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By W. J. Carlson, I. Iwasaki

A previous article reported a combination process for recovering both metallic iron and metallic manganese from the manganiferous iron ores of the Cuyuna Range in Minnesota.' In this process, the iron was recovered by direct reduction and magnetic separation and the manganese was recovered from the nonmagnetic tailing by leaching and electrolysis. The current efficiency during the electrolysis of manganese is quite low, in the range of 60 to 70%, due to the simultaneous plating of hydrogen.2,3 The parameters that affect the current efficiency are (1) the concentrations of the manganese ion and the ammonium sulfate buffer, (2) the effect of autoxidant, (3) temperature, (4) pH, and (5) current density. To study the plating characteristics of manganese metal.

Jan 1, 1969

By AIME AIME

IN A STATEMENT summarizing general conditions in the Federated American Engineering Societies, the executive secretary, L. W. Wallace, expresses the belief that the Federation has made substantial progress. At the annual meeting of the American Engineering Council, to be held in Washington Jan. 5 and 6, this progress will be shown by reports covering activities in many fields. "Unquestionably," says Mr. Wallace, "the Federa¬tion has made favorable and permanent contacts in Washington. Through the, activities of Congress and of the new Federal administration. we have had the opportunity to render some really constructive service. We feel, however, that the great body of engineers are not adequately informed of the organization of the Federation, of its aims and purposes and of its activities.

Jan 1, 1921

The Pennsylvania State College, Mineral Industries Experiment Station, State College, Pa For publications address the Director The Pennsylvania State College through the Minerals Research Experiment Station has issued 10 Bulletins and three Technical Papers, from which the following have been selected as of greatest interest to mining engineers and geologists: Bulletin 1, An investigation of the properties of smitliing coals (1922), free; 2, Petrography of the Mica Pendotite Dike at Dixonville (1926), free; 4, The Helderberg Group from cen¬tral Pennsylvania to southwestern Virginia (1929), 25 cents, 5, Bentonite in Pennsylvania (1929), 10 cents, 6, Production data on Appalachian oil fields (1930), free; 8, Oil field waters of Pennsyl¬vania (1930), free; Technical Paper 2, Condition of water in coals of various ranks.

Jan 1, 1933

By AIME AIME

THE Petroleum Division held a very successful meeting in Los Angeles, Oct. 4 and 5. The meeting was held on the eighth floor of the Chamber of Commerce building, the first day being devoted to technical sessions. Seventy-five members were registered before the opening of the first session. Glenn D. Robertson, vice-chairman of the local section, opened the meeting and introduced Edwin Higgins, managing director of the California Oil and Gas Association, who gave an interesting talk on the recently enacted gas conservation law in California. He explained that the law is an experiment which will be watched with a great deal of interest. The purpose of the law, which went into effect on Sept. 1, is to curb wastage and over-production of gas,

Jan 1, 1929

By Freeman Bishop

Quietly picking his way through the thorny thicket of conservation issues is William E. Ruckelshaus, director of the Environmental Protection Agency in which President Nixon gathered the various anti- pollution units from the Interior, Commerce. Agriculture and Health. Education and Welfare departments. Mr. Ruckelshaus. EPA's first administrator, moved over from being Assistant Attorney General in charge of the civil division at Justice to this new post. Essentially, EPA is charged with administering swiftly proliferating antipollution programs. This means policing industry cities, farms and everything else. Ruckelshaus has been quietly fitting together the various pieces of this new agency, pulling then1 out of other Federal departments. Some 5800 employees are involved. The budget in 1971 for these segments will total about $1.5 billion.

Jan 1, 1971

Sept. 3-8, AIME, Fall Meeting, Industrial Minerals, Minerals Beneficiation, Mining, Geology, & Geophysics, Iron and Steel, and Coal Div., Palmer House, Chicago. Sept. 3-13, AIME, Chicago Section, Centennial of Engineering, Chicago. Sept. 5-8, Engineers' Council for Professional Development, annual meeting, Hotel Sheraton, Chicago. Sept. 11-13, American Institute of Chemical Engineers, Palmer House, Chicago, Ill. Sept. 13, Columbia Section, AIME, Canadian Institute of Mining and Metallurgy, joint all-day meeting, Metaline Falls, Wash. Sept. 18, AIME, Utah Section, Newhouse Hotel, Salt Lake City. Sept. 20, Colorado Section, AIME, Denver. Andrew Fletcher, speaker. Sept. 22-25, American Mining Congress, Metal and Nonmetallic Mining Convention and Exposition, public auditorium, Denver. Sept. 23-25, Institution of Mining and Metallurgy, symposium on mineral dressing, Royal School of Mines. London.

