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By Robert R. Walden, LeMont West

K ENTUCKY'S first acid-grade fluorspar flotation Kmill, shown in Fig. 1, was placed in operation Aug. 1, 1952, by the Pennsylvania Salt Manufacturing Co. at Mexico, Ky. During 1951 a critical shortage of acid-grade fluorspar developed and it became necessary for the company to produce part of its fluorspar requirements. In 1951 the company purchased the Crider and Lennen metallurgical fluorspar mill and an adjacent stockpile of tailing at Mexico, Ky. The tailing, assaying about 26 pct calcium fluoride, originated from log washer and jig mill concentrators in the area. As the mill did not have a fluorspar dryer or convenient rail facilities, the company leased the Burleson concentrator at Marion, Ky., where these facilities were available. At Marion, Ky., on the Illinois Central Railroad, dry acid-grade fluorspar is transported direct to the company's Calvert City, Ky., hydrofluoric acid plant. The Mexico flotation plant was reconditioned and designed to produce acid-grade fluorspar from the jig tailing stockpile. The new plant flowsheet is shown in Fig. 2. The ore feed, old tailing, which contains 10 pct of waste rock and coarse gravel assaying approximately 8 pct CaF,, is bound together by sticky clay

Jan 1, 1955

By William M. Sheehan

TRANSPORTATION is one of the most important problems of the mine operator and the possibilities of cost reduction in this field should not be overlooked. In the railroad industry, cars and locomotives have been improved greatly, and the progress there made is well worthy of study by the mine operator looking for maximum efficiency in every branch of his activities. One of the outstanding developments in the construction of railroad equipment in recent years has been the wide-spread adoption of large one-piece steel castings for the framework of locomotives, passenger and freight cars. Some of the advantages and applications of this type of construction will be outlined in this paper, with particular thought of the needs of the mining industry. The inherent qualities of cast steel: homogeneity, unrestricted size and shape, high tensile strength, flexibility of metal distribution, resistance to corrosion, and gracefulness of outline, make it the most versatile member of the ferrous group. Not only is it a strength-giving element, but it is corrosion resistant, a combination that makes for large economies in equipment maintenance. Flexibility of metal distribution allows the integral foundation to be in the shape best suited for the purpose. These cast structures are really assembled in the mold in liquid form and the metal can be placed in the right pro¬portion exactly where it is needed, thus securing weight economy and uniformity of fibre stress. Such a process permits the incorporation, with ease, of necessary brackets, utilizing them to provide not only greater strength for the derail part itself, but often to add to the value of the entire unit. Laps, seams, and joints, which are necessary in all fabricated forms, are eliminated.

Jan 1, 1933

By C. H. Frick

Before presenting the main topic, as indicated by the title, this paper will give some of the high-spot history of the anthracite industry. Introduction The earliest recorded use of anthracite was in the year 1762, when a company of Connecticut pioneers discovered anthracite near the present city of Wilkes-Barre, Pennsylvania. In the early days of the industry, the coal was used only in large pieces, the smaller pieces being discarded to waste piles. As the output of the industry increased during the nineteenth century, uses were developed for somewhat smaller sizes down to and including pea coal. Early in the twentieth century, sizes smaller than pea, such as No. I and No. 2 buckwheat, were developed and used. Accumulations of piles from current mining operations were still increasing; that is, the smaller sizes were still being discarded. It was not until after World War I that preparation of the so-called steam sizes began commercially. This was largely No. 3 buckwheat, which is screened through a 3/16-in. round-hole screen and over a 3/32-in. or a 1/16-in. round-hole screen. Use of Smaller Sizes The earliest recorded experience in burning the small sizes of anthracite for steam production, other than in a previous small experiment, was in the year 1913, when a size known as "boiler fuel" was introduced—a mixture of rice and barley (No. 2 and No. 3 buckwheat). At that time, there was still no method known for burning the still smaller sizes. At the present time, various sizes down to and including No. 5 buckwheat are being prepared (Table I) from current mining and bank-reclaiming operations. The sizes of No. 4 and No. 5 buckwheat and smaller are generally being used for steam production in large boilers. The Pennsylvania Power and Light Co., following World War I, used 680,000 tons of anthracite per year, burned largely on stokers for production of steam, whereas for the year 1943 it used 1,940,000 tons of stoker sizes and 400,000 tons of smaller sizes for grinding and burning in pulverized form. This company has taken a very large part in the research and development of ways and means of burning these smaller sizes of anthracite, including the grinding of the very small sizes. This paper is particularly concerned with the latter feature.

