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By H. H. Podgurski, H. E. Knechtel

Annealed Fe-Al alloys do not react readily to form AlN when held at 500ºC in NH3-H2 gas mixtures, but do so upon the introduction of dislocatims. Nuclea-tion of the nitride phase occurs on dislocation sites. In turn, the growth of the aluminum nitride particles causes the ferrite phase to yield plastically, generating more dislocations for the nucleation process. The nitride phase extracted from an Fe-2 pct A1 alloy nitrogenated at 500°C was identified as stoichio-metric aluminum nitride with a hexagonal crystal lattice. THIS investigation reveals the role that dislocations play in initiating and sustaining the nitriding reaction in Fe-A1 alloys. As early as 1931 the work of Meyer and Hobrock1 suggested that the initiation of the nitriding reaction could involve a nucleation controlled process. Recently Bohnenka2 depicted the gas-phase nitriding process below 600°C as one of mixed control limited by nitrogen penetration through the surface, by nitrogen diffusion, by aluminum diffusion, and by nucleation of the nitride phase, Fig. l(a). In our research in a comparable alloy (0.57 pct Al) at 575ºC, we have observed a nitrogenation which we feel is better described by Fig. l(b). In the case of a 2 pct-A1 alloy partially nitrided at 500°C we propose the profiles shown in Fig. l(c). For a complete and accurate description of the process, a concentration profile of the dislocation density in the test specimen would be needed. EXPERIMENTAL Nitrogenization was conducted between 500" and 575°C in a variety of NH3-H2 gas mixtures on three Fe-A1 alloys: 1) zone-refined iron + 0.16 i 0.2 pct Al—levita-tion melt, 2) zone-refined iron + 0.57 0.02 pct Al— levitation melt, 3) plastiron + 2 pct Al—melted by induction heating. To demonstrate the effect of dislocations on reactivity, both cold-worked and annealed samples were investigated. All nitrogenation rate studies were conducted gravimetrically with a gold-plated invar balance4 contained in a gas-flow system. To avoid contamination of the specimens in the reaction zone of the system, the reaction chamber was constructed of high-purity dense alumina. The activity of nitrogen was fixed by specific NH3-H2 gas mixtures whose compositions were continually monitored by calibrated thermal conductivity gages and checked by chemical analysis. Variations of ± 0.1 pct NH3 could easily be detected by both methods. Throughout this paper the activity of nitrogen is defined as PN3 /PH23/2 , where PNH3, and Ph2 are partial pressures in atmospheres. Electron transmission, density measurements, and chemical analyses were made on specimens before and after nitrogenating in order to reveal structural and chemical changes. Similar studies as well as X-ray diffraction studies were conducted on nitride extractions from the nitrogenated 2 pct-A1 alloy. These extractions were obtained by the use of an anhydrous bromine-methyl acetate solution which dissolves the iron and leaves the insoluble nitrides as a residue. Hardness profiles were obtained on cross-sections of partially nitrided specimens to demonstrate the extent of nitriding through the thickness of the specimens. RESULTS AND DISCUSSION The nitrogen activity in the NH3-H2, atmospheres was never allowed to reach a level capable of producing iron nitride (Fe4N). Hence, the term nitriding as used in this paper refers only to the formation of aluminum nitride whereas nitrogenation refers to the total uptake of nitrogen regardless of how it is distributed throughout the alloy. The weight increases observed during the initial stage of a nitrogenating treatment are due primarily to the solution of nitrogen in the ferrite phase, particularly when starting with annealed specimens. Because this initial nitrogenation rate in the case of the 0.57 pct A1 alloy, see Figs. 2 and 3(a), was most rapid the weight change that occurred thereafter might be attributed to the nitriding reaction with the exception of a small weight increment due to the irreversible pickup of oxygen by aluminum. The oxygen (<70 ppm) came from traces of H2O and 0, in the hydrogen and ammonia gases. On the basis of discrepancies between total weight increase and the increase in the nitrogen content of the sample as determined by chemical analysis, it was estimated and later established by activation analysis, that as much as 200 ppm of oxygen were taken up by a fully nitrided Fe-0.57 pct A1 specimen at 575°C. Most of the oxygen could have been picked up from the nitriding atmosphere on the surface of the samples during cooling to room temperature. Even 50 ppm of water in the gas phase will become oxidizing to iron before the sample has cooled to room temperature. The lack of reactivity* of these alloys in the annealed

Jan 1, 1970

By AIME AIME

ASIDE from the annual dinner-dance, the two outstanding social events of the Annual Meeting were the dinner- smoker on Monday night and the informal dance on Tuesday night, both of which were held at the Commodore Hotel. Approximately 400 attended the former event, compared with 570 a year ago, and about 250, people were attracted to the dance.

