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By P. R. Sperry, A. P. Beck

It has been shown1 that in poly-crystalline strips of high purity aluminum with a fairly random orientation distribution, grain growth progresses gradually until the average grain diameter reaches a value approximately equal to the strip thickness. Recent work at this laboratory led to the realization that grain growth might be impeded to a considerable extent in the presence of a sharply defined texture, where orientation differences between neighboring grains are small. In order to investigate this effect the following experiment was carried out with the same lot of high purity aluminum previously used for grain growth studies in randomly oriented material.' Very large grain size was developed by grain growth at 650°C in specimens of 0.200 in. thickness. These specimens were then rolled to a thickness of 0.050 in. or 1.25 mm—a reduction of 75 pct. In the rolled strip each large grain corresponded to an elongated area easily identified by etching. After annealing for 1 to 25 min at 600°C and re-etching, these elongated areas were again recognizable. Within each area, corresponding to a single large grain before annealing, there formed by recrystallization a multitude of new grains with a fairly well developed preferred orientation. The orientation and the size of the new grains formed in areas corresponding to different large grains, varied widely depending on the orientation of the parent grains with respect to the rolling direction and the plane of rolling. Many areas were found where the average grain size was considerably smaller than the specimen thickness. Such an area occurred in a specimen cut in half before annealing. One half, containing a portion of the area in question, was annealed 1 min at 600°C, the other half, with the remaining portion of this area, for 25 min at the same tempera-Aluminum killed low carbon steel, § which is now used extensively for severe deep drawing or other difficult forming operations, is unusual in that its grain structure, after cold reduction and box annealing in accordance with conventional continuous sheet or strip mill practice, often is elongated, although at times it is equiaxed. Since this unusual structure has been found superior for many, but not all, severe forming operations, recrystallization of the steel, both at constant temperature and on continuous heating, was investigated and compared with that of rimmed steel in the hope that something might be learned about the mechanism of, and the factors controlling, the formation of such elongated grains. In this structure, the grains are elongated both in the lengthwise direction of the strip and transverse to this direction, even though nearly all of the extension in both hot and cold rolling is in the lengthwise direction. The grains are thus roughly pancake-shaped, being longer and wider than they are thick, as observed also by Burns and McCabe,1 and as illustrated by the typical structures shown in Fig 1. Fig la, representing a conventional longitudinal section, shows the length and thickness of the grains, whereas Fig Ib shows their length and width as seen by examining a section parallel to the sheet surface. Both illustrate the very irregular grain boundaries usually associated with the elongated grain shape. A finer equiaxed grain structure in this same grade is shown in Fig Ic. Either the elongated or the equiaxed structure may be present in the annealed product, and in rare instances the two types may coexist in a single specimen, as shown in Fig 1 d. Isothermal Recrystalliza-tion of Rimmed and Alamimum Killed Steel An aluminum killed steel known to have an elongated grain structure after conventional processing (Steel B, Table l), was selected for the initial recrystallization studies; for comparison, a rimmed steel, A in Table 1, was used. Samples of each in the form of hot rolled strip 0.075 and 0.095 in. thick, respectively, were cold rolled on a small laboratory mill in steps of about 0.010 in. per pass to obtain total reductions of 40 and 60 pct. Small pieces of the cold reduced strip were heated in lead at selected constant temperatures for one of several periods of time, then cooled in air. Rate of heating in the lead was, of course, very fast. Hardness of the cooled specimen was measured and a longitudinal section examined metallographically. Isothermal recrystallization curves for these two steels at 1050°F, based on hardness of the air cooled specimens, are shown in Fig 2 in which the amount of recrystallization corresponding to each plotted point is indicated. The marked difference in the behavior of these two types of steel is evident. After a corresponding amount of cold reduction, the rimmed steel recrys-tallizes in a much shorter time than the killed steel and the shape of its recrystallization curve, (plotted on a logarithmic time scale), is very different. The curve for rimmed steel indicates that recrystallization is analogous to isothermal transformation of aus-i.enite in that it proceeds at a progressively faster rate up to some 50 pct recrystallization, then at an increasingly slower rate. For the aluminum killed steel, however, the start of

Jan 1, 1950

By T. E. Evans, C. T. Baroch

ZrB2 was produced in batches of 4 to 6 Ib by interaction of ZrO2, B4C, B203, and carbon at around 2000°C in a simple graphite resistance furnace. Techniques of production are discussed and the final design of a suitable furnace is described in detail. Several other borides were made by the same technique and the process appears to have possibilities for commercial production. N seeking out new hard and refractory com- pounds, many researchers have turned to the investigation of the borides and excellent papers have been published on the properties of these compounds. Few papers, however, have appeared on the techniques and problems concerned with the production of these high temperature substances. This report describes progress made in developing a method for preparing zirconium diboride, ZrB2, on a pilot plant scale. The literature of the borides and other refractory hard metals recently has been reviewed, annotated, and classified so completely' that it is needless to attempt such an outline here. It is enough to say that three borides of zirconium have been reported: ZrB, ZrB2, and ZrB12.2 ZrB2 is the most stable of these and is especially stable in the presence of carbon up to and including its melting point of around 3000°C. Like most borides, it can be prepared in several ways. It can be prepared by synthesis of the elements, but these are expensive and difficult to produce in a high state of purity. Obviously, production directly from the oxides would have decided economic advantages. In electrolytic production such as that of calcium boride,:' the product is recovered as a sludge mixed with electrolyte; and separation of product from adhering electrolyte and regeneration of the electrolyte is an involved and difficult process. The work on borides was started on a small scale in 1948. Late in 1949, Naval Ordnance expressed a specific interest in ZrB2 and the project then centered on this compound. After the usual experimental work necessary in a new field, ZrB2 of good quality was produced by heating mixtures of B4C, ZrO2, B2O3, and carbon to a temperature of about 2000 °C in a resistance-type electric furnace. Over 100 lb was made for experimental use tests, and the method of production probably could be expanded into a commercial operation. A similar process has been described by Kieffer and coworkers.' The main chemical problems were the development of proper charges to insure complete reduction of the elements, determination of the proper temperature range at which these reductions took place, and adoption of techniques necessary to pre- vent inclusion of such impurities as carbon and nitrides. The mechanical problems consisted of developing a simple practical furnace that would attain the high temperatures required and permit use of a controlled atmosphere when necessary and determining of suitable refractories. Both problems were solved by designing a crucible resistance furnace. Crucible Resistance Electric Furnace Attempts were first made to produce ZrB2 in an electric arc furnace, but such a furnace would not provide the degree of carbon control required for producing clean graphite-free borides, so it was decided to try working in a crucible. Obviously, the furnace would have to be constructed of graphite, as the temperatures required are too high for other refractories or heating elements. Crucibles were made by hollowing out segments of graphite electrodes, which were fitted with a cover and clamped between two electrodes so that the current passing through the thin wall of the crucible would generate heat, using the principle of the Helberger crucible furnace."? Preliminary tests with this type of furnace were encouraging and led to the furnace design shown in Fig. 1. The essential components were a thin-walled graphite crucible resting on a graphite block, which formed the lower electrode assembly, and a top electrode assembly swung from a pipe column making contact with the top of the crucible. The space around the crucible was filled with graphite prepared from waste electrodes crushed to about ¼ in. This packing had excellent insulating properties, both electrically and thermally, and could be removed easily and quickly from around the crucible by means of an industrial vacuum cleaner. The largest resistor crucibles were machined from 8 in. electrode stock and were 26 in. long, with a side wall Yi in. thick and a 1 in. bottom. Temperatures were determined optically by sighting down a 1 in. hole drilled longitudinally through the top electrode and the crucible cover. Sealing this hole at the top was a water-cooled brass sight-glass assembly, shown in Fig. 2. An opening was provided for a light flow of helium to keep the sight opening clear of smoke, and a glass prism above the sight glass changed the line of sight to the horizontal for easier reading. More recently, the prism and optical pyrometer were replaced by a photoelectric recording pyrometer. At first the charges were placed directly in the resistor crucible but this meant that everything had to be withdrawn from the furnace every time the charge was emptied. Later, smaller crucibles were made up that could be placed inside the resistor