Jan 1, 1949

By Andrew Allen

WHEN a mine is changed from hand, to me-chanical loading, the character of the coal dumped at the tipple is changed in many ways. Selective mining is not so easy with mechanical load-ers, and where much picking is done at the face it is apt to be wasteful anyway. Much recoverable coal is apt to be lost by too free gobbing and, in my opinion, picking at the face should be confined to removal of heavy rock, such as pieces of roof or bottom or sulfur balls. and to such clearly defined and persistent bands as can be readily recognized and segregated. With mechanical loaders of the shovel type, even this amount of gobbing is almost impossible. When coal is shoveled into a conveyor there should be no difficulty in doing as much picking as now by hand loading. The size of lumps may be greatly increased, on ac-count of the ease of handling them with a shovel, as the miners will not break them up in order to lift them into cars. Fines may be increased. This is, of course, not universally true, yet it is my opinion that a shovel breaks the coal more, as a rule, than hand loading. This might not be true with all types of shovels and is cer-tainly not true with a conveyor, either with or without the "duck-bill." The average car load will be greatly reduced in fields such as Illinois and Indiana, in which it is the practice to build up the coal above the sides. Where "level full" regulations prevail there should be no material change. When the coal comes to the tipple these differences usually result in the discovery, that many changes are necessary in the preparation plant. The increase in the percentage of fine sizes will probably not bother the screen, but may overload the conveying apparatus. The larger size lump may clog the chute, but as a rule the efficiency of the sizing screens is not greatly affected. In one completely mechanized mine the proportions of 6-in. lump and 2-in. screenings, when loading by hand, were 16.9 and 51.3 per cent respectively. When loading mechanically, these proportions changed to 15 per cent lump and 53.5 per cent screenings. The picking force on the tipple has been increased from 14 on hand loading to 33 men on mechanically-loaded coal. This is for an output of about 5000 tons.

Jan 4, 1927

By B. E. Lindsly

The withdrawal of gas and/or oil in appreciable quantity from a natural oil reservoir causes the pressure within the reservoir to diminish, and if the oil is completely saturated with gas, this dissolved gas begins to evolve from solution. The liberation of gas from solution in oil causes the oil to change in several ways, the principal changes being: (1) reduction in volume or "shrinkage"; (2) increase in specific gravity (decrease in degrees A.P.I.); (3) decrease of energy in the oil; (4) increased viscosity; (5) increased surface tension. As the writer's investigations have been concerned more with the first three items than with changes in viscosity and surface tension the following discussion relates particularly to the volumetric shrinkage of the oil, to the increased specific gravity, and to the decreased energy in the oil, each caused by the liberalion of dissolved gas. One of the most surprising facts that have developed in the study of high-pressure well-head and "bottom-hole" samples is the great reduction in volume that occurs in some oils when the naturally dissolved gas is liberated. High-pressure samples taken from well heads in the Oklahoma City, Kettleman Hills and Ventura, Calif., fields decreased in volume from 11.2 to 40.5 per cent when the dissolved gas was liberated in reducing the pressure on the sample to atmospheric. The amount of shrinkage an oil undergoes when gas is liberated depends upon the quantity of gas liberated and also upon its composition. A given volume of the heavier gases, propane and butane for example, will occupy more space in the oil than an equal volume of methane. The reason for this probably is that the molecules of the heavier gases are larger than those of the lighter gases. When gases are not in solution, and particularly when they are at low pressures, the distance between the gas molecules is so much greater than the dimensions of the molecules themselves that the mere size of the molecules has little effect upon the space occupied by the gas, Avogadro's hypothesis, which in effect states that all gases under the same conditions have the same number of molecules per unit volume, relates to this phenomenon. The fact that the heavier gases occupy more space than the lighter gases in the oil, and