Jan 1, 1933

By R. J. Teitel

The Pb-U system has been investigated by X-ray, thermal, and microscopic analyses. Two pyrophoric intermetallic compounds were found; UPb3 and UPb. The crystallographic structure of UPb3 is reported. A phase diagram was drawn for the system showing three eutectic and one syntectic reaction. AS a result of the interest in uranium metallurgy, the Pb-U system has been investigated. Practically no quantitative data appears in the literature concerning this system. Chips were machined from bars of high-purity uranium obtained from Ames Laboratory and the lead was 99.9 pct high-purity grade from Bel-mont Smelting & Refining Co. The chips were pickled in a dilute solution of nitric acid, washed in water and then alcohol, and dried prior to use for alloy preparation. The lead was simply sheared from the pig with no chemical treatment. Lead and uranium were placed in graphite crucibles and loaded into an induction furnace. In order to insure good alloy formation, the lead was loaded above the uranium to wash the uranium chips into the melt. After the charge was held at the desired preparation temperature for 15 to 30 min, it was allowed to cool in the crucible. The entire melting operation was accomplished in an atmosphere of helium (double charcoal refined grade with no further treatment). The procedure was to outgas the furnace by first evacuating it to 10-% m Hg, admitting helium to 8 psi gage and sealing the furnace off. An optical pyrometer focused on the charge through a hole in the crucible cover was employed for thermal measurements. Usually a 50° to 70°C correction had to be added to the instrument value. The most suitable alloy preparation temperature range was found between 1220° and 1280°C. The reason for this is explained by the phase diagram, Fig. 7. Above this temperature range two liquids separate preventing alloy formation upon cooling at a reasonable rate. On the other hand, below this range the uranium was coated with a layer of both compounds and the rate of reaction was diminished by diffusion processes. The fastest reaction rate occurred in this narrow range of temperature because only UPb coats the uranium and it evidently does not protect the uranium as well as UPb,. Apparatus and Procedures The development of apparatus and techniques was determined by the peculiar properties of the alloys. All the alloys were pyrophoric, and, consequently, the alloys had to be protected from oxidation by handling them in a dry box or inert atmosphere furnaces. Other operations performed outside of this equipment had to be done as quickly as possible. Thermal analyses were conducted in a furnace and arrangement similar to that described by the author.&apos; Graphite crucibles having a thermocouple well in the bottom were used to contain the prepared alloy, while a helium atmosphere protected the melt from oxidation. The furnace was outgassed by pumping a 10-3 mm Hg vacuum until the furnace had been heated to 400°C. Then helium was admitted and the furnace sealed under 8 psi gage pressure. Chromel-alumel thermocouples were used for thermal analysis and the accuracy of thermal measurements was judged to be k 5°C. At first, an attempt was made to use platinum-platinum-rhodium thermocouples, but evidently lead vapors attack it at high temperatures forming low melting alloys. These lead vapors had direct access to the thermocouple because the graphite crucible was porous. A differential temperature control was used to regulate thermal analyses. The thermal gradient across an alundum tube placed between the windings and the crucible was maintained constant by a controller.

Jan 1, 1953

By S. W. Ross

In 1936 a description of the plant (Fig 1) and process employed by the Electrolytic Zinc Co. of Australasia Ltd. for the recovery of zinc from zinc concentrate by the electrolytic process was prepared. † During the twelve years which have elapsed since the preparation of the earlier paper, several major changes in the metallurgy of the process have been introduced. It is the purpose of the present paper to give a general description of these changes and thus to bring up to date the description of the plant and process. Summary The major changes in Risdon practice since 1936 have been: 1. Replacement of two stage roasting by a preliminary roast followed by the flotation of all the leach residue and the roasting of the flotation concentrate. 2. Screening of all calcine fed to the pachucas. 3. Continuous leaching of calcine and improved classification of pachuca discharge. 4. Close control of hydrogen ion concentration during purification for iron removal. 5. Recovery of cobalt as a good grade oxide. 6. Production of part of the zinc output in the form of "four nines" metal (99.99 pct purity). 7. Closer spacing of electrodes thus increasing the potential output of cathode zinc per cell by 50 pct. Changes which are in prospect and for which construction work is proceeding at the present time involve the starting up of: 1. Two suspension roasters. 2. A contact acid plant to produce 150 tons‡ of acid per day and replacing the existing Mills Packard chamber plant. 3. Extra power station capacity to permit greater current flow to existing cell room units. This will increase the output of cathode zinc from about 245 to 290 tons per day. Plans for the future envisage the building of an ammonium sulphate plant, the first unit of which will produce about 50,000 tons per year, and improved treatment of zinc plant residue for the recovery of zinc, lead and other metals. At the end of this paper tables of metallurgical data are presented relating to the year ending June 30, 1948. Details of Changed Practice Output In 1936 the production of cathode zinc amounted to about 200 tons per day. This has since been increased to about 245 tons per day while plant extensions are practically complete which will permit of an output of about 290 tons per day in the near future. Roasting Division ROASTING POLICY A major change has occurred in the roasting policy. Twelve years ago the method in use was to carry out a two stage roast in the first stage of which sulphide sulphur was reduced to about 6 pct. The pre-roast calcine was re-roasted in modified Leggo furnaces using coal as fuel, sulphide sulphur being reduced to about 0.8 pct. The whole procedure was described on pp. 482491 of the earlier paper. Although this roasting procedure had certain advantages it possessed some distinct disadvantages. For instance, it appeared uneconomical to heat up the entire input of pre-roast calcine to roasting temperature by the expenditure of fuel in order to oxidise a few percent of sulphide sulphur. It was argued that if the pre-roast calcine were leached and a process could be developed for the recovery of a zinc sulphide concentrate from the leach residue, this concentrate, small in weight compared with the pre-roost calcine, would probably roast autogenously, thus virtually eliminating the expenditure of fuel as well as greatly increasing the weight of sulphur oxidised per square foot of furnace hearth area. The obvious method of producing a suitable concentrate from leach residue was by flotation. It will be recalled (see p. 495 of the earlier paper) that when two-stage roasting was practised the leach residue was classified, the granular fraction was ground and floated while the slime fraction was thickened, filtered and dried ready for shipment to a lead smelter. This process worked quite successfully. However, when trials were made of leaching a calcine carrying several percent of sulphide sulphur the granular fraction still floated well, but the slime fraction carrying 8-10 pct sulphide sulphur yielded very poor results when subjected to flotation. This fact held up the application of "pre-roast" leaching for many years. However, successful flotation of the slime fraction of leach residue was finally achieved and in August 1940 the slime flotation plant began operation, while the leach-