Jan 1, 1956

By R. F. Domagala, M. Hansen, D. J. McPherson

Iodide zirconium was combined with calculated amounts of nitrided zirconium sponge and arc melted to prepare alloys in the 0 to 6 wt pct N region. Annealing treatments were carried out at 21 temperature levels. Metallographic examination of the heat-treated specimens permitted construction of the binary phase diagram from 0 to 6 pct N. Features of the diagram include the peritectic formation of both a and ß solid solutions. The maximum solubility of nitrogen is 0.8 pct in 8 zirconium and 4.8 pct in a zirconium. An X-ray study of nitrided materials was made in the range 6 to 13 wt pct N region because serious nitrogen losses were experienced when attempts were made to arc melt these high nitrogen alloys. PHASE relationships in the Zr-N system have been determined. Due to the inability to retain nitrogen in nitrogen-rich alloys subjected to arc melting, definitive work was possible only in the range 0 to 6 wt pct (0 to 30 atomic pct) N. Sufficient complementary X-ray work was done to permit construction of the binary phase diagram up to 13.3 wt pct (50 atomic pct) N (ZrN). Small ingots were prepared by arc melting master alloys with enough zirconium to produce an alloy of the desired composition. Following pretreatment, alloys were annealed at temperature levels between 600" and 2020°C. Determination of the phase boundaries was then accomplished by metallographic evaluation of specimens quenched from the various temperatures. Incipient melting techniques were used to corroborate solidus curves, and X-ray diffraction was employed to study the nitrogen-rich region of the a + ZrN phase field. Materials Westinghouse Grade 1 iodide zirconium crystal bar served as the base material for this investigation. The as-received bars were lightly sandblasted, pickled in a 20 pct HN0-5 pct HF aqueous solution, rinsed in water and acetone, and dried. They were rolled to about 1/32 in. strip and acid-pickled, followed by water and then acetone rinses. The material was sheared to approximately 1/4 in. squares, cleaned with acetone, and stored for use. Pure zirconium nitride is not commercially available, according to correspondence with possible suppliers. A literature survey indicated that nitrogen may be introduced into zirconium metal by passing nitrogen or ammonia gas over zirconium at an elevated temperature. After considerable experimentation, a train was devised whereby high quality nitrogen was passed through a series of bubblers to remove the last traces of oxygen, through an H,SO, bubbler and a cold trap to remove moisture, and finally over zirconium within a resistance furnace. Hand-picked Bureau of Mines magnesium-reduced zirconium sponge proved more amenable to nitriding than the crystal bar. The nitrogen used was extra pure gas purchased from Linde Air Products Co. The first two bubblers through which the gas was passed contained a solution suggested by L. F. Fieser" as being ideal for removing the last traces of oxygen from nitrogen. The solution contains 20 g KOH, 2 g sodium-anthraquinone ,9-sulphonate, and 15 g NaHSO, dissolved in 100 ml water. It is blood-red and turns brown when contaminated with oxygen. A saturated lead acetate solution, next in the series of bubblers, removed any H2S which might have formed in the 0, removal stage. An H,SO, bubbler and cold trap removed moisture before the nitrogen was passed over the zirconium. The zirconium was contained in a stainless steel screen within a Vycor or quartz tube in a resistance furnace. Unreacted nitrogen passed out of the system through a mercury bubbler. A nitriding run was performed in the following manner: Zirconium was placed in the screen within the furnace tube. The unit was assembled, suitably clamped off, and evacuated to remove the air and moisture within the tube and that trapped by the zirconium sponge. The unit was flushed with nitrogen and evacuated twice. After nitrogen was allowed to pass over the zirconium for about 30 min, the furnace was turned on; several hours were required to reach temperature. The reaction was allowed to continue at temperature for about 4 hr and the screen was then withdrawn from the hot zone of the furnace by means of a Nichrome or Kanthal rod. The screen and its contents were allowed to cool at the end of the tube and were then removed. At 800°C no more than about 5 pct N could be introduced into the sponge zirconium. This material was designated M-1 (master alloy No. 1) and reserved for the preparation of alloys in the dilute nitrogen region. A second set of experiments was conducted at 1000°C; no more than 7.2 pct N could be introduced into the zirconium at this temperature. Enough material (M-2) of this nitrogen content was prepared to produce a second set of alloys to complement the first and to provide alloys in the 0 to 6 wt pct N range. It was hoped that a diffusion anneal plus a re-nitriding might yield a material of higher nitrogen content. The material containing about 7 pct N was therefore given a homogenization treatment at 1000°C for 6 hr under an argon atmosphere. It was