Jan 1, 1934

WASHINGTON, D. C. HERBERT C. HOOVER, Chairman H: FOSTER BAIN, Vice-chairman DAVID WHITE, Vice-chairman HARVEY S. MUDD, Secretary-Treasurer, Room 2114, Dept. of Interior Bldg. J. F. CALLBREATH HENNEN JENNINGS E. W. PARKER T. T. READ An inspiring meeting of the Washington, D. C., Section was held at the Cafeteria of the Interior Building on Friday evening, Dec. 6, 1918. One-hundred and thirty-five members and guests attended, and Vice-chairman H. Foster Bain presided. The Committee on Nominations reported: for Chairman, Herbert Hoover; for Vice-chairmen, Frederick G. Cottrell, and F. L. Ransome;

Jan 1, 1919

By R. M. Bird

Few persons outside of the foundry trade have any conception of the great variety of sands now regularly specified and furnished, nor of the differences in foundry practice frequently resulting from apparently minor changes in sands. Conditions in each locality where the sands are mined and prepared necessitate special equipment designed to perform the work efficiently. The description that follows of the foundry-sand producing operations is typical of the areas in New York and New Jersey, and particularly refers to the operations of the George F. Pettinos Co. A few years ago the so-called Albany sands were dug by simple methods and hauled by horsecart to railroad. Depletion of sand near railroad sidings and extended use of automotive power have appreciably extended the area from which sand is now being dug. It is not unusual to haul 5 miles to the railroad. As stripping is quite shallow, 6 to 18 in., and the banks of usable sand generally run from 12 in. to 4 ft., it is economical to work the bank by benches so narrow that the overburden can be thrown by hand shovel to the exposed bottoms. In effect the top soil goes back to where it was, but on a lower level. Consequently the general surface appearance of a mined acreage is the same as before. This condition is in fact cutomarily required when a farm owner sells his sand in the ground. After such replacement, in the course of 3 to 5 years the soil is no less fertile than it was before mining. The sand itself varies as to grain and bond vertically and also along the breast. No mechanical equipment has been developed to compete with hand shovels and no machine has as yet been devised that grades the sand as required. Uniformity of sand, as shipped, depends first, last and all the time on the man on the job. Mixing equipment can change the appearance of the sand and mask its lack of uniformity, but it will never correct wrongly graded sand, dug from the bank. Modern methods of testing are helpful in setting up standards against which the man in the bank can compare his sands, but a good bank foreman is the only assurance that the sand, as dug, matches the required sample.

Jan 1, 1926

By Albert L. Toenges

Alaska requires an adequate fuel supply for its development, and has large potential coal reserves ranging from lignite to subbituminous and anthracite. Coal production in the Territory now is less than the requirements. In 1947, production was 361,000 tons, divided about equally between bituminous coal from the Matanuska field and subbituminous coal from the Nenana field. There is need for development of modern mechanized mines, which should produce the required output with a minimum of workers. These mines should not be thought of in the light of large potential capacity, as in the States. However, these new mines should be developed by modern methods, which should result in lower costs than at present. Because of the diverse physical conditions in the coal fields, intensive investigation by diamond drilling is necessary to properly plan the development and equipment of mine sites at minimum cost. The Bureau of Mines is doing this now in the Wishbone Hill area of the Matanuska field. All coal land in Alaska is government-owned and subject to the Coal Leasing Act.