Jan 1, 1950

By John Hays

AT the December Board meeting, the report of the William Lawrence Saunders Medal Committee, recommending the award of the medal to John Hays Hammond, was received and unanimously approved. The citation is: "For his notable work as an engineer and developer of mines at home and abroad, his industrial leadership and his public services." The medal will be presented as usual during the meeting in February, presumably at the annual dinner at the Waldorf, on Feb. 20. The other medals to be given on the same occasion are the James Douglas, which goes to Paul D. Merica, and the Robert W. Hunt, which is awarded this year to Edgar C. Bain, as already announced. This will be the third award made of the Saunders Medal for "Achievement in Mining," previous recipients having been David W. Brunton in 1927, and Herbert Hoover in 1928. The list is a distinguished one and Mr. Hammond&apos;s name is appropriately included. His career is so widely known that it is not necessary to repeat the account, published in MINING AND METALLURGY last April.

Jan 1, 1929

By K. R. Janowski, A. B. Chase, E. J. Stofel

Ruby crystals of exceptional optical quality have been grown from fluxes composed of Bi2O3 + PbF2 or Bi2O3 + BiF3. Careful control of growth conditions was required to minimize the number of growth defects consisting primarily of dislocations, occluded flux, and growth twins. Slow growth rates coupled with the addition of small amounts of La2O3 as a flux dopant were helpful in producing nearly perfect crystals. Chromium concentrations up to 1 pet were incorporated into these crystals without adversely affecting their perfection. Crystals up to 10 mm in diameter having as few as one to ten dislocations per crystal were typical of those produced under optimum growth conditions. Under these same conditions the occlusions were eliminated, and growth twins were either eliminated or reduced to one to three twin boundaries per crystal. INTEREST in the nature of lattice imperfections produced during the growth of ruby crystals (Al2O3-corundum structure) has been stimulated recently by the need for ruby lasers of good optical uniformity. As a result, ruby crystals grown by the flame-fusion (Verneuil) process have been studied in detail and have been found to contain high densities of dislocations (106 to 107 dislocations per sq cm) and mosaic structures that impair their optical quality.&apos;-3 Attempts to improve the quality of Verneuil-grown crystals by controlling the growth variables have not been entirely successful. On the other hand, rubies grown by the flux process have received little attention even though their more nearly equilibrium growth conditions suggest that they would have fewer growth defects. Nelson and Remeika have shown recently that small flux-grown rubies can indeed be made into very low-loss lasers. However, they did not report information on crystalline imperfections in these crystals.4 Stephens and Alford have reported briefly on defects found in a flux-grown corundum crystal but they neither described these defects in detail nor related them to the method of growth.5 The present investigation was undertaken to establish the relationship between growth conditions and crystalline perfection of flux-grown rubies, sapphires, and other crystals of the corundum family. EXPERIMENTAL PROCEDURE The corundum crystals used in this study were grown by slowly cooling solutions of A12O3 in molten-salt solvents of PbO + PbF2, Bi2O3 + PbF2 or Bi2O3 + BiF3. The materials employed were Linde A (a Al2O3 powder) with reagent-grade chemicals as solvents. Some of the solutions also contained small additions (1 pet or less) of one or more of the transition metal elements chromium, manganese, iron, and titanium as crystal dopants. La2O3 was added to some of the solutions to alter the growth habit of the crystals. The La2O3 promoted the occurrence of growth facets parallel to (0112) and {1011} planes, where the indexing system is the morphological system described in detail by Kron-berg6 and used throughout this paper. The melts from which the crystals were grown were prepared by mechanically mixing the various constituents and placing them in platinum crucibles. The covered 50- and 100-ml platinum crucibles were heated in muffle furnaces at 1250°C for short periods of time (1 to 4 hr) and then program-cooled at either 2° or 4°C per hr to 1000°C. At this lower

Jan 1, 1965

By R. A. Generes, H. C. H. Darley

Laboratory tests showed that at elevated temperatures a reaction takes place between all metal hydroxides and clay muds, which results in a thickening or solidifying of the mud, the extent of which depends on the nature of the ingredients. Calcium hydroxide gave the strongest solidification whereas barium hydroxide only caused a mild thickening, indicating that the use of barium hydroxide muds instead of lime muds would be a good way of preventing high-temperature solidification. It was found possible to prepare barium mud in the laboratory with caustic soda and a thinner in the same manner as lime muds, and these barium muds had the same or better toleration of high solids content, resistance to salt contamination, and low gel strengths as the corresponding lime muds. Three field trials have been made with barium mud. The principal difficulty encountered was in determining the correct proportions of the tourly treatments required to maintain low gel strengths. A satisfactory systern was finally developed, and low gels were maintained throughout the third test. The wells on which the trials were made were not carried deep enough to test the resistance to solidification adequately, but oven tests at 350°F were made periodically and no tendency to solidification was noted except immediately after severe cernent contamination had introduced excessive amounts of calcium into the system. Although barium hydroxide costs considerably more than lime, the total mud costs were as low, and on the last well significantly lower, than the average cost of lime mud wells drilled in the vicinity. INTRODUCTION The advantages of repressing dispersion and hydra-tion of clay cuttings carried in the mud, particularly when drilling through thick clay formations, are well recognized. This repression is generally achieved by the use of lime, and lime muds have in consequence the desirable characteristics of high toleration of solids, low thixotropy, and good resistance to contamination. They have, however, the disadvantage of high-temperature solidification. This phenomenon has been described in detail by Gray et al, who have shown that it is the result of a chemical reaction between the hydroxides and the clay minerals. The work described in this paper was undertaken to find a substitute for lime which would not cause this solidification. LABORATORY EXPERlMENTS The principal positive requirement for a substitute for lime is that it should repress the hydration and dispersion of clay. It is well known that monovalent cations promote hydration while polyvalent cations repress it. Therefore, a few representative polyvalent salts and hydroxides were tested to determine whether they could be used as substitutes for lime. Their efficiency at repressing hydration and dispersion was measured by means of the clay-volume test. It has been shown elsewhere&apos; that this test is a good measure of degree of dispersion of clay in suspension and that hydration accompanies and correlates with dispersion, so that measuring one measures the other. The test is made by centrifuging a 1:100 mixture of mud and 1-N NaCl and observing the volume of sediment—the greater the volume, the greater the dispersion. The tendency to caux solidification was measured by heating the muds in pressure vessels for 16 hours at 150°F and 370°F. An approximate quantitative