Jan 1, 1957

By George A. Roberts, Arthur H. Grobe

H. H. Hausner (Sylvania Electric Products Inc., Bayside, N. Y.)—I tested the 18-8 stainless steel powder described by Grobe and Roberts and the results were excellent. The powder was compacted and sintered in purified hydrogen to a very low density (approximately 20 pct and more porosity). Where the other powders show very little ductility when sintered to such a low density, the described stainless steel was surprisingly high in ductility. I would appreciate it if the authors could give us some data on a similar powder but without silicon and also data on 430 stainless steel powder. H. S. Kalish (Sylvania Electric Products lnc., Bay-side, N. Y.)—I should like to verify the excellent results obtained by Grobe and Roberts with their pre-alloyed stainless steel powder. It seems to me, however, that their data are conservative and that even better densities and higher tensile strength can be obtained with these powders by the selection of proper particle size fractions. The accompanying data were obtained by sintering compacts pressed from the powder made by Vanadium-Alloys Steel Co. to 0.8 in. in diam about % in. high in a cylindrical double action die without the use of lubricant. The compacts were sintered for 1 hr at 2370°F in hydrogen purified by passing it through a Deoxo unit (palladium catalyst) and a Lectrodryer. Even the density obtained using the as-received (—100 mesh) compacted at 40 tsi was quite high as was the hardness. This indicates that by increasing the sintering temperature slightly above 2350°F the coining and subsequent secondary sintering operation can be avoided. With the — 325 mesh fraction, however, very much higher density can be obtained and a high hardness. I have no tensile data to present, but I feel that it is not too optimistic to expect. that unusually high tensile strengths and good ductility can be obtained in this sintered material on the basis of the density and hardness data. The sintered stainless steel made by the above-described methods came out of the furnace very bright and clean. The purified hydrogen atmosphere is important in sintering stainless steel to reduce the oxide present in the powder. The result of such a sintering is good densification and good ductility of the sintered product. G. A. Roberts (authors' reply)—We are greatly indebted to Messrs. Hausner and Kalish for their discussions of our paper. Their encouraging remarks are greatly appreciated and their confirmatory data will do much to add to the value of the paper. At the present time it is impossible to provide complete data on a similar stainless steel powder without silicon, but we do know that, in general, the properties are slightly inferior. Data on such a powder and on other stainless steel types are to be published in the near future.

Jan 1, 1952

By Walter R. Hibbard, Harold Margolin

DURING preliminary tests on the aging of a Cu-plus 5 pct Ag alloy,' a specimen which had been overaged 24 hr at 550°C was annealed in a nitrogen-hydrogen atmosphere first for 2 hr and then for an additional 28 hr at 600°C. After each anneal the specimen was cooled to room temperature in about ½ hr and X-ray photograms were made. The first film, Fig. la, revealed two sets of copper-base lines, one intense and corresponding to the parameter at 550°C, the other fainter and shifted away from the beam, corresponding to the larger parameter at 600°C (see arrows). The 30-hr film, Fig. lb, revealed the same two sets of copper-base lines with a reversal of intensity. In neither case do the copper lines form a broad band which would be indicative of a range of compositions. This phenomenon is thus a "discontinuous" type of solution. A similar phenomenon was observed in a Ag-rich Cu-Ag alloy.' Finlay and Hibbard9 have suggested that directional rather than random solution of precipitate occurs in some alloys. Conceivably, for Cu-Ag alloys, the matrix-transition-precipitate precipitation sequence is reversible for the re-solution of the precipitate caused by rapidly raising the annealing temperature of an overaged specimen. A copper-base transition structure supersaturated with solute might be formed around the precipitate as it dissolves, thus obviating the necessity for a gradually changing solute composition of the matrix. The solute atoms then might be transferred rapidly and locally from the transition to the matrix phase in the proper amount and at the proper location to obtain directly the new ex- panded solid solution. The theory implies a minimum of diEusion of solute in the matrix (i.e., no significant range of matrix composition) and possibly suggests that the composition of the transition structure will vary with the conditions of re-solution. A transition copper phase found in aged Cu-Ag alloys1 might fulfill this function. Evidence regarding this suggestion could be obtained in Cu-Ag alloys by overaging a specimen until no trace of the expanded copper lattice is present and then subjecting the specimen to a retrogression treatment. Re-appearance of the transition copper phase would confirm the theory. Additional details could be secured by varying both aging and retrogression temperatures. References 'H. Margolin and W. R. Hibbard, Jr.: Effect of Ternary Additions on the Age Hardening of a Copper-Silver Alloy. Trans. AIME (1951) 191, p. 174; Journal of Metals (Feb. 1951) TP 3002E. 2 W. Ageew, M. Hansen, and G. Sachs: Decomposition and Changes in Properties of Super-saturated Silver-Copper Alloys. Ztsch. Physik (1930) 66, p. 350. 3W. L. Finlay and W. R. Hibbard, Jr.: Some Effects of Applied Stresses on Precipitation Phenomena. Trans. AIME (1949) 180, p. 255; Metals Technology (Sept.

Jan 1, 1952

By A. U. Seybolt

DURING the course of experiments involving oxygen equilibrations with a high-purity Pd-5 at. pct Rh alloy, the appearance of a subscale was noted. Most of the heat treatments in a pure oxygen atmosphere were performed at 900°C. The presence of the subscale was noted when the oxygen partial pressure was in excess of approximately 95 mm, up to 1 atm, the highest pressure used. According to available thermodynamic information' on the free energy of formation of Rh2O3 (the only reliably reported solid oxide of rhodium), this oxide should not be stable under these conditions, nor, of course, any oxide of palladium. Extraction of the subscale from the matrix was affected by treatment with aqua regia, and the resulting X-ray diffraction powder pattern is shown in Table I. This pattern is not that of Rh2O3, nor that of any known rhodium or palladium oxide. It can be indexed on a hexagonal lattice with a. = 5.22Å and co = 6.0Å. In addition to this unknown material, there was a weak Rh2O3 pattern. An X-ray fluorescence analysis of the powder gave 3214 palladium counts per sec and 5381 rhodium counts per sec, thus indicating the likelihood of a double oxide of palladium and rhodium. In view of the fact that the above result was obtained on a single sample, it is perhaps best not to insist upon the above ratio of about 0.6, but possibly to tentatively assume 0.5 or 1/1. The small amount of Rh2O3 in the X-ray pattern might have occurred on cooling, and it seems possible that the double oxide, below some temperature level, is not as stable as Rh2O3. To examine this point, some of the extracted double oxide was heated on a sheet of pure palladium in air at 900°C, and allowed to furnace-cool over a period of several hours. The X-ray diffraction pattern of the powder showed approximately the same intensity of Rh2O3 and the "hexagonal" oxide as before, but, in addition, a rather faint pattern of another crystalline species made its appearance. This finding again suggests partial transformation of the major (double) oxide to other oxides on cooling from 900°C. Application of the phase rule shows that only one equilibrium oxide (subscale) could have been present at temperature. Vacuum-fusion, oxygen analysis of the extracted subscale showed 7.7 ± 0.7 pct O. Combining this information with that of the X-ray fluorescence analysis suggests the formula PdRhO. This compound should have an oxygen content of 7.07 pct, which is within the range of error of the oxygen analysis. However, until a more careful stoichiometric study is made, it is suggested that the formula be written