Jan 1, 1949

By E. W. Parker

THE anthracite region, from which there is produced annually about 80,000,000 tons, or approximately 15 per cent. of the total coal supply of the United States, has a combined area of a little less than 500 sq. mi. The total area occupied by the bituminous fields (including the sub-bituminous and lignite fields) is in the neighborhood of 400,000 sq. mi., so that 15 per cent. of the total output comes from this small area of only a little more than 0.1 per cent. of the coal-producing territory. of the United States. The productive anthracite area is divided into a series of basins or troughs, roughly parallel, extending. in a northeast-southwest direction through the. Counties

Jan 1, 1921

By J. Kent Smith

THE object of this investigation was to ascertain the effect of varying percentages of beryllium upon pure copper and the properties of the resultant alloys in their softest condition, the effect of heat hardening on them, and the extents to which these properties could be augmented by different combinations of heat hardening and cold rolling. The data compiled in this paper represent partial results of continuing work done by the writer during the years 1930 and 1931, which was a continuation of the unpublished ground work incepted in the laboratory of the Beryllium Corporation of America by H. B. Pulsifer in the year 1926. A short bibliography on beryllium alloys is appended to this paper. It has, of course, long been known that copper subjected to cold work is hardened and strengthened to a considerable extent, furthermore it had been qualitatively noted in previous experiments that copper-beryllium alloys seemed to take on hardness and strength as the result of cold work at a greater rate even than does plain copper. It was decided therefore to endeavor quantitatively to determine such rate of increase, as also the relative increases by combinations of cold working and heat hardening. The results are summarized in Tables 3, 4 and 5. A preliminary series of experiments had indicated that by an exposure to the heat of 575° F. for 2 1/2 hr. age-hardening of a 2.50 per cent beryllium-copper alloy took place. Slab ingots of nine different beryllium-copper alloys were prepared under identical conditions by means of the addition of a previously prepared 12.5 per cent beryllium-copper alloy to well melted and deoxidized pure copper. The ingots were then reduced by hot rolling to 12 gage (about 0.080 in.). These strips were heated to 1450° F. and quenched in cold water, and thus brought to their softest condition. (See Table 1.) Strips were next "precipitation-hardened" by reheating to a definite temperature. Similar strips to those itemized in Table 1 (which had been quenched from 1450° F.) were reheated for varying periods of time at 575° F. The hardness figures show that a metastable condition, of which the range of stability is dependent entirely upon time at the given temperature, begins to be noted in copper samples containing as little as 0.85 per cent beryllium. It is extremely noticeable in samples containing

Jan 1, 1932

By R. W. Bartlett

Hydrometallurgical processes for copper flotation concentrates avoid the SO2 emission problems associated with smelting, but they require oxidation of copper to obtain solubilization during leaching. The resulting copper ions must be reduced to metal, which normally requires large amounts of energy or energy equivalent reagents such as hydrogen or iron. The conventional reduction method is electrowinning which is labor intensive and involves 35 to 40% of both the entire operating and capital cost of the better hydrometallurgical processes. There is considerable incentive to reduce the cost and energy required for producing copper ions from solution. Furthermore, it is thermodynamically possible to do this using sulfur contained in the concentrate itself. In fact, the thermodynamic potential of oxidizing sulfur from S+4 to the S+6 state is greater than required to reduce cupric ion to metallic copper.1 Realization of this potential in a practical process would significantly reduce the cost of hydrometallurgical processing of sulfide concentrates because sulfur would become a cost-free reducing agent. An apparently practical method is to use SO: and HSO3 ions, obtained by ammonia scrubbing of SO2 from a concentrate roaster gas, to reduce leached copper to metal in an autoclave. This reduction step is the Jumau 1907 A series of steps, including sulfite reduction, constituting a crude flowsheet was suggested by Parker in 1976.3 The present paper describes a detailed complete. sulfite process flowsheet based on materials and energy balances, discusses the chemistry, and discusses further work that is required to develop this process. Process materials, utilities costs, and energy requirements are projected to be unusually low because of the utilization of sulfur from the concentrate. Process Description The sulfite reduction process requires a copper concentrate containing approximately as much sulfur on a weight basis as copper. For those few concentrates that are deficient in sulfur, additional sulfur can generally be obtained by allowing more pyrite to float in the concentration process. The process steps, shown in [Fig. 1], are (1) a fluid bed roast of the concentrate, (2) a leach of the roaster calcine using recycled barren liquor from the reduction autoclave, (3) scrubbing of the SO2 gas with ammonium sulfite liquor to produce ammonium bisulfite, (4) reduction and precipitation of copper in an autoclave by combining part of the SO2 scrubber effluent (SO5