Jan 1, 1957

By C. L. HUNTZINGER

THE mine here described is in the Witbank district, a coal area of the Transvaal, about 100 miles north- east of Johannesburg. and is owned by the Witbank Colliery, Ltd. The plant has a capacity of 4000 tons per eight hours, and prepares five sizes of coal. The coal seam lies at a depth of about 200 ft. below the surface, and is reached by an inclined shaft sunk at an angle of 18° with the horizontal. Although the thickness of the coal seam varies from 10 to 14 ft. or more, only about a 7-ft. bench is mined. Mining is by the hord and pillar system. Bords are driven 18 ft. wide, with pillars measuring 18 ft. square. The mine is laid out into four sections, each sewed by a main haulage way from the shaft. Arc-wall machines are used for cutting the coal. but all loading is done by hand. Native labor is employed under the supervision of white miners, who do the required blasting. The workings are practically free from gas and water, and very little timber is needed.

Jan 1, 1931

By H. E. Lee, P. C. Feddersen, D. R. Gittinger, G. W. Dunn, J. B. Schuettenhelm

The new Bunker Hill slag-treatment plant, designed ior, a capacity of 300 to 400 tons of hot slag per day, was "blown in" April 5, 1943. In the ensuing I5-months period, 157,530 tons of slag was processed, with an average recovery of over go per cent of the zinc and practically all of the lead contained. In addition to this high metal recovery, utilization of the waste heat in the gas and fume venting, the process has enabled the generation of 231,376 tons of steam at 250-lb, gauge. Over the first six months opcration the volume of slag treated averaged somewhat under 300 tons per day. Reclaimed dump slag made up only about 1 5 per cent of the plant feed. In October 1943, preparations for the smelting of additional tonnages of dump slag were completed and the plant capacity was increased to an average of about 420 tons of slag per day. During the nine-months interval since that date, monthly averages of 450 toils per operating day have been maintained several times. The new plant (Fig. I) is constructed in close proximity to blast-furnace operations. The fuming furnace and other necessary equipment are housed in an eastward extension of the existing blast-furnace building. Beyond this housed extension the dust-laden gas is conveyed about the perimeter of a large rectangle formed by the flues, cooling towers and baghouses. The course of a 10-ft. balloon flue, which transports the fuming furnace gas, describes the west and south perimeters. This flue connects with a set of cooling towers located at the southeast comer. The flue and cooling-tower system serving the deleading kiln constitute the north side and the two baghouses, serving the kiln and furnace operations, -border the east side. From these baghouses the several discharge gas flows are come biped and conveyed in to the rectangle, being vented to atmosphere by means of a fan through a centrally located zoo-ft. brick stack. In general, the plant design and operation follow quite closely that dictated by experience gained in years of slag-fuming practice by the Anaconda Copper Mining Go., at East Helena, Mont., and the Consolidated Mining and Smelting Co. of Canada, Ltd., at Trail, B.C., and more recently by the International Smelting and Refining Co. at Toocle, Utah. : Fuming operations at the East Helena and the Tooele plants are more or less identical. Trail practice differs chiefly in the methods employed for the storage of the hot feed slag and in the methods utilized for the handling and cooling of the fuming furnace gas. The new Bunker Hill fuming plant closely follows Trail procedure in the treatment of the furnace discharge gas while East Hclcna methods have been adopted for the storage of feed slag.

Jan 1, 1944

By Harrison Everett Ashley

Prof. Hofman&apos;s diagrams, Figs. 5 and 7 of his paper, which are reproduced as Figs. 1 and 2 of the present contribution, confessedly fail to show comprehensively the properties of the silicates investigated. Each curve is carefully discussed, and the author has evidently drawn all the conclusions that can be thus reached; but he says :* "The curves do not show, as was hoped, any simple connection between silicate-degree, percentage of lime, and minimum of formation-temperature." There is, therefore, in this case, an excellent opportunity of

