual grains of the aggregate can increase the resistance of the material to plastic deformation, either as measured by tension tests at room temperature or by creep tests at higher temperatures.'" " Although the foregoing observations seem to have established the fact that substructure can have a strengthening effect, the test conditions were too complex to give much information concerning the mechanism. In the foregoing cases, a network of intersecting boundaries having various orientations and boundary angles were present. Before their apparent strengthening effect can be understood, it will be necessary to isolate and study separately the effect of a number of variables: 1—boundary angle, 2—boundary orientation with respect to the active slip direction, 3—number of boundaries, 4—intersections of boundaries, 5—detailed structure of the boundaries, and 6—interaction of impurity atoms with dislocations in boundaries. The object of the present work was to study the effect of dislocation boundaries on flow stress under the following simple experimental conditions: 1— substantially pure shear deformation and 2—boundaries of controlled angle, orientation, and number. In this way, it might be possible to distinguish the important variables from the relatively unimportant ones. Experimental Procedure Stress-strain curves of hexagonal metals are generally nearly linear even out to very large strains."

Jan 1, 1956

By C. R. Tinsley

A strictly limited number of specialist project finance banks exists, with the necessary specialist personnel able to address project cost-competitiveness, cost and commodity forecasting, joint venture negotiations, and completion and sales undertakings. Different techniques of internal bank appraisal are applied, with the usual equity investment project valuation criteria being seldom useful for loan assessment purposes. Company attention paid to the preparation of a sensitivity structured bankable presentation can prove most effective for securing development project finance. Substantial scope is possible for savings of time and money.

Jan 1, 1985

"Coulter's Rainbow and Crooked Falls are situated about five miles below the City of Great Falls. Coulter's, the first of the series in the course of the river, is unimportant and has been submerged by the Rainbow dam. Next below Coulter's is the Rainbow Falls, 47 feet in height. Following Rainbow Falls is the Crooked Falls, 21 feet in height. The power developed at this point is such that the one clam, power house and tail-race utilize the power from all three of the above falls.The development at Rainbow was started October, 1908, and completed July, 1910. It has a total capacity of 21,000 k-w. in generators, and 36,000 h-p. in waterwheels, and operates at 105 foot head. The general scheme of development is typical of what may be called standard practice in the west for plants of medium head, and consists of a low diverting clam, a double pipe line feeding into a balancing reservoir near the plant, and individual pen-stocks supplying the turbines from this reservoir.The dam is a rock-filled crib structure 1,146 feet long and 29 feet high, the up-stream side of which slopes at such an angle that the stability of the clam is assured even under the greatest floods, the weight of the water acting to hold it down, so that the higher the flood the greater the stability. The down-stream side is also sloping and tapers off into a long apron so designed as to take care of any overflow which may occur without shock or commotion. The clam is founded on solid rock throughout its entire length."