Jan 1, 1952

Nov. 4, 1952, AIME, Morenci Sub-section, Longfellow Inn, Morenci, Ariz. Nov. 5, AIME, Chicago Section, Chicago Bar Assn., Chicago. Nov. 8-8, New Mexico Mining Assn. and International Mining Days, joint convention, Alvarado Hotel, El Paso. Nov. 7, AIME, Pittsburgh Section, National Open Hearth Steel Committee, off-the-record meeting, Hotel William Penn, Pittsburgh. Nov. 7-8, Birmingham Technical Meeting of Southeast Section, AIME, Birmingham. Nov. 10-11, Eighth Annual Meeting of The Magnesium Assn., Hotel Biltmore, New York City. Nov. 12, AIME. Connecticut Section, Hartford, Conn. Nov. 18, AIME, Buffalo Section, National Open Hearth Steel Committee, Hotel Statler. Buffalo. Nov. 19, AIME, Connecticut Section, Hartford, Conn. Nov. 19, American Mining Congress Coal Div. Conference, Wm. Penn Hotel, Pittsburgh.

Jan 1, 1952

By David S. Butts

The high cost of energy has made many solution mining corporations turn from fuel consuming evaporators to solar energy and solar ponds. The generally held concept of a solar pond is an area enclosed by dikes into which brine is pumped, water evaporated by the sun, and the resulting salts scraped from the bottom of the pond. This paper will show that solar ponding is not simple. It is a science involving six main areas. These areas are (1) land conditions, (2) meteorology, (3) fresh water, (4) accessibility, (5) manpower and (6) mineral resources. Each area is discussed to identify important parameters that must be investigated before the viability of a solar pond complex can be established as a mineral recovery step.

Jan 1, 1985

By A. F. Crawley

THIS communication reports measurements of the densities of dilute liquid alloys of 0.1 and 0.5 pct Ag in Sn over temperature ranges of 170" and 210°C, respectively, above the melting point of pure tin (232°C). The work was earried out to provide accurate density data for some liquid diffusion studies performed by Davis.1 Densities were measured using a pycnometric technique established in this laboratory. Earlier papers2, 4 attest to the accuracy of ±0.05 pct and the reliability of the method. Tin, 99.999 pct pure, and silver 99.99 pct pure, were melted in a graphite crucible in a vacuum furnace and held at temperature for 10 hr to ensure homogenization. Ingots suitable for machining

Jan 1, 1970

By Charles L. Elliot

Worldwide manpower utilization reached a new high at 10,482 professional man-months and expenditures increased to $19.9 million for mining geophysical activity during 1965. This is up from 9323 man-months and $14.5 million in 1964. Worldwide geophysical activity measured in percent distribution of the total manpower utilization and expenditures is presented in the accompanying Figs. 1 and 2. In terms of the total manpower utilization, ground surveys accounted for 61%, airborne surveys 18%, and mining geophysical research activity 21%. For expenditures, the breakdown was ground surveys, 49%; airborne surveys, 3901o; and research, 12%. Industry was responsible in general for 74% of the manpower utilization and 80% of the expenditures. Manpower costs in 1965 averaged $1900 per professional man-month.

Jan 11, 1966

By Per-Martin Sandgren, Alrik Anttila

LKAB's ores have specific mineralogical properties that make them especially suitable for the production of supergrade concentrates. Conditions are particularly good for this purpose at Malmberget, where a concentrate for high-purity sponge iron production has been produced for many years. This product assays approximately 71.5% Fe and 0.20% SiO2. Potential exists for still further improvement. In recent years, the production of fractioned concentrates has been started. The material lies within the size range 74-125 µm and the approximate chemical analysis is 71.4% Fe and 0.30% SiO2. Other special products are under discussion. Malmberget ores are also suitable for the production of high- purity direct reduction pellets with a SiO2 content below 1%.