Jan 1, 1902

By G. Y. Chin, M. T. Dolan, W. L. Mammel

We have obtained by computer methods the solutions of the Taylor analysis1 for axisymmetric flow in bcc metals. Four modes of slip have been treated in detail:2-4 (111), {112}(111), {123}( 111), and a mixture of all three. In addition to obtaining anisotropy of strength data for randomly oriented or textured polycrystalline material,4 we have also obtained the lattice rotation resulting from slip on the predicted systems. The patterns of lattice rotation are essential to an improved understanding of texture development during deformation. The present note shows the results of lattice rotation for 5 pct axisymmetric compression, for fifty-two axial orientations distributed at 5-deg intervals throughout the standard stereographic triangle. The data are presented in Figs. 1 to 4 for the four modes of slip. The lattice rotation is indicated by a vector, the ends of which correspond to the positions before and after the deformation. The different vectors emanated from a given orientation represent different combinations of five slip systems that satisfy Taylor&apos;s minimum shear criterion.&apos; Fig. 1 shows the results for {110}< 111> slip. They are similar to those obtained by Bishop5 for the case of (111 )(110) slip in axisymrnetric tension, since in axisymmetric flow the sense of lattice rotation for {111)( 110) in tension is the same as that for (110) (111) in compression. The pattern of lattice rotation may be divided into three regions: region A in which the rotation is toward [100]; region B, toward [lll]; and region C, toward either [ loo] or L lll]. Although some slip combinations in region C lead to [1101, the latter is not stable as continued activity of the same combinations will eventually move the axis toward [loo] or Llll]. It may also be noted that [loo] is itself not stable. However, close inspection of the vectors in region A shows that it is impossible for an axial orientation within A to rotate outside its boundary. Hence after heavy compression, all orientations from A and some from C are expected to form a diffuse band in the [100] vicinity. By far the largest region is B. Here all orientations rotate to [lll], which is a truly stable position. Thus the [111] texture component is expected to be rather sharp. For the case of (112 }( 111) slip, Fig. 2, region C is enlarged at the expense of A, with B about the same as for {110}( 111) slip. A significant difference, however, is that [loo], as well as [Ill], is now truly stable. Fig. 3 shows the results of slip on {123}( 111) systems. Region B is substantially enlarged at the expense of C, with A being intermediate in size between the {110}(111) and {112}(111) cases. Like the case of {110)( 111) slip, [100] is itself unstable. However, the lattice rotations here are confined to less than 5 deg; hence it may be considered "stable" for practical purposes. Finally, Fig. 4 shows the results of mixed slip. Here region B is the largest, and C the smallest, of all the cases considered. Both [loo] and [ill] are stable. The behavior of the three corner positions is, in fact, identical to the case of {112)( 111) slip, Fig. 2; it turns out that in these positions for the mixed slip case, all the active slip systems (based on Taylor&apos;s criterion) belong to pure {112}( 111) .4 In summing up the results for the four modes of

Jan 1, 1968

By Research Staff ? Verde Copper Mines

FLOTATION is now commonly practiced in alkaline ore pulps, yet little is known regarding the action of the alkaline solutions on the ore particles beyond the fact that films of oxidized material form. We wish to chronicle our discovery of the presence of soluble reducing agents in alkaline ore pulps of the United Verde, and present some data on lime consumption. During the grinding and flotation of a pyritic ore containing small amounts of ferrous sulfate and other soluble salts, an excess of lime was added to precipitate the salts, and filtered samples of the solution were titrated with standard permanganate solution. Even in pulps of high causticity an appreciable permanganate titration was always obtained, in spite of the fact that the solutions were shown to contain little iron. Investigation of the cause brought about the discovery of several previously unsuspected compounds in flotation pulps made from pyritic ore. Not only the reducing agents present had to be identified, but also the amount of dissolved oxygen, and a survey was finally made of the free oxygen content and reducing agents of the mill pulp in the concentrating mill at Clarkdale. A great many compounds might form, caused by oxidation of pyrite or other metal sulfides or by reaction between a lime solution and pyrite. The most probable compounds considered were calcium sulfides; polysul-fides, thiosulfates, and polythionates. Later it was discovered in the literature that in alkaline pulp polythionates do not exist and if introduced. are decomposed into sulfites and thiosulfates.1 Any precipitated sulfur is changed by alkali into thiosulfate and polysulfide. Sulfites and sulfides react to form thiosulfate, so that in the end it is possible to have in an alkaline solution only thiosulfate and an excess either of sulfide or sulfite. Confirmatory tests were made and it was finally established that the alkaline mill pulps made from the United Verde ore contained

Jan 1, 1929

By K. D. McBean, W. H. Hannay, B. A. Stimmel

The electrolytic plant at Trail, B. C., was erected by the Consolidated Mining and Smelting Company of Canada, Ltd., for the treatment of zinc ores and concentrates, particularly those of the Sullivan mine at Kimberley, B. C. It began operations in 1916 at a rated capacity of 60 tons of cathodes per day, which has been steadily increased to the present production of 400 tons per day. The Sullivan has furnished the greater part of the zinc so far produced, although notable tonnages of customs zinc concentrates have been treated. The maximum yearly tonnage of customs concentrates, 25,000 tons, was treated in 1926. Practically no customs concentrates hale been treated since 1929. The total bar zinc production to the close of 1935 was 1,092,782 tons. The zinc mineral in the Sullivan ore is marmatite of somewhat variable composition, ranging between 6ZnS.FeS and 8 ZnS.FeS. Practically all the zinc ores tributary to this plant are marmatites; and the iron content of the zinc mineral varies considerably. The formation of zinc ferrite during roasting is now a matter of common knowledge, so the possible extraction from any zinc concentrate is largely a function of the iron content; the progress made in concentration is reflected directly in zinc-plant recovery. The Trail plant operafes on the low-acid system, as do all the other major plants on this continent at present operating, except the electrolytic plant of the Sullivan Mining Co. at Kellogg, Idaho. The new Magdeburg plant, in Germany, occupies an intermediate position between high and low acid. Plant operation at Trail will be treated in this paper under five main sections: roasting, leaching and purification, electrolysis, cadmium recovery and melting. The oxide section of the plant, treating zinc fume from re-treatment of lead blast-furnace slag, is practically a separate zinc plant; this is necessary because of the presence of fluorine in the smelter zinc fume. Cadmium is recovered electrolytically from the purification residues of both the sulphide and oxide leaching plants.