Jan 1, 1965

By K. R. Van Horn

RESIDUAL stresses in metals operate under a cloak of mystery, as they have neither been seen in the laboratory nor detected by means of the microscope. In spite of their phantom-like nature, they frequently exert metallurgical effects that cannot be ignored. In some cases the results have been detrimental, causing rejections or premature failures, but frequently the effects have been highly beneficial to the producer or consumer of metal products. First, however, what is a residual stress? When a metal is plastically deformed by bending, rolling, pressing, or by a phase transformation or precipitation from solid solution, or by a sharp temperature gradient resulting from nonuniform cooling, quenching, or welding, it remains in a state of strain. The strains or strain gradients produced by such operations and retained after all external forces are released are known as residual strains, and the accompanying stresses as internal or residual stresses. Many defects or failures in metal products have been ascribed to residual stresses, sometimes erroneously, because there was no other apparent explanation after the usual metallurgical tools of diagnosis had been applied. For example, during World War 11, the forged aluminum alloy aircraft cylinder head in the reciprocating engine began to replace the cast head with the familiar cooling fins. The fins were machined in the solid forged head by an ingenious milling operation. One plant reported an epidemic of excessive distortion during the delicate high-speed milling. A thorough examination revealed that the composition, heat treatment, mechanical properties, and metallurgical quality of these heads were comparable to those of forgings that machined satisfactorily. It was then claimed that the cause of the machining difficulties was connected with residual stresses resulting from the quenching during the solution heat treatment. An elaborate stress analysis actually demonstrated, however, that the magnitude of residual cooling stresses was lower in the cylinder heads which machined poorly than in those which were satisfactory in this respect. Subsequent tests proved that the machining problems in this case originated from variations in the tools and tool design. Sources of Residual Stresses in Metals Residual stresses are of two origins—mechanical and thermal. Thus, stresses may be produced in a metal by any cold-working process. The distribution and magnitude of these mechanically produced stresses can be calculated in a satisfactory, although approximate, manner for such simple cases as bending, torsion, and expanding of tubes. However, most manufacturing processes are too complex, and the original stress-strain relations in the products are not sufficiently known to permit calculation of the resulting residual stresses. Also, a specific process, such as wire drawing, may vary in complexity or uniformity of working, and large or small residual stresses may result, depending on the conformation of the dies and other features of the working process. Neither substantially unidirectional deformation, such as can be imparted by stretching a metal product having essentially the same mechanical properties throughout the cross section, nor deformation

Jan 1, 1954

By S. C. Sircar, B. K. Dhindaw

KINETICS and mechanism of sulfation reactions have been studied extensively. Qualitative and quantitative data are reported for the kinetics and mechanism of sulfation reaction of copper oxide pellets;''2 yet it remains a controversial Subject. The mechanism and kinetics of the sulfation of zinc oxide powder (B.D.H. analar quality) were studied by gravimetric technique. A spring of high-carbon steel wire with accuracy well within 0.2 mg was used for measuring weight change. The sample was taken in a Pyrex glass bucket, hanging freely inside a Pyrex glass tube reactor, with a gold wire attached to the spring, the reactor being surrounded by a movable furnace (double wound type) with a temperature control within *5"C. Flow of oxygen, 60 cu cm per min, and sulfur dioxide, 45 cu cm per min, were measured through calibrated flowmeters and the mixture dried over PZ05 before entering the reactor. The experimental results are presented in Figs. 1 and 2. The plot of weight change of zinc oxide, giving the amount of zinc sulfate formed, was found to be linear over the temperature range of 500" to 700° C and up to a conversion of approximately 60 pct, as beyond it they divert from linearity.' The rate of sulfation was found to be affected by total flow rate of gases at a fixed ratio of SO2/O2, up to 60 cu cm per min, and was found to be linearly dependent on quantity of total powdered sample taken. The plot of rate of sulfation of zinc oxide, 70 mg, with varying amounts of vanadium pentoxide, at a constant ratio of gases as mentioned above, and at a constant temperature of 625"C, was also found to be linear as seen in Fig. 2. Extrapolation to zero V2O5 addition gives the same rate of sulfation, as in case of pure zinc oxide, 70 mg. Vz05 was prepared by heating ammonium vanadate at 600°C for 15 min in a muffle furnace. The available literature points out that the theory of sulfation that has received the maximum support postulates the following mechanism for sulfation of ZnS: 2ZnS + 30, = 2Zn0 + 2SOZ; the ZnO formed acts as a catalyst for the reaction, 2 S02 + O2 = 2S03. This SO3 reacts with ZnO to give zinc sulfate. It is suggested here that the above widely supported mechanism is operative in the sulfation reaction and that the rate-controlling step in the sulfation reaction of ZnO is the formation of SO3 from SO, and 0,. The authors are carrying on further work in this line, and the details will be published later. The authors wish to acknowledge the facilities provided and the help extended by Prof. P. R. Dhar, Head, Department of Metallurgical Engineering, and the permission granted to publish this note by the Director, I. I. T., Kharagpur.

Jan 1, 1969

By Basil B. Zavoico

The World War I1 spread to Russia on June 22, 1941, when the German Armies began their invasion. The Soviet industries, which were already engaged in a tremendous armament program, further accelerated the flow of munitions, and equipment and supplies for all purposes not directly military were either entirely eliminated or reduced to an absolute minimum. With the occupation by German armies of the Dniepr and Kharkov industrial regions, this trend was necessarily further accentuated. The oil industry of Russia, in consequence, was left to rely more and more upon itself, its own very limited manufacturing facilities, extensive repair shops and probably much used equipment out of order stacked in the warehouses. All evidence available to date points to the fact that the new situation not only did not affect the production either quantitatively or qualitatively, but, on the contrary, caused a larger flow of much needed fuels to the country's war machine, primarily by renaissance of both management and labor. The oil industry of the Soviet Union, left to depend entirely upon itself for equip ment and supplies, and even for new workers and technicians to replace those called into the services, did and is still doing a good and effective job. Since it could not hope for new equipment and parts and could not blame any other industry for the delays in delivery, it dragged out old machines from storage and repaired them in its own machine shops. Often such stored and used equipment was but slightly defective, waiting for some small part from factories in Central Russia, plants that now were either in German hands or entirely converted to the manufacture of munitions. More particularly, instead of the pipe that could not be taken to the Caucasus from Central Russia, casing reclaimed from abandoned or submarginal wells was used, or pipe from the abandoned or but slightly used pipe lines; and this practice is being continued even now on a large scale, to create an ample reserve for the duration of the conflict. Indirectly such a development was even an improvement on pre-war days, when many wells about to be completed had to wait for weeks, even months, for the arrival of new pipe, all blame then being placed outside of the industry on the factories in Central Russia. For the purpose of reclaiming equipment and pipe still usable, special crews were organized. The war also caused much quicker adaptation of certain American practices and introduction of many emergency measures, such as: removal of derricks upon completion of wells and the use of drilling equipment mounted on skids for rapid transfer from location to location—both of these practices, while standard in the U.S.A., being new in Russia; installation of simplified surface pumping units; substitution of wooden bearings in the surface pump equipment; completion of wells in the Ural-Volga district, where formations are hard and tight throughout the sedimentary column, without either casing or