Jan 1, 1983

By E. H. Wells, A. Andreas

Greater progress than in any previous year was accomplished by the oil industry in New Mexico in 1936. The total number of completions in the state was 631, of which 549 were oil wells, 21 were hydrocarbon gas wells, three were carbon dioxide gas wells, and 58 were dry holes. The total oil production for the year was 26,804,446 bbl. Compared with the production for 1935 of 20,228,947 bbl., this represented a gain of 32.5 per cent. Of the total production, 25,337,382 bbl. came from Lea County. The average daily nonmarginal well allowable for that county was 115 bbl. the first of the year and 86 bbl. at the close. Production was regulated by the New Mexico Oil Conservation Commission,

Jan 1, 1937

By Walter L. Crow

MUCH has been published on highly technical phases of grinding. Very little has been written on how a mill man can improve his operations by determining the optimum size assortment of grinding balls that should be added as a makeup charge. This ball rationing is not to be confused with the ball ration used as an initial charge when the mill is started up. Ball rationing is considered for one or more of the following purposes: 1) to increase throughput of the mill, 2) to reduce the power required per ton of ore ground to the desired size, 3) to reduce steel consumption per ton of ore ground, 4) to improve product size, and 5) to lower retention time of ore in the mill.

Jan 7, 1957

By Cyril Stanley Smith

The following table, which is composed of data given in the author's first paper on the thermal conductivity of copper alloys1, contains tile results which have been obtained by previous workers on the thermal conductivity of the copper-tin, the copper-phosphorus and the copper-tin-phosphorus alloys (the phosphor bronzes). a Dr. Ing. Diss., Aachen, 1909. Quoted by Schenk: Ann. der Phys. (1910) 32, 261. b Beibl. Ann. der Phys. (1906) 29, 178. c Jnl. Inst. Metals (1928) 39, 375. d Jnl. Inst. Metals (192.5) 34, 43. e Ges. Abhand. Kennt. Kohle (1919) 4, 400. Experimental Methods Since the method of obtaining measurements of the thermal conductivity was identical with that described in the author's previous paper

Jan 1, 1931

By Roger K. Clifford, Gary W. Hudiburgh

The amine flotation of feldspar from a magnetite concentrate produced at a domestic concentrator was investigated using zeta potential measurements, Hallimond tube flotation tests, and laboratory-scale flotation tests. The point of zero charge of six feldspars (microcline, orthoclase, albite, anorthite, anorthoclase, and oligoclase) range from pH 1.4 to 2.5. Hallimond tube flotation tests using amine flotation reagents were performed on these feldspars and on gangue material (quartz, albite, and microcline) from the magnetite concentrating plant. Laboratory-scale (623 g and 2500 g) flotation tests were performed on the magnetite concentrate to float the feldspar. The effects of three different collectors, two levels of collector concentration, three pH levels, starch, HF acid and regrind were investigated.