Jan 1, 1913

By Morris Cohen, Robert C. Ruhl

The phases in Fe-C alloys over a wide composition range have been studied after splal quenching from the liquid state. Binary alloys containing 0 to 5.1 wt pel C as /cell as a large number of ternary Fe-C-Si alloys with 2.5 to 5.0 wt pct C and 0.3 to 5.1 wt pct Si were attlong those sludied. Olher Fe-C-X alloys, zcilh X being Co, Cr, ,Wn, Ni, and Ru , were also inrestigated after splat quenching. At high carbon contents, a new hcp phase (designaled 6 phase, but different from e carbide) is retained upon splat quenching. The .fraction of this phase varies up lo 97 pcl for a Fe-4.K-1.9% alloy. The composition of the E phase ranges from about 3.8 10 4.8 wt pet C, and the corresponding laltice parameters increase linearly ulith carbon content, while the c/a ratio remains essentially conslc~nl. The E phrtse appears to he a solulion of carbon in E iron, the latler being nornially found only at high pressures. It is deduced that the unit cell of the E phase corresponds to the formula Fe12C3, and llzal il is relaled to tlie ordered slruclures 0.f 6 iron carbide and c iron nilride. The E phase is compared and contrasted to the olher known carbides and nitrides of iron and nickel. An exlrapolaTion of the atomic volume 1,s carhon conlent of /he E pllase lzcts giz.en a neu7 estitnale jor /he alomic volume of E iron, 11.30 cu A, a1 atmospheric pressure and temperature. Other alomic volume relalionships lead to /he co~zpositioti Fe2.iC tor E iron carbide, /he unit cell fortr~ula being -Fe2rClo The E phase undergoes a lulo-slage decomposition upon healing, .forrning firsl rnarlensile plus E carhide, a/ler 1 hr at 140" lo 200°C, slid then ferr ite Plus cementile, after 1 lir a1 330" to 460°C. A1 carbo,l contents between 1.5 and 3.0 LC/ pcl, (he predo.wirzar/t plzase alley quenching is fcc austenite. The retained carbon content of this phase increases with itlcreasing silicon in certain concentration ranges, reaching a maximum of 2.37 wt pct C itz a Fe-2.6C-4.OSi alloy. This is the highest carbon conten1 reLaitled in austenite to date. These high-carbon aus-tenites can be partially tm?zsforttled lo tnartensile hy severe deformation in the temperature range of — 190 to -50°C. TECHNIQUES for splat quenching from the liquid state have been utilized in numerous recent investigations to produce metastable phases in a variety of alloy systems. Among the several ways of splat quenching, the shock-tube method appears to yield the highest cooling rates1-3, 7, 8 and was adopted here. Estimated cooling rates attained in the present experiments ranged from 10' to 10 80Cper sec.' As a part of a research program on interstitial al- loy phases, the Fe-C system was selected for splat-quenching studies. It was hoped that splat quenching would allow high metastable supersaturations of carbon to be retained in solution. Also of considerable interest were the conditions governing the occurrence of the various intermediate phases upon solidification. The alloys investigated included both binary Fe-C compositions as well as six ternary Fe-C-X alloy systems. The known phases in the Fe-C system are summarized in Table I.* Only the ferrite and graphite are ent investigation.14 and is described in detail herein Table II summarizes corresponding data on Fe-N phases, which are also of interest here because of their similarity to the Fe-C phases. EXPERIMENTAL PROCEDURES Alloys were prepared by melting the elements. 99.9 pct purity, in an inert gas nonconsumable electrode arc furnace. The buttons. weighing about 5 g. were remelted twice. were then fragmented. and their interior surfaces were examined for uniformity: if any doubt existed. they were remelted again. Chemical analyses were performed on all the alloys. the accuracy being about k0.05 wt pct. At high temperatures, carbon-containing alloys react with alumina crucibles as follows: If the atmosphere in the splat-quenching furnace does not contain sufficient carbon monoxide the alloy can be depleted of carbon and contaminated with aluminum. Calculations and experimental observations showed that 50 to 100 torr CO partial pressure effectively blocked the above reaction in all the alloys investigated. The splat-quenching equipment in Figs. 1 and 2 provides for evacuation and back-filling with CO-Ar mixtures. The furnace is capable of operation up to 1650°C. and the gettering action of the graphite heating element reduces the oxygen partial pressure in the furnace atmosphere to below 10-5 torr, thus preventing oxidation of the specimens.

Jan 1, 1970

By M. K. Barnett

[ ] ENGINEERING research consists, broadly speaking, in the investigation of the effect of the variations in a number of factors on some property of a product or characteristic of a process. The unambiguous description of the product or process requires that the property or characteristic be expressible in quantitative terms. For the purpose of practical control, it is likewise desirable that the independently variable factors governing the product or process be quantities, although this ideal goal is not always attained. Maximum efficiency-i.e., the attainment of the maximum amount of reliable, useful information relating to the influence of the factors on the property of the product or characteristic of the process, for the least expense-is an important requirement for the satisfactory operation of a research organization. Obviously, a necessary condition for the attainment of maximum efficiency is an adequate knowledge of the specialized field in which the experimental research lies. While necessary, this condition is not sufficient. Proper attention must also be given to the general principles of experimental design together with the modem methods for the analysis and evaluation of experimental data. The present discussion is confined to a single design, the so-called "factorial" design. This design is of special interest in that it attains its goal, maximum efficiency, by directly departing from the