Jan 1, 1980

By AIME AIME

THE accompanying photograph: submitted by C. L. Bransford, assistant district manager of the Republic Steel Corp., in Birmingham. Ala., shows the remains of the old Tannehill blast furnaces, one of the first furnace plants in the South. They were built by Moses Stroup and operated during the Civil War period, when cannon balls were cast there. The record day's run of this furnace plant was said to be 30 tons of iron. The furnaces were fed by a water-wheel-operated bellows and used charcoal, a product of the neighboring forest. They were first owned and operated by the Pioneer Mining & Manufacturing Co., that later became the Republic Iron & Steel Cu., and subsequently the Republic Steel Corp. in that district.

Jan 1, 1936

Records of coal in Colorado begin only a few years before the Civil War. In 1859 Macomb reported beds of lignite on both sides of Galisteo Creek, and in the foothills of the Placer Mountains, a place where an outburst and overflow-of trap had changed the lignite into bright, hard anthracite.1 The Union Pacific Railroad sent Joseph T. Hodge to investigate the coal deposits in the Rocky Mountains, close to the projected line, in the fall of 1863. He was told of coal on South Boulder and Rock Creeks, and that somewhere on Lodge Pole Creek it was being worked for supplying fuel for stage stations; a bed was also reported seven miles north of the stage road between Laporte and Latham. It was only in the vicinity of Denver that coal mines were being worked to any extent; these openings were on Coal Creek about 22 miles north of the town, said to have been opened in. 1860. The coal was used by the smiths with ,difficulty and slacked badly on exposure., Some coke was made from one of the seams, the coke being preferred to the raw coal by smiths. Another district was opened along South Boulder Creek, about two and a half miles from the base of the Rocky Mountains, two mines being worked to supply the Denver market.2 Hayden reported a large bed of coal at Golden in 1861 and of having seen a similar one in 1862 about 65 miles east of Pikes Peak, and in 1866, he saw large beds on Rock Creek 16 to 19 miles from Golden. In 1867 he saw the Belmont or Marshall's mines opened in 1863 on South Boulder Creek, which he said was the finest exhibition of coal in the state. The next one was the Murphy mine, on Ralston Creek, five miles north of Golden. A mine was also being worked near Canon City at that time.3 The coal at Golden was being worked in 1864.4 In 1867 the coal mined at Golden was being used in a firebrick' works. At Canon City and other places on the waters of Arkansas River, coal was being mined for use in the valley towns, bringing $5.00 per ton at the mines.5