Jan 1, 1977

By A. U. Seybolt, J. L. Walter

The effects of the addition of 0.5 pct ThO2 (by volume) on the grain structure and texture of heavily rolled tungsten sheet were studied. Powder metallurgy ingots were rolled to sheet, 0.001 in. thick, and samples were annealed at temperatures from 1200" to 2500°C. The heating rate to the anneal temperature was varied from 3°C per min to 6500°C per min. The orientations of the largest grains were determined by X-ray diffraction. The disposition and loss of the ThO2 particles were determined by electron transmission microscopy and the activation energy for remozlal of the thorium was measured by mass spec-troscopy. Heating rates below about 800 C per min produced large, highly elongated grains. Higher heating rates produced much smaller, less elongated grains. The grain structure and texture of the slowly heated samples were identical to the structures and textures of heavily rolled tungsten foil conventionally doped with aluminum, silicon, and potassium but the recrystallization temperature was about 200°C lower. There was stringer-like dispersion of larger ThO2, particles superimposed on a uniform dispersion of fine particles. The particles increased in size and decreased in number with time at temperature. The loss of particles was accompanied by formation of grain boundary voids and surface pits. The activation energy for removal of the ThO2 was about 40 kcal per mole. THE addition of small amounts of aluminum, silicon, and potassium to tungsten has a profound effect on the grain structure of heavily rolled sheet1 or drawn wire."4 Thus, "doped" tungsten sheet, rolled to 0.001 in. and recrystallized, develops a structure consisting of large, highly elongated grains of a specific preferred orientation.' It has been shown that the elongated grain structure was caused by a dispersion of particles, identified as mullite (Al6si2O13),1,4 in strings parallel to the rolling direction in sheet or to the wire axis. Identical results were obtained for iron which was doped with glass and rolled to 99 pct reduction of thickness and recrystallized.5 Again, the glass particles were disposed in strings parallel to the rolling direction. The strings retarded boundary migration in the lateral direction but grain growth was able to proceed relatively unhindered along the direction parallel to the strings.1,5 In both the doped tungsten and the glass-doped iron, the particles were highly plastic during the high-temperature deformation. Since mullite melts at about 1800°C and the glass employed melts at about 810ºC, the particles were probably molten during the recrystallization anneals (above 1800°C for the doped tungsten and 850°C for the glass-doped iron). There are indications in the literature that particles not plastic at hot-working temperatures (up to about 1550°C for tungsten) may also impart elongated grain structures by primary recrystallization of worked alloys. Examples are dispersions of tantalum carbide in chromium,6 and ThO2 in nickel where elongation ratios of recrystallization grains of up to 20:l were obtained.7 Strings of ThO2 particles in W-ThO2 wire have been seen by Rieck.8 In view of the available evidence, it was of interest to extend the previous studies of doped tungsten and glass-doped iron to include W-ThO2 sheet materials. Of specific interest was the grain structure, preferred orientation, recrystallization temperature, and disposition of the thoria particles. EXPERIMENTAL PROCEDURE A) Material Preparation. About 380 g of blue tungsten oxide (approximate composition WO3) was wet with a sufficient amount of aqueous solution of Th(N03)4 to provide 0.5 vol pct ThO2. The wet mixture was stirred to distribute the doping material uniformly throughout the powder. Stirring was continued while the mixture was heated until it was completely dry. The dried, doped mixture was then reduced to tungsten powder by heating at 850°C for 2 hr in a stream of dry hydrogen. The doped tungsten powder was hydropressed in a rubber sack at pressures of 50,000 psi to produce an ingot approximately 2 cm diam by about 5 cm long. Next, the pressed cylinder was heated in hydrogen for 2 hr at 1350°C to render it strong enough for machining. The cylinder was machined to a square cross section of 1.6 by 1.6 cm with rounded corners. Finally, the bar was heated for 2 hr at 2150°C in hydrogen to provide a sufficiently dense mate rial to withstand the hot-rolling operation. Prior to rolling, the ingot was reduced in thickness by about 20 pct by forging at 1550°C. This served to increase the density of the material and to widen it slightly for better rolling characteristics. The forged ingot was then rolled at 1550°C to a reduction of 45 pct of thickness, following which the rolling temperature was reduced to 1300°C and the slab rolled, with several reheats, to 0.050 in. Further reduction was accomplished at 800°C in tungsten sheet packs to a total reduction of about 99.85 pct. B) Annealing Treatment and Observation of Structure. Small samples of the rolled foil were annealed in one of two ways. Some of the samples were suspended in a covered tungsten can and annealed at temperatures from 1200" to 2200°C for various times in vacuum of l0-7 to 10-6 mm Hg. The can was heated by induction and temperatures were determined by optical pyrometry