Jan 1, 1947

By F. W. Bloecher, A. M. Gaudin

H. H. Kellogg—There is one point that the author has failed to emphasize sufficiently in his paper. What is commonly called the equilibrium contact-angle (the author's "maximum contact-angle") can have only one value on a smooth, flat, homogeneous surface under a given set of conditions. The equilibrium contact-angle is defined, for such a system, as the angle between the solid-liquid and liquid-gas interfaces, measured through the liquid. The value of the equilibrium contact-angle is uniquely determined by the value of the interfacial energies of the three intersecting interfaces and is independent of other forces in the system. When the liquid-gas interface intersects the solid at an edge—as was the case for all the experiments reported in this paper—the orientation of the solid-liquid interface is indeterminate or varies through 90" for a right-angle edge. Mr. Morris has called the angle between the horizontal and the liquid-gas interface for this edge condition a "static contact-angle." I feel that this term is unnecessarily misleading. In the first place, "static contact-angle" sounds too much like "equilibrium contact-angle." In the second place, the magnitude of the "static contact-angle," which I would prefer to call the "supporting angle," is determined by the forces in the system other than those derived from the interfacial energies, hence "contact angle" is misleading. If Mr. Morris had said that the "supporting-angle" is variable and depends on the weight of the particle and size of the bubble and that it has a maximum possible value equal to the equilibrium contact-angle, his discussion would have been more accurate. T. M. Morris (author's reply)—Mr. Kellogg puts forth a reasonable criticism of some of the terminology used in the paper. I agree that the term "static contact angle" may be misleading. Substitution of the term "supporting angle" or "vector angle" may be more suitable. F. X. Tartaron—In this paper the author presents a very interesting mathematical development of the forces present when a mineral particle adheres to an air bubble. Excellent concordance is obtained between mathematical formulation and experimental results. It is the writer's understanding that when the mineral surface presented to an air bubble is greater than the area of contact, the maximum contact angle is obtained. However, this contact angle represents distortion of the bubble, the normal shape of which is spherical or in cross-section, circular. This distortion produces a force that acts in opposition to the force of adhesion between the bubble and particle. Hence, at maximum contact angle, the force of adhesion between bubble and particle is at a minimum for static conditions. However, when the size of bubble is increased, the size of particle remaining the same (and all other conditions remaining the same), the contact angle decreases, the distortion of the bubble decreases and the force in opposition to adherence of bubble and particle also decreases. Thus, there is stronger attachment between bubble and particle. When this situation is applied to actual flotation conditions, it is doubtful that it has any significance. The reason is that the bubbles are normally so much larger than the particles, that in substantially all cases, it is probable that negligible distortion of the bubble takes place. In table IV, the author makes computations for bubbles from 0.50 to 2 mm diam. This is from 0.02 in. to 0.08 in. Certainly the bubbles generated in a flotation machine are far larger than this. The surfaces of the author's bubbles range from 0.79 to 12.6 sq mm. The area of contact of the glass rod (0.15 mm diam) is 0.017 sq mm. Thus, ratio of bubble surface to mineral area of contact ranges from 47 to 741 in round numbers. If we take a %-in. diam bubble and a 65-mesh (0.208 mm) particle of cubical shape, the ratio of bubble surface to mineral area of contact is 2931. Mineral particles do not readily become attached to air bubbles. Taggart has shown that in pneumatic flotation machines collector-coated particles are only temporarily attached to bubbles. They keep falling off and down in the froth but at a delayed rate as compared with gangue. Spedden and Hannan's motion pictures confirm the difficulty of attaching particles to air bubbles. In the agitation froth process, according to Taggart, air is precipitated from the water selectively on to the collector-coated particles and these