Jan 1, 1942

By J. Kent Smith

The object of this investigation was to ascertain the effect of varying percentages of beryllium upon pure copper and the properties of the resultant alloys in their softest condition, the effect of heat hardening on them, and the extents to which these properties could be augmented by different combinations of heat hardening and cold rolling. The data compiled in this paper represent partial results of continuing work done by the writer during the years 1930 and 1931, which was a continuation of the unpublished ground work incepted in the laboratory of the Beryllium Corporation of America by H. B. Pulsifer in the year 1926. A short bibliography on beryllium alloys is appended to this paper. It has, of course, long been known that copper subjected to cold work is hardened and strengthened to a considerable extent; furthermore it had been qualitatively noted in previous experiments that copper-beryllium alloys seemed to take on hardness and strength as the result of cold work at a greater rate even than does plain copper. It was decided therefore to endeavor quantitatively to determine such rate of increase, as also the relative increases by combinations of cold working and heat hardening. The results are summarized in Tables 3, 4 and 5. A preliminary series of experiments had indicated that by an exposure to the heat of 575" F. for 2 1/2 hr. age-hardening of a 2.50 per cent beryllium-copper alloy took place. Slab ingots of nine different beryllium-copper alloys were prepared under identical conditions by means of the addition of a previously prepared 12.5 per cent beryllium-copper alloy to well melted and deoxidized pure copper. The ingots were then reduced by hot rolling to 12 gage (about 0.080 in.). These strips were heated to 1450" F. and quenched in cold water, and thus brought to their softest condition. (See Table 1.) Strips were next "precipitation-hardened" by reheating to a definite temperature. Similar strips to those itemized in Table 1 (which had been quenched from 1450" F.) were reheated for varying periods of time at 575" F. The hardness figures show that a metastable condition, of which the range of stability is dependent entirely upon time at the given temperature, begins to be noted in copper samples containing as little as 0.85 per cent beryllium. It is extremely noticeable in samples containing

Jan 1, 1932

By Robert Rhea Goodrich

This research was done partly in the non-ferrous laboratory of the Department of Metallurgy of Columbia University, under the direction of Dr. Edward I?. Kern, and completed elsewhere. Acknowledgment is due to Prof. Arthur L. Walker, Dr. Edward F. Kern and Dr. William Campbell of the Department of Metallurgy, for their kind advice and for the inspiration derived from their instruction. This report is given under the following heads: Petrographic Description (Microscopic Study); Sampling and Preparing Ore for Treatment; Chemical Analysis; Treatment of Ore. Petrogeaphic DescRiption Texture: variable. Fine to medium mixed aggregate. Original Structure: Obscurc. Secondary structure: Fractured; healed. Mineralogy (Minerds are grouped for interpretation purposes and are arranged, in each group in approximate order of abundance)

Jan 1, 1916

THE Pacific Northwest's joint meeting of the Industrial Minerals and Metals Branch in Spokane, Wash., drew 260 members, 72 students, and 30 ladies. Theme of the meeting was to acquaint men in the industry with students and younger men. The special appeal to the students was coupled with an attempt to attract young technical men from the companies located in the northwestern area. The activities of the meeting were available without charge to students. Contributions were made by the industries in the area to assist student attendance. Following the special student and faculty trip to the Trentwood rolling mills and research laboratory on Friday afternoon everyone enjoyed a complimentary dinner. A. Y. Bethune of the Sullivan Mining Co., spoke to the group on the operations of Kellogg, Idaho electrolytic zinc plant. The Industrial Minerals Div. session was opened on Saturday morning by R. G. Vervaeke, Conference Chairman who introduced A. O. Bartell of the Raw Materials Survey, Portland, Ore. Mr. Bartell in turn introduced C. W. Sweetwood who discussed Open-Pit Phosphate Mining.

Jan 1, 1952

By John C. Branner

Inquiries are frequently made concerning the chalk- and clay-beds of Arkansas, usually with a view to the manufacture of Portland cement. The chalk-deposits were first described by Professor R. T. Hill in the annual report of the Geological Survey of Arkansas for 1888, vol. ii., pp. 153-162. Since the publication of that report I have visited localities then unknown, and have accumulated considerable additional information concerning these deposits, dl of which is brought together in the present paper. My report upon the clays of the State has never been published; only a few of the more conveniently available deposits are mentioned in the present paper. The Chalk-Deposits. Stratigraphic Position of the Chalk.—The chalk-deposits of Arkansas belong to rocks of Cretaceous age. The Cretaceous rocks are confined to a single definite area in Southwest Arkansas. Beginning on the Ouachita river, a little northeast of Arkadelphia, its southern or upper margin follows a line about five miles southeast of, and approximately parallel to, the St. Louis, Iron Mountain and Southern Railway from Arkadelphia