Jan 1, 1942

By W. J. Kroll

W. J. Kroll (Belgium)—Those who are acquainted with the metallurgy of our forefathers may have occasionally a good time when glancing at recent publications in which aged discoveries are unconsciously reported as novelties. We know very well, that oxygen blowing of iron has been described by old Bessemer. The author of the present article is, however, not aware of the fact that the process he describes, the fused salts scrubbing, was already used in the middle of the last century by St. Claire Deville in his attempts at making higher-purity aluminum from raw AlCl3 by sodium reduction. The same fact escaped the three investigators to whom the author refers. The technical grade AlC13 produced by St. Claire Deville from impure oxide, chlorine, and carbon (Oersted process) was contaminated with Sic4 and FeC13, which he removed on an industrial scale by various methods.' He sublimed, for instance, his chloride in contact with iron nails, or aluminum chips, or in hydrogen, which reduced the FeC13 to the less volatile FeCl2. He used also alkali-alkaline earth chlorides as a solvent for A1C13 and FeC13 in presence of iron as a reducing agent, and sublimed his purified AlC13 from solvent salts. The successors of Deville used also zinc or lead as a reducing agent. These methods were later used currently for the purification of BeCl2 and for collecting this compound in a salt bath, suitable for fusion electrolysis. More recently, the same Deville process has been described as applied to the purification of ZrCL4, as part of a method of extraction of ZrCL4 from silico zirconium, which later was reacted with FeC12 in a separate part of the equipment. According to the patent referred to3 the ZrCL4 is dissolved as a gas in a carrier salt such as alkali-alkaline earth chloride, from which it can be reclaimed in a purified form by distillation. A bath of NaCl/KCl is recommended in the specifications. The FeC12-FeC13 go in the salt solution in which raw ZrCl4 is introduced by bubbling, while Sic4 and Tic4 pass through the bath and escape in the atmosphere. purification by this salt-solvent method is thus well described. It may be worth while insisting on some minor details about which the author did not bother too much. One of these concerns the material of construction for the container. If iron is used, and if no other reducing agent is added, then it is the iron of the pot that acts as a reagent in the breakdown of FeC13 to FeCl2, and corrosion can be expected. This shows the importance of using extraneous large surface-reducing agents, of which there is a choice. Zir-

Jan 1, 1963

By Walter Miller

Crude oil stocks were some 10,000,000 bbl higher on June I, 1947, than at any time during 1946 but the extremely heavy refinery runs the last half of 1947 cut crude inventories to approximately the 1946 closing level of 225,000,000 bbl. Many refiners were seriously short of crude oil during the year. This shortage was reflected in numerous advances in the posted price of crude, justified in part as an incentive for more production but more generally due to competitive bidding. Some purchasers of crude, endeavoring to keep their plants running, resorted to the payment, either directly or indirectly, of premiums above the posted price. Another common practice employed by some suppliers of crude oil was to demand refined products in exchange or trade for their raw material. The refined products picture has darkened in spite of record throughputs. Stocks of gasoline and light and heavy fuel oils were uncomfortably low at the beginning of the year and were in general still lower at the close. The rationing of some products, principally gasoline, to dealers and stations? initiated during the year, gained momentum as stocks continued to diminish. The emphasis placed by the manufacturers of oil-burning equipment on the convenience and economy of heating with oil, together with the tight situation in coal, has developed a tremendous demand for burning oils. Consumption of liquefied petroleum gas for domestic and household fuel had more than doubled in 1946 over 1943, and the demand seems to be limited only by the ability of the equipment builders to furnish necessary storage. transportation, and burning equipment. The supply situation is likely to become more acute in 1948. Demand for petroleum products is being pushed to new heights not only by the unprecedented domestic market but by a sudden and drastic upswing in estimates of military and governmental requirements. Additionally, oil exports are running far below the volume requested, amounting to less than forty percent in a recent quarter, and export licenses are reportedly being approved on the basis of urgent need *only. AX recent White House release sees little likelihood that estimated requirements of the sixteen nations participating in the proposed Marshall Plan can be met in full over its projected life—1948 to 1951. Present demand dictates maintenance of refinery operations at the highest possible level and the Bureau of Mines has forecast daily average crude runs in 1948 of 5,265,000 bbl. The Economics Advisory Committee of the Interstate Oil Compact Commission recently estimated the 1948 demand for petroleum products at nearly 6 pct above 1947. They further estimate daily average crude runs of 5,375,000 bbl in 1948, some 2 pct higher than forecast by the Bureau of Mines. Projected demand exceeds supply to the extent that Capitol Hill is reportedly investigating ways of enabling oil companies to act in concert without danger of antitrust prosecution, such as elimination of crosshauls, pooling of products, and lowering of octane.

Jan 1, 1948

The Climax Molybdenum Company' s newest operation is the Henderson project, which is located on the east side of the Continental Divide. Ore reserves are estimated at more than 300 million tons at a grade of 0.49% MoS2. For mining the ore a modified panel caving system is used. The ore is transported to the Henderson mill on the west side of the Continental Divide on a 42 in. (1.07 m) gauge railroad through 9.6 miles (15.4 km) of tunnel and 4. 8 miles (7.7 km) of surface track, a total distance of 14.4 miles (23. 2 km). Each train consists of 30 ore cars with capacity of 22 st (20 mt) of ore or 660 st (599 mt) per train. The unmanned trains operate completely automatically. At the 54 in. by 84 in. primary gyratory crusher, the bottom dump ore cars pass over a dump scroll to discharge at a maximum rate of 100 st (91 mt) per minute. Dumped ore falls onto a rock box before passing over a 17 ft long by 46 ft wide (5. 2 m by 14 m) grizzly set at a 40° angle with bar spacings of 7 ½ and 8 ½ in. (191 mm and 216 mm) openings. An estimated 30 to 50% of the ore (which at times is wet and sticky) passes through the grizzly. The operators report that a shallower angle on the grizzly, perhaps 35º to 37º, would have been sufficient and would have prevented impact on the back of the crusher pocket by large boulders. This pocket as well as the crushed ore pocket under the crusher is lined with AR plate. The accompanying drawings show a "future splitter" and the operators are planning the installation of this unit to prevent impact and subsequent damage to the crusher spider. Crushed ore at an 8 to 9 in. (203 mm to 229 mm) size joins the grizzly undersize in the pocket beneath the crusher. This pocket is sized at 660 live st (599 mt) so that it will accept an entire trainload of ore. Crushed ore is removed from the pocket by a four-speed, 84 in. (2. 1 m) apron feeder operating at 9.6 to 29. 3 fpm (2.9 to 8.9 mpm). A 60 in. (1.5 m) takeaway conveyor operating at 480 fpm (146 mpm) delivers the crushed ore to a 58,000 st live and 193,000 st total (52,600 and 175, 100 mt) open stockpile under an A -frame supported tripper gallery. Impact idlers on the takeaway conveyor under the apron feeder discharge are mounted on wood blocks for a cushioning effect and ripped belt detecting bars are located behind each impact idler. The conveyor tunnel is of corrugated and galvanized steel construction rather than concrete. The concrete crusher enclosure is circular in design from its lowest level at elevation minus 110 ft 4 in. (minus 33. 6 m) to elevation