Jan 1, 1937

By E. Keller

Some years ago the writer&apos;s attention was called to the fact that rolling-mill scales from auriferous copper do not have the gold content proportional to the gold contained in the copper from which they are derived.&apos; So, later, he made a few simple experiments, which are described herewith. In order to test the gold movement on the changing surface of a copper plate under the influence of oxidation, plates 6 in. by 8 in. by 1 in. (15.2 cm. by 20.3 cm. by 2.5 cm.) of converter copper, refined, of 99.29 per cent. purity, and leaded copper with a content of 95.65 per cent, copper, were obtained. Ten cuts were made through the thickness of the plates along the longitudinal center and the silver and gold content ascertained in each of the 10 samples in both plates, as shown in the accompanying illustration. The assay results, recorded in Tables 1 and 2, show that the gold distribution is relatively uniform in both plates, while silver has greater variations, especially in the leaded plate. The plates subjected to oxidation were placed in a red-hot muffle for about 2 hr., two small scarifiers being used as supports. Arranged alongside each other, they nearly filled the width of the muffle, and so were practically under equal conditions of heat and draft. The accurate observance of the time was not possible, however, because of other work, but the time of the exposure of each plate in a pair was identical. At the end of each period, each plate was plunged into water and completely freed of scale, which was carefully collected, dried, weighed, and analyzed. Samples of the plates had also been taken of the molten metal and duly analyzed. Table 3 contains the analytical data for the two plates and their several sheets, or layers, of oxide scales. These figures show that in the oxidations of the converter copper the silver is fairly uniform, while the gold is highly irregular and especially low in the first layer. In the oxidations of the leaded copper plate, the silver and gold contents are variable; however, this irregularity is due to two different causes. The

Jan 1, 1919

By Felix E. Wormser

REGISTRATION started bright and early Monday morning in the Silver Corridor at the Waldorf-Astoria with Mrs. W. H. Bassett as chairman. What a registration-over 200 ladies! Several joined us from as far away as California and Washington State. Apparently they enjoy our meetings so much that present travel inconveniences didn&apos;t discourage their coming. At noon the ladies joined the men at the All-Institute Luncheon and Monday evening we had our informal dance, which is separately reported. Tuesday morning was devoted to our annual meeting at which all Section annual reports were read. At noon we were all the guests of the W.A.A.I.M.E. at a luncheon at the Port Arthur Restaurant on Mott St. in Chinatown. Many of us rode down on the old 3d Ave. elevated railway-the last of four. It, too, is soon to be torn down. The luncheon was delightfully unusual, with huge dishes of delicious Chinese food on each table. Our chairman, Mrs. Read, who lived in China in her youth chose our menu, and she chose it well, for most of us indulged so heartily that as we arose from the table we felt we couldn&apos;t eat again for 24 hours. Someone donated sherry wine, and boxes of Chinese pencils as favors. We wonder who? All owe a big vote of thanks for this lovely party to Mrs. T. T. Read and Mrs. H. A. Prosser, chairmen, and Mrs. H. W. Hardinge, Mrs. R. Hursh, and Mrs. R. L. Lloyd, vice-chairmen.

Jan 1, 1944

By Jean Howard

RECENT attempts to produce secondary recrystalli-zation in high-purity iron have given conflicting results. Coulomb and Lacombe1&apos;2 did not find it but Dunn and Walter3,4 did. The latter workers have stated that (100) [001] and/or (110) [001] orientations develop depending on the oxygen content of the annealing atmosphere. This Technical Note records results which are in agreement with Dunn and Walter in so far as it shows that secondary recrystallization can be produced in high-purity iron, but does not confirm that both types of orientation are obtainable. Similar observations have been made on chromium-iron and molybdenum-iron, although when this technique is used on 3 1/4 pct Si-Fe, both types are obtained as in the work of Dunn and alter.&apos; Pure iron strip was cold-rolled from sintered compacts prepared from Carbonyl Iron Powder-Grade MCP of the International Nickel Co. (Mond) Ltd. The powder contains about 0.5 pct 0, 0.01 pct C, 0.004 pct N, (0.002 pct S, $0.005 pct Mg and Si, and 0.4 pct Ni—that is, it is substantially free from metallic impurities other than nickel, which is thought to be unimportant in the present work. The iron powder was (a) pressed at 25 tons per sq in. into blocks measuring 3 by 1 by 0.3 in., (b) deoxidized in hydrogen (dewpoint -60°C) by heating first at 350°C and then at 600° C until the dewpoint returned to -60°C at each temperature and (c) sintered in hydrogen (dewpoint -40°C) at 1350°C for 24 hr. (when dewpoint is referred to in this Note, it is the value as measured on the exit side of the furnace). The sintered compacts were cold-rolled to 1/8 in., annealed in hydrogen (dewpoint -60°C) at 1050°C for 12 hr and cold-rolled to 0.004, 0.002, and 0.001 in. with inter-anneals at 900°C for 5 hr and a final reduction of 50 pct. Final annealing of strip between alumina or silica plates at 875" to 900°C in hydrogen with dewpoints of -20°, -55" and -80°C produced secondary grains with the (100) in the rolling plane; the extent of secondary recrystallization was greatest when the dewpoint was -55°C. Annealing in a vacuum of 2 x 10"5 mm Hg at the same temperature produced no secondary recrystallization at all. With strip thicker than 0.002 in. very few secondary crystals developed whatever the conditions of annealing. Using a processing schedule somewhat similar to that described above, secondary recrystallization was produced in two bcc alloys of iron, viz. 80 pct Fe + 20 pct Cr and 96 pct Fe + 4 pct Mo. The former was reduced to final thicknesses of 0.001 to 0.004 in. and the latter to final thicknesses of 0.001 to 0.016 in. With the chromium-iron, a final anneal at 1250°C (found to be the most effective temperature for developing secondary crystals in the 0.004-in material) with a dewpoint of -25°C produced a greater degree of secondary recrystallization than with dewpoints of -50°C or -20°C. Secondary crystals developed in strips of all thicknesses from 0.001 to 0.004 in. Final annealing in vacuum produced no secondary crystals at all. For the molybdenum-iron a temperature of 1200°C was most effective. It was found that a dewpoint of -50°C during the final anneal gave better results than a dewpoint of -25 "C on the 0.008 in. material. Final annealing in vacuum gave slightly worse results than annealing in hydrogen with a dew-point of -50°C. Secondary crystals were developed in strips of all thicknesses up to 0.008 in. The experiments show that the extent of secondary recrystallization is a maximum for certain critical values of oxygen content of furnace atmosphere and annealing temperature, and that these values are different for different alloys. The thinner the material, the less critical these values are. The general conclusions are that secondary recrystallization can be obtained in high-purity iron, chromium-iron, and molybdenum-iron, using a processing schedule similar to that which will cause the phenomenon to take place in high purity 3 1/4 pct Si-Fe. Unlike the silicon-iron, however, only the (100) (0011-- orientation has been produced in these alloys, irrespective of the temperature of final annealing and the oxygen content of the furnace atmosphere. The information used in this Note is published by permission of the Engineer-in-Chief of the British Post Office.