Jan 1, 1898

By Yuri D. Tretyakov, Robert A. Rapp

The stoichiometry ranges ofNiOl+y and LiFe,O,-d were established by high-temperatwe electrochemical meas7rements in a stabilized-zirconia electrolyte cell. The results were consistent with doubly ionized cation vacancies in NiO,+y and interstitial lithium or iron ions in . The defect structure of the ternary ferrite was derived from the consideration of equilibration with respect to oxygen between the solid and the gas phase. The absolute magnitudes of defect concentrations were calculated. Pavtial molar enthalpies of oxygen in the compounds were calculated and interpreted in terms of the enthalpy of defect formation in these crystals. NICKEL oxide (NiO,,?) is a metal-deficient, p-type, extrinsic semiconductor whose properties are consistent with a structural model based on the presence of cation vacancies as the predominant ionic defect at sufficiently high temperatures and oxygen activities. A survey of previously reported conductivity studies and the presentation of some more recent conductivity measurements will be given in a later paper.' The absolute magnitude of the equilibrium vacancy concentration in NiO has been reported from combined conductivity and thermogravimetric data of ' However, disagreement exists concerning the state of ionization of the nickel vacancies in NiO. Some authors3-' have proposed that the predominant defects in NiO are singly ionized nickel vacancies and positive holes (h') formed by the reaction where, accorhng to the notation of Kroger and Vink,6'7 Oq represents an oxygen ion on its normal lattice site. Other authors"27E have proposed that doubly ionized nickel vacancies (V{i ) and positive holes are predominant and are formed by the reaction One purpose of the present investigation was to establish the nature of the predominant defect in NiO,+? as well as its equilibrium concentration and thermo-dynamic properties at elevated temperatures and known oxygen activities. To accomplish this purpose, the coulometric titration of oxygen into and out of NiO was accomplished using a galvanic cell involving the calcia-stabilized zirconia electrolyte. The ternary oxide, lithium ferrite (LiFe50,-6) is ferromagnetic and has the inverse spinel structure LiFe,O,-d Thus, in the ideal stoichiometric XY204 lattice, Fe3 ions occupy one-eighth of the tetrahedral (A) sites, and i' and Fe3' ions share at random one-half of the octahedral (B) sites within the fcc sublattice of oxygen ions.g The structure and thermodynamics of the spinel structures have been comprehensively decribed.'-' A recent compilation of literature for lithium ferrite is also available. 15 Oxygen-excess LiFe50sis not expected to exist because both i' and 17e3& ions are in their highest normal valency states (positive hole formation is not favorable). As will be discussed, equilibration of the ferrite crystal with oxygen of a surrounding gaseous phase will result in the introduction of equilibrium concentrations of ionic and electronic defects. In the Results and Discussion section a defect model for LiFe50,-d is proposed. This defect model is tested by high-temperature coulometric titration experiments. EXPERIMENT The oxygen activities in nonstoichiometric NiOl+, (and also LiFe,O,-d) were measured by means of coulometric titration with the high-temperature galvanic cell The critical characteristic of a suitable experimental cell is the complete isolation of the phase to be investigated in a minimum sized chamber which is free from extraneous sources and sinks for oxygen (leakage). Then oxygen is only admitted to the chamber or removed from it in known amounts by coulometric titration, which involves the passage of oxygen ions through the solid electrolyte with electrochemical oxidation and reduction reactions at the platinum contacts to the electrolyte. The experimental cell is shown in Fig. 1. The cap of the cell was the tip from a closed-end alumina tube, which was found to be leak-free from a helium leak-detector test. This alumina cap was about 1.2 cm OD and about 1.5 cm high. A Zircoa calcia-stabilized zirconia tablet (crucible lid) of 1.5 cm diam and 0.3 cm thickness served as the solid electrolyte. A Pyrex ring of about 0.1 cm thickness was placed between the electrolyte and the cap. The electrolyte tablet was painted with platinum paste on the entire outer face and on that part of the inner face which would be within the enclosure; these electrodes were further prepared by heating in air at 1000°C for 2 hr. Nickel oxide powder, listed as 99.999 pct pure, was purchased from Leico Industries, Inc. Pills of the NiO were cold-pressed and sintered at 1050°C for 3 hr in a platinum crucible. This poorly sintered NiO was crushed, and chunks were wrapped in 52-mesh Pt gauze (to catalyze the solid-gas exchange) for place-