Jan 1, 1978

record with the Royal Flying Corps was considered a remarkable one, for he was at the front within two months of the date on which he was granted a commission, during which interval he took the prescribed technical course at Oxford, and aviation training at Netheravon and Bristol. On Sept. 14, 1916, he took his first flight over the German lines, when his engine stalled and he had to volplane down, fortunately landing on the French side of the lines. On Sept. 16, he went over the lines with six others, and not returning immediately with the others, was lost. He tried to make for the sea and come back following the course of a river, but when he did descend he found that he was 60 miles west of Paris and 100 miles south of his lines. He flew over to Paris and stayed there for the night, going back to his squadron the next morning. Then on Oct. 4, he was sent up at night for the first time, and in making a landing he passed the flares just as he struck the ground, which put him in total darkness. He struck something and his machine turned a complete somersault, which accident put him in the hospital for ten days. In December, 1916, he left the 21st Squadron and was transferred to the 24th, as the 21st was made an Artillery Squadron and he preferred to remain a fighting scout. In the same month, he was made Acting Flight Commander for about 6 weeks, and about April 3, 1917, his rank of Flight Commander was confirmed. The beginning of May he started to introduce a number of new machines for his squadron, these being of an entirely new type. On May 19, he was up with one of the machines in the evening, practising sharp turns and dives, when the wings suddenly crumpled up and he fell 700 ft., being killed instantly. He was buried in a French Cemetry at Monchy Lagache about 8 miles southeast of Perronne, and about 25 miles east of Amiens. Sergeant Herbert Moore Harbach Herbert Moore Harbach was born in Lebanon, Pa., Apr. 4, 1891, graduated from the Lebanon High School in 1911, and entered State College from which he received his degree of Bachelor of Science in Metallurgical Engineering in 1915. He was employed by the Lackawanna Iron Co., at Buffalo, W. Y., and was later transferred to their Lebanon plant to start up the newly erected benzol plant. He was later made foreman of the coke ovens, which position he held after it was bought by the Bethlehem Steel Co., and until he enlisted in the service of his country in September, 1917. He was stationed at Camp Meade, Md., until the spring of 1918, when he was transferred to the C. W.

Jan 1, 1920

The Pinto Valley, Arizona, plant of Cities Service Company is one of the newest copper producers in the United States, having started production in 1975. It is located a few miles west of Miami, Arizona, on the site of the Castle Dome Mine, a World War II operation which was shut down and its mill later moved and renamed the Copper Cities plant. The Pinto Valley concentrator uses six 18 ft (5. 5 m) diameter by 21 ft (6.4 m) long, 4000 hp, single-stage ball mills, taking crushed ore from four 7 ft (2. 13 m) standard and eight 7 ft shorthead crushers. It has a design capacity of 40,000 stpd but has higher tonnage capability for an expanded concentrator. The copper porphyry-ore is mined by two 15 yd and one 20 yd shovels (11.5 and 15.3 cu m) and is transported to the primary crusher by 150-ton trucks. The dump pocket is relatively shallow (14 ft or 4. 27 m deep); and because of the width necessary for the 150-ton trucks, it was designed to use the ore itself instead of manganese steel as an abrasion- resistant lining, although a heavy steel cap protects the dump pocket top edge. The pocket has a capacity of 300 tons of ore. Water sprays under the dumping positions direct a fog toward the truck being dumped for excellent dust control. Breaking of oversize is done by a hydraulic impact breaker mounted on a hydraulically operated articulated arm situated at the side of the dump pocket. Again because of the shallow pocket, no splitter is used to protect the spider of the 60 in. by 89 in. Traylor gyratory crusher, which is equipped with a hydroset mechanism. Crushed ore at 8 in. (203 mm) drops into the 360 st surge chamber lined with AR plate and then is fed directly to the 60 in. (1.52 m) stock- pile conveyor by an 84 in. by 20 ft (2. 13 m by 6.1 m) four-speed apron feeder at a rate of up to 4000 stph. Early in 1977, Cities Service will replace the four -speed electric drive with a hydraulic pump and motor with infinitely variable speed. They are also studying the replacement of the apron feeder with an 8 ft wide (2.44 m) belt feeder similar to those at Similkameen and Palabora. Peak crushing capacity would then be increased to 5000 stph. The AR plate in the crushed ore pocket was installed in large, rectangular sheets which required much less embedded metal to hold it in place than would the more conventional, smaller arid square pieces of cast manganese steel. For duty in the crushed ore pocket, where wear is not severe, the AR plate is a satisfactory material. The new Palabora Figure-8 crusher also uses this design.