Jan 1, 1951

By F. W. Bloecher, A. M. Gaudin

H. H. Kellogg—There is one point that the author has failed to emphasize sufficiently in his paper. What is commonly called the equilibrium contact-angle (the author's "maximum contact-angle") can have only one value on a smooth, flat, homogeneous surface under a given set of conditions. The equilibrium contact-angle is defined, for such a system, as the angle between the solid-liquid and liquid-gas interfaces, measured through the liquid. The value of the equilibrium contact-angle is uniquely determined by the value of the interfacial energies of the three intersecting interfaces and is independent of other forces in the system. When the liquid-gas interface intersects the solid at an edge—as was the case for all the experiments reported in this paper—the orientation of the solid-liquid interface is indeterminate or varies through 90" for a right-angle edge. Mr. Morris has called the angle between the horizontal and the liquid-gas interface for this edge condition a "static contact-angle." I feel that this term is unnecessarily misleading. In the first place, "static contact-angle" sounds too much like "equilibrium contact-angle." In the second place, the magnitude of the "static contact-angle," which I would prefer to call the "supporting angle," is determined by the forces in the system other than those derived from the interfacial energies, hence "contact angle" is misleading. If Mr. Morris had said that the "supporting-angle" is variable and depends on the weight of the particle and size of the bubble and that it has a maximum possible value equal to the equilibrium contact-angle, his discussion would have been more accurate. T. M. Morris (author's reply)—Mr. Kellogg puts forth a reasonable criticism of some of the terminology used in the paper. I agree that the term "static contact angle" may be misleading. Substitution of the term "supporting angle" or "vector angle" may be more suitable. F. X. Tartaron—In this paper the author presents a very interesting mathematical development of the forces present when a mineral particle adheres to an air bubble. Excellent concordance is obtained between mathematical formulation and experimental results. It is the writer's understanding that when the mineral surface presented to an air bubble is greater than the area of contact, the maximum contact angle is obtained. However, this contact angle represents distortion of the bubble, the normal shape of which is spherical or in cross-section, circular. This distortion produces a force that acts in opposition to the force of adhesion between the bubble and particle. Hence, at maximum contact angle, the force of adhesion between bubble and particle is at a minimum for static conditions. However, when the size of bubble is increased, the size of particle remaining the same (and all other conditions remaining the same), the contact angle decreases, the distortion of the bubble decreases and the force in opposition to adherence of bubble and particle also decreases. Thus, there is stronger attachment between bubble and particle. When this situation is applied to actual flotation conditions, it is doubtful that it has any significance. The reason is that the bubbles are normally so much larger than the particles, that in substantially all cases, it is probable that negligible distortion of the bubble takes place. In table IV, the author makes computations for bubbles from 0.50 to 2 mm diam. This is from 0.02 in. to 0.08 in. Certainly the bubbles generated in a flotation machine are far larger than this. The surfaces of the author's bubbles range from 0.79 to 12.6 sq mm. The area of contact of the glass rod (0.15 mm diam) is 0.017 sq mm. Thus, ratio of bubble surface to mineral area of contact ranges from 47 to 741 in round numbers. If we take a %-in. diam bubble and a 65-mesh (0.208 mm) particle of cubical shape, the ratio of bubble surface to mineral area of contact is 2931. Mineral particles do not readily become attached to air bubbles. Taggart has shown that in pneumatic flotation machines collector-coated particles are only temporarily attached to bubbles. They keep falling off and down in the froth but at a delayed rate as compared with gangue. Spedden and Hannan's motion pictures confirm the difficulty of attaching particles to air bubbles. In the agitation froth process, according to Taggart, air is precipitated from the water selectively on to the collector-coated particles and these

Jan 1, 1951

By H. Margolin, E. Ence

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

Jan 1, 1962

By Frederick W. DeVries

Since we first agreed to present this talk we have learned that some of you may have been covering ground we intend to discuss: Bob Schechter, Daryl Tweeton, Don Seidel, Herb Burgman; however, the ideas were original when we began, "novel" as in the title of the talk, and whether our results are news or merely corroborative, we feel they point a direction that could be valuable to all. We worked with many of you in the past on using hydrogen peroxide in in-situ uranium leaching. Our talk today is not directly related to peroxide; it is, I hope, illustrative of Du Pont&apos;s interest in providing service to this industry in any way we can. The scouting work we are presenting was stimulated by field inputs: First, ammonium carbonate leaches cause restoration problems, primarily because ammonium ions exchange on clays with calcium. Second, sodium carbonate solutions, especially in South Texas deposits, can cause intolerable swelling of clays. From discussions with Dr. van Olphen, who wrote the book on clay chemistry, we inferred by comparison of the radii of the hydrated ions of the elements in these clay systems, that since potassium had about the same radius as ammonium, and sodium was much larger, potassium occupied a unique position to solve both problems. We have shown: FIGURE 1 Potassium bicarbonate systems leach uranium without loss of permeability found with sodium Potassium salts are very effective in restoring ammonia-leached sites Before reviewing the details of our work, which was performed by Hazen Research, Inc., I should like to stress its scouting nature. We are trying to assist the in-situ industry by pointing out new, potentially important directions. But, as with our previous work on sodium silicate to restore permeability, we feel the development phases can generally best be carried out in cooperative programs with companies directly involved with operations. DISCUSSION Test Parameters Now for the details: Our leaching tests were designed to note pressure-drop changes across the ore sample as the uranium was leached. Figure 2 shows the apparatus. The [ ] packed length was 20.5 inches (52 cm) with fifteen hundred grams of ore in the two-inch (5 cm)-diameter bed. Pressure drop was measured by manometer and feed rates were maintained constant with a tubing pump. The samples, from a South Texas leach site, were sealed in "Zip Loc" bags, frozen with "dry ice", crushed (still frozen) through six mesh, and blended before placement into the columns. The ores analyzed as shown here: FIGURE 3 Ore Analyses [Sample A Sample B U308 015% 0122% Mo 0004% 0086% Se0012% <0001% Fe3,078%076% Fee- 098% 044%]