Jan 1, 1970

By J. W. Freeman, D. N. Frey

Fundamental reasons for the improvement in creep resistance of an austenitic alloy by cold working were investigated mainly by X-ray diffraction. The creep resistance was found to be improved by the internal stresses in the lattice of the alloy induced by the cold work. THIS investigation was concerned with the fundamental reasons for improvement in creep resistance of an austenitic alloy as a result of cold working. Also, the investigation was carried out to elucidate the conditions under which cold working could be expected to improve the creep resistance. To achieve these ends, creep resistance and internal structure were correlated for a variety of cold-worked conditions. Since the aim of the investigation was not to obtain specific and extensive information on any one alloy, creep testing was done with a single stress at 1200°F. Structural studies were carried out primarily with X-ray diffraction characteristics. The alloy used, low carbon N-155, was selected on the basis of being representative of at least some of the alloys used in gas turbines. Low carbon N-155 alloy in the form of %-in. sq bar stock was used in this investigation. The chemical composition, in percent, was: C, 0.13; Mn, 1.43; Si, 0.34; Cr, 20.73; Ni, 18.92; Co, 19.65; Mo, 3.05; W, 1.98; Cb, 0.98; N, 0.14; and Fe, balance. The bar stock was produced from a 13-in. sq billet, finished to 7/s in. round cornered square between 2060" and 1910°F. Prior to use in this particular investigation, the bar stock was solution-treated 1 hr at 2200°F and water quenched. This procedure was used in order to put the stock in a condition where effects of prior processing were minimized. Experimental Procedure The specific approach to the problem was twofold. First, the influence of cold working, under various conditions, on the creep rate under a single stress at 1200°F and on the internal structure was in part determined. Second, the effect of annealing at various times and temperatures on the creep rate and internal structure of the cold-worked samples was in part evaluated. The first step was basic to the investigation—creep resistance and structure were to be correlated. The second step was taken to see if the annealed samples showed some internal changes which could also be correlated with changes in creep resistance. This it was felt would facilitate solution of the basic problem. The creep and structural studies were carried out on samples reduced approximately 5, 15, and 40 pct at room temperature and 15 pct at temperatures up to 2200 °F. Annealing of various of the samples was done at 1200°, 1400°, 1600°, and 1800°F for time periods up to 1000 hr. Studies of the annealed samples were concentrated on materials rolled approximately 5, 15, and 40 pct at room temperature and 15 pct at 1400°F. The creep tests were carried out at 1200°F under 40,000 psi, the latter being approximately the 1000 hr rupture stress of the material

Jan 1, 1952

By Arthur F. Taggart

MR. CHAIRMAN: Congratulations! Your four-ring milling show this year was a dandy. It cleared our minds, for a few hours at least, of what Hitler, Hirohito, the New Deal, and the tribe in the Treasury are trying to do to strangle American enterprise. We mustn't forget this, but it's a relief to get our thoughts away from it occasionally. GRINDING-There was a further contribution to the excellent work that the Allis-Chalmers laboratory staff has been doing for the grinding fraternity in compiling-and publishing-a carefully quantitative list of comparative resistances of ores and other materials to comminution (T.P. 1579, Bond-Maxson). A diagnostic accuracy of ± 10 per cent was claimed for estimates based on these figures. Are they really that good? How about some of you men in the field writing M&M about it?

Jan 1, 1943