Jan 1, 1962

By V. J. Decarlo, J. J. Gilman

POLISHING pure zinc differs somewhat from polishing less reactive metals. The problem is not that of finding a suitable reagent, but rather of producing the polish in such a way that the surface remains polished after it is removed from the polishing bath. In other words., the anodic film that is vital to the polishing mechanism&apos; must be tightly adherent and nonporous. It is usually desirable that it be thin. Polishing solutions consist of proper proportions of an acid and a strong oxidizing agent. In electro-polishing, the external circuit acts as the oxidizing agent. The proportions are critical because the essential surface film must be maintained at approximately constant thickness during the polishing process. In the case of zinc, chiefly two oxidizing agents, chromic and nitric acids, have been used. The simplest polishing reagent is concentrated nitric acid. However, it has certain disadvantages. It tends to pit: an excessive amount of heat is evolved during polishing; and the oxide film that it produces is not very stable, so that the polished sur-

Jan 1, 1957

By Clarence Zener

The internal friction of nonferrous metals vibrating at low stress amplitudes has so far always been successfully interpreted in terms of inhomogeneities of one sort or another. Examples are the fluctuation of stress across a specimen vibrating transversely,1,2,3 the stress inhomogeneities due to the elastic anisotropy and partial random orientation of the individual crystallites, localized weak regions introduced by cold-working,6&apos;7 grain boundaries and possibly twinning planes.8&apos;9 Perfect single crystals are, by definition, homogeneous. Actual single crystals usually, perhaps always, contains some imperfections. The present investigation was undertaken to determine whether the internal friction of single crystals may likewise be attributed to inhomogeneities. This study was made possible through the gift of a large single crystal of 70-30 alpha brass by H. L. Burghoff, of the Chase Brass and Copper Co. The specimen, 3.i in. in diameter and 10 in. long, was similar to samples previously described by Mr. Burghoff. Experimental Method The experimental method used has previously been described in institute papers.5&apos;6&apos;9 The measure of internal friction adopted here, I/Q, is X the logarithmic decre- ment, a measure used by some writers, and is also X the specific damping capacity, a measure used by other writers. In all measurements the stress level was kept so low that the measurements were independent of stress level. In all measurements in which the temperature was varied, observations were made as the specimen slowly cooled from its highest temperature. The specimen was vibrated transversely. Observations were made at the fundamental frequency and at the first overtone, of about 620 and 1710 cycles per second, respectively. No attempt was made to avoid acoustical losses. Experimental Results The specimen was annealed for several hours at 450°C. The temperature dependence of the internal friction was then determined from room temperature to 400°C. As shown in Fig. I, the internal friction increased by only a factor of 2 from room temperature to 300°C., then by a factor of 100 during the next Ioo° interval. These measurements are consistent with the view that the observed internal friction is the superposition of two distinct parts. One, dominant at room temperature, is nearly independent of temperature. This part may be accounted for by acoustical losses and by transverse thermal currents. It was not further investigated. The second part, when plotted in the manner of Fig. I, lies upon a straight line. Therefore it has a heat of activation H; i.e., it varies with temperature as Internal friction e-H/RT [I]