Jan 1, 1978

By E. H. Burdick

THE difficulties inherent in table concentration operations as applied to gold, silver, lead and zinc ores, are accentuated in the scheelite mill, which has a flowsheet that is similar in general principles. The narrow "spread" in the specific gravity between scheelite and the usual gangue in which it occurs often makes its clean separation extremely difficult and in some cases impracticable. The problem is further complicated by the extreme friability of the mineral and its inordinate tendency to "slime," particularly where fine grinding is necessary and wet grinding methods are employed. The physical aspect of the occurrence of scheelite in the ores, the kind and character of the rock in which the mineral is present, its hardness, friability and the specific gravity of its constituents, as well as like characteristics of the associated minerals-pyrite, pyrrhotite, sphalerite, and others, all have a bearing on the successful milling of crude ores and the production of a concentrate that is marketable with minimum price penalty or none at all. Most tungsten deposits are considered low grade when the limiting factor of low percentage recovery by gravity methods is borne in mind. The great majority of deposits developed or in process of development carry from 0.4 to 1.0 per cent tungstic oxide. Ore carrying I per cent is considered good grade; 0.7 to 0.8 per cent, fair, and below that figure, low grade. Steady mill feed averaging upward of 1.0 per cent W03 is exceptional. Inasmuch as buying specifications demand a 60 per cent W03 content, the mineral content of the ores as mined must be concentrated to at least that degree. A few companies have constructed chemical plants for the treatment of their complex concentrates and low-grade flotation product, but the smaller operator must rely on table concentration, borrowing the tools and to a large extent the methods of his predecessors in the gold, silver, lead and zinc mills. Whether these are the best tools and methods that can be devised is an open question. Except in rare instances, table concentration, however carefully conducted, does not yield a satisfactory final recovery of the mineral content in headings as indicated by chemical determinations of tungstic oxide content. A saving of 60 to 65 per cent is considered fair, and an average 80 per cent recovery, exceptional. Each scheelite ore body is a separate problem. Details of handling that give best results in one case may not be successfully operative at a property on the same contact zone and but a short distance removed. Supplementary treatment of tailings by flotation may be successful in producing a low-grade concentrate of around 15 per cent WO3, which is adapted to further treatment chemically at a given property and entirely unsuccessful at another. This problem constitutes another of the unanswered questions. The following paragraphs relate solely to the beneficiation of scheelite ores by table concentration and supplementary methods.

Jan 1, 1942

By Walter Miller

Crude oil stocks were some 10,000,000 bbl higher on June I, 1947, than at any time during 1946 but the extremely heavy refinery runs the last half of 1947 cut crude inventories to approximately the 1946 closing level of 225,000,000 bbl. Many refiners were seriously short of crude oil during the year. This shortage was reflected in numerous advances in the posted price of crude, justified in part as an incentive for more production but more generally due to competitive bidding. Some purchasers of crude, endeavoring to keep their plants running, resorted to the payment, either directly or indirectly, of premiums above the posted price. Another common practice employed by some suppliers of crude oil was to demand refined products in exchange or trade for their raw material. The refined products picture has darkened in spite of record throughputs. Stocks of gasoline and light and heavy fuel oils were uncomfortably low at the beginning of the year and were in general still lower at the close. The rationing of some products, principally gasoline, to dealers and stations? initiated during the year, gained momentum as stocks continued to diminish. The emphasis placed by the manufacturers of oil-burning equipment on the convenience and economy of heating with oil, together with the tight situation in coal, has developed a tremendous demand for burning oils. Consumption of liquefied petroleum gas for domestic and household fuel had more than doubled in 1946 over 1943, and the demand seems to be limited only by the ability of the equipment builders to furnish necessary storage. transportation, and burning equipment. The supply situation is likely to become more acute in 1948. Demand for petroleum products is being pushed to new heights not only by the unprecedented domestic market but by a sudden and drastic upswing in estimates of military and governmental requirements. Additionally, oil exports are running far below the volume requested, amounting to less than forty percent in a recent quarter, and export licenses are reportedly being approved on the basis of urgent need *only. AX recent White House release sees little likelihood that estimated requirements of the sixteen nations participating in the proposed Marshall Plan can be met in full over its projected life—1948 to 1951. Present demand dictates maintenance of refinery operations at the highest possible level and the Bureau of Mines has forecast daily average crude runs in 1948 of 5,265,000 bbl. The Economics Advisory Committee of the Interstate Oil Compact Commission recently estimated the 1948 demand for petroleum products at nearly 6 pct above 1947. They further estimate daily average crude runs of 5,375,000 bbl in 1948, some 2 pct higher than forecast by the Bureau of Mines. Projected demand exceeds supply to the extent that Capitol Hill is reportedly investigating ways of enabling oil companies to act in concert without danger of antitrust prosecution, such as elimination of crosshauls, pooling of products, and lowering of octane.

Jan 1, 1948

By Nicholas J. Grant, H. C. Chang

EMPHASIS on the importance of grain boundary sliding as a mode of deformation at elevated temperatures has been presented elsewhere.' The extent to which boundary sliding occurs under certain creep conditions has been determined for high purity aluminum2,3 and aluminum alloys.' In general, boundary deformation extends quite far into the adjoining grains, resulting in a rather wide band of deformation along the grain boundaries. This has led some investigators to doubt that grain boundary sliding consists of shearing along the boundary surface; it has been contended instead that boundary sliding is a result of concentrated slip in the neighborhood of the deformed grain boundaries."' The purpose of this note is to present evidence that grain boundary sliding takes place by a bulk shear process. gh purity polycrystalline aluminum, wherever and whenever there is grain boundary sliding, boundary migration and concentrated deformation along both sides of the deformed boundary are associated with it. Therefore, it has been rather difficult to obtain unambiguous evidence of boundary sliding. On the other hand, it would be expected in certain alloys of aluminum, when tested under particular conditions. that the severity of the interfering effects of boundary migration and concentrated deformation along the deformed boundary might be reduced. Current research in this laboratory' shows that a 20 pct Zn-A1 solid solution alloy fractures in an intercrystalline manner during creep at 500°F with a small total elongation of not more than about 14 pct, and that it does so with extremely limited grain boundary migration. Accordingly, this alloy was chosen for the present study. The experimental procedure was similar to that used in previous work and has been presented elsewhere.' Two parallel flat surfaces were milled from a round specimen. The gage portion of the specimen was 1 in. x .09 in. x .17 in. The specimens, which were annealed at 1030°F for 24 hr, showed two to four grains across the width of the test bar. The specimens were subjected to creep at 500°F at stresses of 2000 to 5000 psi. The rupture times were from 10 sec to 3 hr. Appreciable boundary sliding occurred in all the tests. A typical example of boundary sliding is shown in Fig. 1. (The tension axis is vertical in the micrographs.) Sliding has taken place along the boundary between grains A and B unaccompanied by important boundary migration. The sharpness of the offset at the triple point can be clearly seen in grain C. As a result of sliding along the boundary between grains A and B, a new boundary surface between grains A and C was created. The offset at the triple point is about 0.07 mm. This boundary sliding is accompanied by the formation of rather sharp kinking bands and, of course, slip on several slip systems in grain C. This type of deformation has been referred to as fold formation' in previous work with high purity aluminum.