Jan 1, 1979

By J. B. Wagner, p. Hembree

The iron tracer diffusion coefficient of umstite has been measured at 110(fC across the phase field and at a single composition at 800°C. Assuming a simple cation vacancy model the tracer diffusion coefficient was found to be a linear function of the cation vacancy concentration at 1100°C. The equation is D = 3 x 20 29 where denotes the concentration of vacancies in numbers per cc. The tracer work at 800°C was carried out to investigate the reported "pinning" of tracer to the wustite surface at low temperatures. No evidence for the "pinning" of the tracer was found at 800°C in COz-CO gas mixtures. HIMMEL, Mehl, and Birchenall,&apos; Carter and Richardson,2 and Desmarescaux and La combe3 have measured the diffusion of iron tracer in wustite at several temperatures and compositions. The present work was undertaken to extend the measurements over a large composition range at 1100°C and to resolve certain apparent discrepancies in the data, expecially at lower temperatures. EXPERIMENTAL Wustite was prepared by oxidizing rectangular iron plates* in C02-CO mixtures. The samples were •The iron was supplied by the Battelle Memorial Institute courtesy of the American Iron and Steel Institute. The analysis is presented in Table I. quenched. Due to the inward flow of cation vacancies during oxidation, the center of the sample contained a thin void. The edges of the wustite slab were sanded until the sample could be split into two parts. Each part was then sanded on the front and back flat area until a smooth surface was obtained. The specimens were then replaced in the furnace and equilibrated at llOO°C in a predetermined COa-CO mixture by methods described elsewhere.4"6 The specimens were again quenched and the surfaces were lightly sanded to remove any roughness following the first equilibration. The specimens were then reequi lib rated in the same C02-CO mixture for thirty minutes in order to relieve any mechanical damage on the surface due to the polishing. The specimens were then quenched and the tracer was applied by an electroplating technique. The work of Carter and ~ichardson&apos; demonstrated that there was no systematic difference in the iron tracer diffusion coefficient in wustite if the tracer was plated, dried, or evaporated on the specimen. In the present study a piece of filter paper was saturated with an iron chloride solution of pH <* 3 that contained the tracer FeS5. The wustite was placed on the filter paper and made the cathode. A current density of 0.4 to 0.6 ma per sq cm was passed for about five to ten minutes. The thickness of the tracer layer was estimated to be about 7 x lom6 cm. This estimate was made by considering the area plated, the current flow, and time for plating and the activity of the iron in the plating solution. Different areas of the specimen were counted using a collimator to determine the uniformity of the tracer. Any specimen which exhibited a variation from the initial count rate (about 1500 cpm) by more than 15 pct was rejected. An estimate of the time necessary to convert the thin layer of iron tracer to wustite was made using the data of Pettit and wagner." he estimated time was 1 sec at 1100°C assuming linear oxidation kinetics. The shortest diffusion anneals were 1800 sec. The samples were suspended in the hot zone of a furnace by two platinum wires. Two separate specimens were run at the same time. Only the edges of each sample were in contact with the wires. The C02-CO gas of the same composition as that used in the pre-diffusion anneals flowed freely around the samples at a linear velocity of 0.9 cm per sec. To initiate a run, the specimens were lowered from the cold zone of a furnace to the hot zone by a magnetic lowering device." bout 60 sec were required for lowering. To terminate a run, the sample was withdrawn from the hot zone to the cold zone. Time zero for the beginning of the experiment was taken when the sample blended into the red glow of the furnace and conversely for the end of the experiment. The surface decrease method of measuring the tracer diffusion coefficient was used to collect the data. This method requires that counting geometry be reproducible because the specimen is counted before the diffusion anneal and after the anneal. A special jig was constructed for each specimen so the specimen could be removed from the jig and returned to the jig such that the well geometry was reproducible.

Jan 1, 1970

G. H. CLEVENGER, Colorado Springs, Colo.-Mr. Crowe&apos;s paper will be of great interest to cyanide operators, as it is a distinct new development in cyanidation. After reading the paper it occurred to me that some of us had done practically the same thing some time ago, but without design and unconsciously. I refer particularly to the operation of some of the earlier types of vacuum filter, used in connection with a dry vacuum pump and a receiver, which is somewhat similar equipment to that employed by Mr. Crowe. However, we did not appreciate the good effects we were getting from such of this solution as was precipitated, and it has remained for Mr. Crowe to bring distinctly to our attention the advantages of removing air from cyanide solutions before precipitation. Full credit is therefore due him for this very clever improvement in the cyanide process.