Jan 1, 1970

By E. T. Turkdogan

The activity of sulfur was determined as a function of composition of ferrous sulfide by equilibrating with hydrogen sulfide-hydrogen gas mixtures at 670° , 800°, and 900". The present results supplement the available data over the composition range from 36.6 to 39.5 pct S. The X-ray lattice spacing measurements made are in accord with the available data and indicate that the limiting composition FeSl.008 may be taken for the iron-iron sulfide equilibrium. The growth rate of ferrous sulfide on iron was measured by reacting iron strips or blocks in hydrogen sulfide-hydrogen gas mixtures. Owing to the slow approach to equilibrium between the gas phase and the surface of the sulfide layer, The sulfidation experiments were carried out for several days. It is shown that the growth rate ullimately proceeds in accordance wilh the parabolic rate law. From the parabolic rate constants and the thermodynamic data on iron sulfide the self-difiusivity and chemical diffusivity of iron in ferrous bisulfide are evalualed. The self-diffusivity of iron thus derived zs found to increase with increasing sulfur content. THE ferrous sulfide known as "pyrrhotite" is a non-stoichiometric phase having a wide composition range from about 50 to about 58 or 60 at. pct, depending on the sulfur activity. RosenQvistl studied the thermodynamics of this phase over wide ranges of temperature and composition. Hauffe and Rahmel' and Meussner and ~irchenall~ studied the parabolic rate of sulfidation of iron in sulfur vapor. By using markers, these investigators showed that the iron cations were the predominant diffusing species in iron sulfide. This is confirmed decisively by the self-diffusivity measurements of condit4 who showed that the self-diffusivity of sulfur in ferrous sulfide is several orders of magnitude lower than the self-diffusivity of iron. Although much has been learned from these studies about the Fe-S system, further research on this subject was considered desirable for better understanding of the physical chemistry of iron sulfide. This work was confined to the study of the kinetics of sulfidation of iron in hydrogen sulfide-hydrogen gas mixtures. The results of this study are given in two consecutive parts. Part I, the present paper, is on the parabolic rate of sulfidation of iron and the diffusivity of iron in ferrous sulfide. The second paper, Part 11, is on the kinetics of the surface reaction between hydrogen sulfide and ferrous sulfide. EXPERIMENTAL Three types of experiments were carried out: i) equilibration of ferrous sulfide with gas of known E. T. TURKDOGAN, member AIME, is Manager,Chemical Metallurgy Division, Edgar C. Bain Laboratory for Fundamental Research, U. S. Steel Corp., Research Center, Monroeville, Pa. Manuscript submitted March 6. 1968. ISD sulfur potential; ii) X-ray studies of ferrous sulfide; and iii) measurements of the parabolic rate of sulfidation of iron. Equilibrium Studies. About 1 g of iron powder or foil. contained in a small recrystallized alumina crucible ind suspended from a calibrated silica spring, was reacted with a hydrogen sulfide-hydrogen mixture of known ratio until no further change in weight was observed. %hen the gas composition was changed and the new state of equilibrium was established after several hours of reaction time. The composition of the sulfide was obtained from the initial weight of the sample and the weight after equilibration. X-Ray Studies. The lattice parameters of some of the equilibrated samples were determined using the General Electric XRD-5 diffractometer with a cobalt tube (no filter) set at 40 kv apd 10 ma; the CoK, radiation was taken as 1.79020A. Observed 220 and 311 diffraction peaks of silicon served as an internal comparison standard to correct for possible misalignment of the goniometer. The lattice parameters of the sulfide phase were calculated from the corrected Bragg angles of the 110 and 102 peaks. Rate Studies. In the initial experiments attempts were made to measure the parabolic rate of sulfidation by measuring the gain in weight of a thin iron strip, -0.05 cm thick, suspended from a silica spring in the reacting atmosphere. The preliminary experiments showed that this technique was not reliable for the measurement of the parabolic growth rate of the iron sulfide layer. In the subsequent experiments the data on growth rate were obtained by measuring, on a microscope stage, change in the thickness of the sample after reaction for a specified time in a hydrogen sulfide-hydrogen mixture of known sulfur activity. For each reaction time a new sample was used. Precision-machined iron blocks, 0.5 by 2 by 5 cu cm, were de-greased and annealed in hydrogen for several hours prior to the sulfidation rate measurements. The experiments were carried out at 670°, 800°, and 900°C in gas mixtures having the ratios, and 1.0 for periods of times from a few hours up to 8 days. Apparatus and Materials. A vertical globar tube furnace with a 3-in.-long uniform temperature zone was used. The glass tube fittings were fused on the zircon reaction tube, 1.5 in. diam. The temperature was measured with a Pt-10 pct Rh/Pt thermocouple placed in the hot zone of the furnace inside the reaction tube (an alumina thermocouple sheath was used). A separate thermocouple was used for the temperature controller which maintained the furnace temperature constant within about 2°C. Anhydrous liquid hydrogen sulfide and oxygen-free dry hydrogen from gas tanks were used in preparing the gas mixtures by the constant head capillary flow-meters. In all cases volume flow rate was 1000 cu cm per min at stp, corresponding to a linear velocity of about 6 cm per sec at 800°C; under these conditions