Jan 1, 1943

By Clarence Zener

The internal friction of nonferrous metals vibrating at low stress amplitudes has so far always been successfully interpreted in terms of inhomogeneities of one sort or another. Examples are the fluctuation of stress across a specimen vibrating transversely,1,2,3 the stress inhomogeneities due to the elastic anisotropy and partial random orientation of the individual crystallites, localized weak regions introduced by cold-working,6&apos;7 grain boundaries and possibly twinning planes.8&apos;9 Perfect single crystals are, by definition, homogeneous. Actual single crystals usually, perhaps always, contains some imperfections. The present investigation was undertaken to determine whether the internal friction of single crystals may likewise be attributed to inhomogeneities. This study was made possible through the gift of a large single crystal of 70-30 alpha brass by H. L. Burghoff, of the Chase Brass and Copper Co. The specimen, 3.i in. in diameter and 10 in. long, was similar to samples previously described by Mr. Burghoff. Experimental Method The experimental method used has previously been described in institute papers.5&apos;6&apos;9 The measure of internal friction adopted here, I/Q, is X the logarithmic decre- ment, a measure used by some writers, and is also X the specific damping capacity, a measure used by other writers. In all measurements the stress level was kept so low that the measurements were independent of stress level. In all measurements in which the temperature was varied, observations were made as the specimen slowly cooled from its highest temperature. The specimen was vibrated transversely. Observations were made at the fundamental frequency and at the first overtone, of about 620 and 1710 cycles per second, respectively. No attempt was made to avoid acoustical losses. Experimental Results The specimen was annealed for several hours at 450°C. The temperature dependence of the internal friction was then determined from room temperature to 400°C. As shown in Fig. I, the internal friction increased by only a factor of 2 from room temperature to 300°C., then by a factor of 100 during the next Ioo° interval. These measurements are consistent with the view that the observed internal friction is the superposition of two distinct parts. One, dominant at room temperature, is nearly independent of temperature. This part may be accounted for by acoustical losses and by transverse thermal currents. It was not further investigated. The second part, when plotted in the manner of Fig. I, lies upon a straight line. Therefore it has a heat of activation H; i.e., it varies with temperature as Internal friction e-H/RT [I]

Jan 1, 1943

By R. G. Davies

The activation energy for steady state creep above -500°C is observed to be independent of the applied stress although it varies from -67 kcal per mole at 2 at. pct Si to -100 kcal per mole at 11 at. pct Si due to changes in crystallographic order. The magnitude of the activation energy, by comparison with Fe-A1 alloys, indicates FeSi type of order in certain alloys. X-ray results confirmed the presence of FeSi type of order. It is proposed that dislocation climb is the rate controlling mechanism for all the alloys. It has been demonstrated that when a diffusion mechanism is the rate controlling process, the formation of a superlattice in brass,1 Fe3A1,2 Ni3Fe,3-5 and Feco6 1) increases the creep resistance, and 2) increases the activation energy for steady state creep. Furthermore, a study of creep in Fe-15 to 20 at. pct A1 alloys7 has revealed that as the alloy composition approaches the long-range order field, there is an increase in the activation energy for steady state creep which is thought to be due to an increase in short range order. Fe-A1 and Fe-Si alloys are similar in that they both form the DO3 superlattice in which aluminum or silicon atoms have only iron atoms as first and second nearest neighbors. There are, however, two important differences between the alloy systems: 1) The superlattice formation at -350°C commences at -10 at. pct si8 as compared to -20 at. pct Al,9 and 2) Fe-A1 alloys form a FeAl (B2 type) super-lattice where aluminum atoms have all iron first nearest neighbors even at 22 at. pct Al, but so far no similar FeSi superlattice has been observed. With the similarity between Fe-A1 and Fe-Si alloys in mind, alloys of iron with 2 to 11 at. pct Si were examined for variations with composition of the activation energy for steady state creep and of creep strength. The temperature range of greatest interest was above 1/2 TM (TM is the absolute melting temperature) where it is usually observed that diffusion is the rate controlling process. A subsidiary X-ray investigation of the Fe-Si system was undertaken in an attempt to define the position of the order-disorder boundary as a function of cooling rate. EXPERIMENTAL DETAILS a) Creep. Specimens whose gage length was 1.5 in. and with a cross-section 0.04 by 0.08 in. were strained in tension by a lever-arm arrangement, and the load was adjusted between each creep test to maintain constant stress. The apparatus and mode of operation have been fully described in a previous publication.7 As each test produced a creep strain of 0.25 pct, the variation in stress during the test was negligible. Creep strain was measured at the end of one of the alloy steel grips by a displacement transducer with the out-of-balance potential being recorded on a variable speed recorder. The full-scale deflection of the recorder could be varied in steps to give limits of sensitivity of between 0.1 and 0.001 pct creep strain. The alloys, Table I, were made available by the Metallurgical Department, National Physical Laboratory (N.P.L.), england,10 and by the Research Department, General Electric Co. (G.E.), Schenectady, N.Y. They were hot worked at -850°C, warm worked at 550° to 650°C, and recrystallized in vacuum at -750°C to give a grain diameter of -0.1 mm. All the alloys had a very low impurity content; those from the N.P.L., for which a complete analysis is available,&apos;&apos; show carbon less than 0.026 pct, manganese less than 0.006 pct, and oxygen plus nitrogen less than 0.0024 pct. b) X-ray Procedure. A General Electric XRD-5 X-ray set with a focussing lithium fluoride mono-chromator in the diffracted beam, and a pulse height analyzer to eliminate harmonic wavelengths of the cobalt radiation, was used to investigate the structure of several very fine grained (grain diameter <.01 mm) Fe-Si alloys after the following heat treatments: 1) Quenched from 700°C, 2) slow cooled from 650°C (-40°C per hr), and 3) very slowly cooled from 400° to 100°C (10°C per hr with a 24 hr anneal every 100°C). The method of obtaining the diffraction pattern over the range of 20 from 15 to 45 deg was to count for at least 100 sec every l/3 deg with a slit subtending 1 deg in 20 at the focus; the probable counting error was less than 2 pct.

Jan 1, 1963