Jan 11, 1918

By B. Paul, C. C. Fu

Experiments indicate that the fatigue limit of various drill steels becomes vanishingly small in the presence of water and other corrosive liquids. Therefore one must generally expect fatigue failures of drill steels in a great many field operations. However, it is theoretically possible to so choose the hammer impact speed of a percussion drill in order to maximize the total length of hole drilled before failure occurs. In this paper the existence of an optimum speed is demonstrated and it is shown to be comparable to presently used piston speeds. The influence on drilling speed and hole length of a number of other pertinent design features, such as bit geometry, hammer geometry and steel properties is also established. Although machinery should be designed to obtain optimum performance, it is not always clear just what performance characteristic is to be optimized. For example in a rock drill it would be desirable to optimize all of the following characteristics: drilling speed, bit life, steel life, total length of hole drilled before failure, and efficiency of energy conversion. The word failure could signify excessive bit wear, bit fracture, steel fracture, or some other type of component failure. It is not possible in general to optimize all performance criteria simultaneously. For example, one could achieve fantastically large drilling rates at the expense of bit or steel life, energy requirements and physical size of system. It therefore becomes necessary to compromise requirements in order to achieve a well-balanced albeit non-optimum design. It is, however, extremely useful to explore the interrelationships between the different performance characteristics. Such a procedure would help to establish theoretical limits of performance within the framework of existing knowledge and also serve as a practical design procedure for special applications where a particular performance characteristic is of greatest concern to the user (e.g., steel breakage might be especially undesirable in certain locations). It is the purpose of this paper to examine the problem of how one may drill the deepest possible hole before breakage of the drill steel occurs. Of course the problem is almost trivial if a well defined fatigue limit (endurance limit) exists for the drill steel. In such cases one merely keeps the piston impact speed sufficiently low to insure that the stresses in the steel never exceed the fatigue limit, thereby achieving an infinite life. If, however, no definite fatigue limit exists, as seems to be the case in the presence of even mildly corrosive agents such as water (see later discussion), then a finite life is inescapable and one can at best hope to maximize the useful life of the system. Indeed it will be shown that the system life is related to drilling speed in the manner shown schematically in Fig. 1-a. Even if a definite fatigue

Jan 1, 1965

By Archer Wheeler

THE copper industry in the Province of Katanga, in the Belgian Congo, which is now controlled and operated by the Union Minere du Haut Katanga, had its inception many years ago in the vision of a Scotsman, Robert Williams, now Sir Robert Williams, Baronet. He it was who personally negotiated the mineral concession with King Leopold of Belgium, sent in the prospecting parties who located most of the present mines of the company, later arranged for the Belgian participation from which the present company was formed, and has been its active mentor ever since. The idea back of his efforts was the establishment of an industry on the Congo-Zambezi divide, of sufficient importance to draw up to it the head of the Cape to Cairo Railroad, the dream of Sir Cecil Rhodes, and the consummation of which he had left as a legacy to Mr. Williams, his successor. The reports of the prospecting expeditions showed that copper in profitable quantity was there, but many difficulties lay in the way of the establishment of the infant industry. The isolated location of the mines, various tribal wars, the Boer War, and many other factors contributed to making progress very slow. However, in spite of these difficulties the railroad was finally built and a blast-furnace plant erected at Lubumbashi, near Elisabethville, the capital of the Province. Operations of this plant were started in 1911, treating high-grade oxidized ores and producing pig copper by a reducing smelting. Production has been continuous since that time and the company has grown so that at present it ranks as the largest individual copper producer in the industry. It is a fitting monument to the foresight, optimism and driving force of its founder, and the progressive policies of his Belgian colleagues. In January, 1914, the Union Miniere du Haut Katanga engaged as its consulting engineer, Archer E. Wheeler, metallurgical engineer, at that time general superintendent of the Great Falls plant of the Anaconda Copper Mining Co. Mr. Wheeler was commissioned by the Board of Directors to proceed into Katanga, and make all necessary investigations to enable him to report on a comprehensive development program, and to recommend a scheme of treatment particularly for their low grade

Jan 1, 1932