Jan 1, 1969

By E. Miller, K. L. Komarek, M. Ettenberg

The activity of aluminum in solid Co-A1 alloys has been measured by an isopiestic technique between 850° and 1200°C from 45 to 80 at. pct Al. The activity shows a Precipitous decrease around the stoichzornetric composition of CoAl. Free energies of mixing have been calculated over a limited composition range. Considering an antistructure-vacancy defect mechanism, the degree of intrinsic disorder, a , in CoAl was related to the alunminum activity. Excellent agreement between the calculated and experimental activity curves was obtained for a = 1.25 x 10-4. ThERMODYNAMIC properties of solid aluminum-transition metal alloy are being studied in an investigation of disordering in ordered compounds. In a continuing series of investigations, activities of solid Fe-1,' Ni-A1, kd r-A13 alloys have been measured. From the results for Fe-A1 and Ni-A1, the degree of intrinsic disorder for the equiatomic compounds was calculated2 using equations derived by Wagner and chottk. From the results for Cr-A1 the degree of intrinsic disorder was calculated from equations derived by Orr.' In this paper, the results of the study of Co-A1 alloys are described. Published activity data in the Co-A1 system has been limited to liquid alloys at 1600°C.° A heat capacity study7 of stoichiometric CoAl indicated that a second-order phase transformation occurs at 790° C, attributed to an order-disorder reaction. Oelsen and Middel,' employing the calorimetric mixing of pure liquid metals, obtained heats of formation for compositions from 6 to 90 at. pct Co. Heats of formation for 50 and 78 at. pct Co alloys have also been measured by acid solution calrimetr. The Co-A1 phase diagram, as compiled by Hansen and Anderko,lo is in good agreement with more recent X-ray evidence. The method for measuring activities of aluminum in this study is essentially that employed in the studies of the Fe-1,' i-Al, and r-A13 systems. This isopiestic method entails placing cobalt specimens, in a temperature gradient, in a sealed alumina system containing a pure liquid aluminum source of fixed vapor pressure. The specimens are equilibrated, cooled to room temperature, and their final compositions determined. From the measured temperature of the specimens and the known vapor pressure of pure aluminum the activities of aluminum in the alloy can be calculated. EXPERIMENTAL PROCEDURE The cobalt was 3-mil-thick sheet of 99.9 pct purity (herritt Gordon Mines Ltd., anada). The major impurities were 0.1 pct Ni, 0.014 pct C, 0.018 pct Fe, 0.004 pct S, and 0.005 pct Cu. The aluminum metal had a purity of 99.99 pct (Aluminum Corp. of America) and all alumina parts were 99.7 pct A1,O3 (Triangle RR Grade, Morganite Refractories, Inc.) with major impurities 0.05 pct SiOz, 0.1 pct Fe203, 0.2 pct NazO, and 0.05 pCt K20. Runs 1 to 3 were made with annular cobalt specimens (12 mm ID by 21 mm OD) punched from the sheet. The specimens were deburred and degreased in carbon tetrachloride and in acetone. The samples, each weighing about 150 mg, were then positioned along an alumina rod, a in. OD by 14 in. long, separated by alumina spacers, i in. ID by | in. OD by & in. long. The lower end of the rod was placed in a hole drilled in the center of an 80-g aluminum cylinder. This assembly was put into an alumina crucible, 1+ in. ID by 13 in. OD by 3+ in. high, and the position of each sample was measured to within 50.5 mm relative to the bottom of the crucible. An alumina tube, 28.5 mm ID by 35.5 mm OD by 14 in. long, closed at the top, was slipped over the whole assembly, so that it fitted snugly into the bottom crucible. The entire reaction assembly was tied with molybdenum wire and lowered into a mullite tube, closed at the bottom. A quartz thermocouple tube, closed at one end, containing a t/Pt-10 pct Rh thermocouple, calibrated according to the specifications of the National Bureau of standards,'' was placed along the reaction assembly inside the mullite tube. The temperature of each specimen could be determined by gradually raising the thermocouple and measuring the temperature gradient along the reaction assembly. The combined error in temperature measurement and sample position resulted in a total error of Q°C in the recorded temperature of each sample. The mullite tube was sealed at the top by a water-cooled brass head, connected to a conventional glass vacuum system. The aluminum reservoir is heated to its melting point sealing the alumina system containing the samples. During this process the pressure is maintained below 0.01 li Hg. During subsequent heating to establish the proper temperature gradient and throughout the entire run the pressure is maintained below 2 1 Hg by means of a two-stage mechanical pump. Equilibration runs lasted from 4 to 6 weeks and were terminated by air cooling. The temperature of the liquid aluminum reservoir was brought below its melting point in less than 20 min. For runs 4 and 5, alloy buttons with 49 and 69 at. pct A1 were prepared from the initial high-purity metals by arc melting under purified argon. The alloy buttons were comminuted to powder with an alumina mortar and pestle until the powder passed through a 400-mesh screen, particle size 0.0014 in. Portions of this powder weighing between 50 and 200 mg were placed in small alumina trays, 25 by 15 by 5 mm, which were then