Jan 1, 1957

By Basil B. Zavoico

The World War I1 spread to Russia on June 22, 1941, when the German Armies began their invasion. The Soviet industries, which were already engaged in a tremendous armament program, further accelerated the flow of munitions, and equipment and supplies for all purposes not directly military were either entirely eliminated or reduced to an absolute minimum. With the occupation by German armies of the Dniepr and Kharkov industrial regions, this trend was necessarily further accentuated. The oil industry of Russia, in consequence, was left to rely more and more upon itself, its own very limited manufacturing facilities, extensive repair shops and probably much used equipment out of order stacked in the warehouses. All evidence available to date points to the fact that the new situation not only did not affect the production either quantitatively or qualitatively, but, on the contrary, caused a larger flow of much needed fuels to the country's war machine, primarily by renaissance of both management and labor. The oil industry of the Soviet Union, left to depend entirely upon itself for equip ment and supplies, and even for new workers and technicians to replace those called into the services, did and is still doing a good and effective job. Since it could not hope for new equipment and parts and could not blame any other industry for the delays in delivery, it dragged out old machines from storage and repaired them in its own machine shops. Often such stored and used equipment was but slightly defective, waiting for some small part from factories in Central Russia, plants that now were either in German hands or entirely converted to the manufacture of munitions. More particularly, instead of the pipe that could not be taken to the Caucasus from Central Russia, casing reclaimed from abandoned or submarginal wells was used, or pipe from the abandoned or but slightly used pipe lines; and this practice is being continued even now on a large scale, to create an ample reserve for the duration of the conflict. Indirectly such a development was even an improvement on pre-war days, when many wells about to be completed had to wait for weeks, even months, for the arrival of new pipe, all blame then being placed outside of the industry on the factories in Central Russia. For the purpose of reclaiming equipment and pipe still usable, special crews were organized. The war also caused much quicker adaptation of certain American practices and introduction of many emergency measures, such as: removal of derricks upon completion of wells and the use of drilling equipment mounted on skids for rapid transfer from location to location—both of these practices, while standard in the U.S.A., being new in Russia; installation of simplified surface pumping units; substitution of wooden bearings in the surface pump equipment; completion of wells in the Ural-Volga district, where formations are hard and tight throughout the sedimentary column, without either casing or

Jan 1, 1942

US 4,137,751-Aerial geophysical exploration for ore deposits by collecting and analyzing atmospheric particulates The aircraft has an Inlet duct extending outward and including a "shave-off" duct, a cyclone separator located inside the cabin which is coupled to the inlet duct, a clean air exhaust duct, and a receiver for the collected particles incoming air is divided into two fractions. The fraction taken by the "shave-off" duct and containing the bulk of the particles is routed to the cyclone Particulates are gathered on a collector tape for subsequent analysis and correlation with the areas covered J. R Rhodes, R D. Sieberg, M. C Taylor, J. C Westkaemper, and R C. Young, assigned to Columbia Scientific Industries, Inc Feb. 6, 1979 7 pp. (73-28) Filed- 2-28-75 (554,114) Same British 1,446,760, dated Aug. 18, 1976. US 4,156,138-Exploration for subsurface deposits of uranium ore Pairs of dosimeters are placed underground in a grid pattern Each dosimeter contains a phosphor which IS capable of storing the energy of alpha particles. One dosimeter is heavily shielded from alpha particles, while the other in the pair is thinly shielded to exclude dust After a period underground the dosimeters are heated to release the stored energy as light. The amount of light produced from the heavily shielded dosimeter is subtracted from the amount of light produced from the thinly shielded dosimeter to give an indication of the location and quantity of uranium underground This patent is a division of US Patent No 4,053,772, dated Oct 11, 1977 P E Felice, assigned to Westinghouse Electric Corp May 22, 1979 5 pp (250-253) Filed. 8-12-77 (824,203) US 4,180,727-Method for measuring the gamma-gamma density of uranium ore in the vicinity of a borehole A first gamma-ray detector receives only natural gamma rays from the borehole, while a second receives both natural gamma rays and scattered uranium-source gamma rays The value of the uranium-source gamma rays is calculated. W W Givens, assigned to Mob11 011 Corp Dec 25, 1979 6 pp (250- 264) Filed 10-20-77 (843,909) US 4,180,72&A neutron activation probe for determining the location and grade of uranium ore, especially where thorium or other fissionable isotopes are present, includes a pulsed neutron source in series with a plurality of delayed neutron reactors for measuring radioactivity in a well bore- hole together with a Nal(T1) counter for measuring the high energy 2 62 MeV gamma line from thorium The signal from the Nal(T1) counter IS subtracted from the signal from the delayed source detectors to ascertain the amount of uranium present in the ore body N. P Goldstein and R C Smith, assigned to Westinghouse Electric Corp Dec 25,1979 6 pp (250-264) Filed. 4-1 1-78 (895,323)

Jan 1, 1980

By E. H. Burdick

THE difficulties inherent in table concentration operations as applied to gold, silver, lead and zinc ores, are accentuated in the scheelite mill, which has a flowsheet that is similar in general principles. The narrow "spread" in the specific gravity between scheelite and the usual gangue in which it occurs often makes its clean separation extremely difficult and in some cases impracticable. The problem is further complicated by the extreme friability of the mineral and its inordinate tendency to "slime," particularly where fine grinding is necessary and wet grinding methods are employed. The physical aspect of the occurrence of scheelite in the ores, the kind and character of the rock in which the mineral is present, its hardness, friability and the specific gravity of its constituents, as well as like characteristics of the associated mineral-spyrite, pyrrhotite, sphalerite, and others, all have a bearing on the successful milling of crude ores and the production of a concentrate that is marketable with minimum price penalty or none at all. Most tungsten deposits are considered low grade when the limiting factor of low percentage recovery by gravity methods is borne in mind. The great majority of deposits developed or in process of development carry from 0.4 to 1.0 per cent tungstic oxide. Ore carrying 1 per cent is considered good grade; 0.7 to o.8 per cent, fair, and below that figure, low grade. Steady mill feed averaging upward of 1.0 per cent WO3 is exceptional. Inasmuch as buying specifications demand a 60 per cent WO3 content, the mineral content of the ores as mined must be concentrated to at least that degree. A few companies have constructed chemical plants for the treatment of their complex concentrates and low-grade flotation product, but the smaller operator must rely on table concentration, borrowing the tools and to a large extent the methods of his predecessors in the gold, silver, lead and zinc mills. Whether these are the best tools and methods that can be devised is an open question. Except in rare instances, table concentration, however carefully conducted, does not yield a satisfactory final recovery of the mineral content in headings as indicated by chemical determinations of tungstic oxide content. A saving of 6o to 65 per cent is considered fair, and an average 80 per cent recovery, exceptional. Each scheelite ore body is a separate problem. Details of handling that give best results in one case may not be successfully operative at a property on the same contact zone and but a short distance removed. Supplementary treatment of tailings by flotation may be successful in producing a low-grade concentrate of around 15 per cent W03, which is adapted to further treatment chemically at a given property and entirely unsuccessful at another. This problem constitutes another of the unanswered questions. The following paragraphs relate solely to the beneficiation of scheelite ores by table concentration and supplementary methods.

Jan 1, 1942