Jan 1, 1969

By A. E. Lee

THE Blackwell Zinc Co., Inc., a subsidiary of the American Metal Co., Ltd., operates a horizontal retort zinc smelter at Blackwell, Okla. The plant has 14 furnace blocks of 800 retorts each, fired with natural gas on a 48 hr cycle. Over 13,000 tons of zinc-bearing material, chiefly sulphide flotation concentrates, are treated monthly to produce slab zinc and high lead-cadmium fume. In 1942 a program of rebuilding and modernizing the smelter was started. By 1947 furnace smelting capacity had been increased to a point where roasting and sintering facilities were inadequate, and it was necessary to purchase oxidized materials to supplement sinter production. The seven 210 ft Ropp roasters and three 42 in. x 44 ft Dwight-Lloyd machines then in use had been in service at least 20 years and were in need of major rebuilding. Thus it was entirely practical to consider all new equipment and a change of method rather than rebuilding and repairing obsolete units. A study of the problem indicated that roasting as such could be eliminated and roasting and sintering accomplished in one step by a modification of the Robson process,' which had been used since the early 1930's by the National Smelting Co., Ltd., at their plants at Avonmouth, England, and Swansea Vale, South Wales. Francis P. Sinn, General Manager, Zinc Smelting Operations, The American Metal Co., Ltd., who was familiar with the practice in England, suggested the use of one large machine for the entire operation from concentrate to sinter. One step sintering appeared to best meet Blackwell's plant requirements and indicated substantial savings in labor, gas, coal, and repair costs. Choice of Machine Size The sinter machine size was set at 12x168 ft for a rated capacity of 540 tons per day. This tonnage, produced on a five day week, would meet the seven day requirements of the 14 furnace blocks. The one large machine was quoted at a lower cost than two or more 6 ft wide machines of similar total capacity. Further, the larger machine could be housed in a smaller structure and only one set of equipment for charge preparation and delivery and for disposal of sinter cake was needed. One machine on a five day week made possible a concentration of the skilled operating personnel and required less men than a plant including two or more machines and related equipment circuits. Fewer units of equipment meant less maintenance, and the two down days weekly allowed ample time to repair and, if necessary, to make up lost production. Experience had indicated better sintering quality and rates with larger masses of material, not only on wider machines, but also in deeper beds. The ratio of windbox perimeter to area for the 12x168 ft machine is 0.179, compared to 0.353 for a 6x102 ft machine and 0.617 for a 42 in. x 44 ft machine. This meant less air leakage with resulting fan power savings and less spoilage of charge along the pallet sides. Performance Initial operation of the new sinter plant was made in November 1951 and regular production attained late in December. The average product sinter output during 1952 and the first half of 1953 has been 18.2 tons per hr. The average for one month has been as high as 22.4 tons per hr. Considerable experimenting with varied operating conditions accounts in part for the below capacity — 24 tons per hr — average output, and work to further improve production rate continues. A typical sinter analyses is 66.0 pct Zn, 0.3 pct Pb, 0.1 pct Cd, 0.3 pct S, 8.0 pct Fe, 2.0 pct SiO,, 0.8 pct CaO, and 0.2 pct MgO. Use of this material has made possible increases in furnace burden and improved furnace operation over the former practice using sinter made from Ropp roasted concentrates. Better lead and cadmium elimination in sintering has permitted the furnace production of slab zinc lower in lead and cadmium. Anticipated economies of operation have largely been gained. The sinter plant is operated by seven men per 8 hr shift — one head operator, three equipment operators and three sweepers — plus one oiler on day shift only. While it has been necessary at times to operate seven days a week to produce the required sinter tonnage, the five day work week usually has been adequate. Consumption of natural gas for sinter bed ignition is 200,000 to 300,000 cu ft per day. Green Ore Sintering Practice The 30 to 31 pct sulphur content of the —200 mesh zinc concentrates is the fuel used to sinter the charge, no coal addition being required. In the feed to the machine, sufficient concentrates are added to crushed return sinter fines containing 0.3 to 0.5 pct sulphur to produce a charge averaging 5.0 to 6.5 pct sulphur. Since the return sinter used in Blackwell's practice is varied from — 1/2 to — 1/8 in., the actual sintering mixture of fine sinter and concentrates is somewhat higher in sulphur. The coarser sinter particles are too large to resinter and merely aid porosity in the sinter bed. The ratio of concentrates to return sinter in the charge ranges from about 1:4 to 1:5.5. Variations are based on the appearance of pried up bed sections, bed exit gas temperature trends, windbox suctions, and return sinter size. Sufficient sulphur must be used to obtain fritting of the charge into a soft sinter cake and to aid in the elimination of lead and cadmium. Excessive feed sulphur will result in partial slagging of the cake impairing porosity and prolonging sintering time.

Jan 1, 1954

By M. J. Marcinkowski, A. Szirmae, R. M. Fisher

Room -temperature hardness measurements obtained from single and polycrystalline samples of a 47.8 at, pet Cr-Fe alloy which were aged for various times al 500°C show a two-fold increase over that of the unaged alloy after annealing for 1000 hr. A detailed examination of the deformation markings in the neighborhood of the hardness imbressions reveals that twinning becomes an increasingly more important mode of deformation as aging proceeds. this observation is shown to be inconsistent with the Proposals that the transformation is eve of order-disorder On the other hand, the results are in agreement with previous observations of Fisher et al. of a coherent chromium-rich precipitate which forms in an iron-rich matrix as a result of a miscibility gap in this alloy system as proposed by Williams . Using the coherent precipitate hypotlzesis as a model, a detailed analysis of the various possible strengthening contributions to both the slip mid twinning stresses is made. In the case of' slip, lattice friction within the chromium-rich phase and the chemical energy associated with the interface between the two phases contribute about 60pet to the total strength. The contributions from coherency strains and modulus differences are thought to contribute the remaining 40 pet of the strength but are difficult to evaluate because of uncertainties regarding the flexibility of the dislocation line. All of the factors have nearly the same or else a smaller effect on the twinning stress in the aged alloy. Twinning is never observed in the unaged alloy because the twinning stress is much higher- than that for slip. With increased aging times, the various contributions to the total stress for both twinning and slip increase, but most of those for slip increase much more rapidly, so that, in the fully aged alloy, it surpasses the stress for twin propagation. When a twin is nucleated by the chance occurrence of an internal stress concentration during a test, the subsequent twin burst results in a low hardness reading. FeRNTIC Fe-Cr alloys from about 15 to 80 at. pet Cr content show considerable change in properties such as hardness, electrical resistivity, saturation magnetization, and so forth, after aging in the vicinity of 500°C.* The most marked change is a large increase in hardness accompanied by a sharp decrease in ductility, so the phenomenon has often been referred to as the 475°C (885°F) em-brittlement problem. Changes in microstructure are rather subtle and most investigators have not been able to observe any X-ray diffraction or metal-lographic changes during aging. There is little doubt that the phenomenon is inherent to the Fe-Cr binary system and is not directly related to the formation of a phase. Two distinct schools of thought have developed during the past decade concerning this problem. Masumoto, Saito, and sugiharal have concluded, from their own specific-heat measurements, that atomic ordering occurs in this temperature range. Pomey and Bastien2 have also attributed the changes in physical properties with aging in the neighborhood of 500°C to atomic ordering. In addition, Takeda and Nagai3 claimed to have found X-ray verification for superlattices corresponding to the compositions FesCr, FeCr, and FeCr3. However, all known attempts to observe superlattices in Fe-Cr alloys using neutron diffraction, which should be much more sensitive, have been unsuccessful. These have been reported by Shull et al.4 for 25 at. pet Cr, williams5 for 75 at. pet Cr, and Tisinai and samans6 for a 28.5 at. pet Cr. steel. The second and more prevalent opinion ascribes the 475°C embrittlement phenomenon to the formation of a coherent precipitate due to the occurrence of a miscibility gap in the Fe-Cr system below about 550°C. This latter concept was first indicated by the results of Fisher, Dulis, and Carroll,7 who were able to extract fine particles about 200Å in diameter from samples of 28.5 at. pet Cr steels aged from 1 to 3 years at 475°C. The extracted material was found to be nonmagnetic, to have a bee structure with a lattice parameter between that of iron and chromium, and to contain about 80 at. pet Cr. Williams and paxton8 and williams5 confirmed these results and first explicitly proposed the existence of a miscibility gap below the a region in the equilibrium diagram. Alloys aged within this gap

Jan 1, 1964