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By John Birkinbine

The experience of the past five years has furnished opportunities to study and to partially explain the operation and some of the causes of the short blast of Warwick Furnace at Pottstown, Pennsylvania, as described in the paper read at the Lake Superior Meeting, in August, 1880.* The many inquiries concerning the details of furnace operation which followed the publication of the paper, and the expressed desire of furnace managers to be informed as to future operations of this plant, have encouraged the preparation of the following data. To make the record continuous, and add to the value of both contributions, the present paper commences where the review of a short blast of Warwick Furnace ended, and includes the data of another short blast of two months, and a subsequent continuous campaign of nearly five years, which, by comparison, we shall designate as "the long blast." Frequent visits to the plant in the five years, during which its operation could be studied, and correspondence with the manager, Mr. Edgar S. Cook, have given a knowledge as to general features and details, and the courtesy of the officers of the Company which has given free access to the books of record permits the presentation of data which it is believed will be welcomed by furnace managers. Interest will undoubtedly be increased by the remarkable results which Mr. Cook has achieved chiefly with anthracite coal in a furnace whose details of construction will scarcely be generally admitted as embodying advanced ideas, its height being but 55 feet, with a bosh diameter of 15 feet 6 inches, its bosh-slope comparatively flat, its crucible smaller than the average, and the heat of the blast never reaching 1000' Fahrenheit. At present writing the credit of the best anthracite blast-furnace practice recorded in our Transactions is conceded to be that pursued by Mr. Fackenthal, at the Durham furnace, and Mr. Cook, at War-

Jan 1, 1886

By Arthur Taggart

THIS paper describes the result of a series of experiments run in the laboratory of the School of Mines, Columbia University, during the winter of 1927-28. It shows that the several operating adjustments of a pneumatic table produce effects in the action of a, given coal that may be grouped into two classes, viz.: stroke length, speed and rocker-arm angle, which affect longitudinal travel; air supply and table slope (transverse and longitudinal), which determine transverse travel. The magnitude of the effect of the different adjustments varies. Some of the adjustments affect stratification of the bed, both as respects size and specific gravity of the bed components, as well as direction of travel. Operation of a pneumatic table is fundamentally different from that of a wet table in that the former exerts, through the air supplied, a force on the particles upward away from the deck which is lacking on the wet table while, on the other hand, it lacks the positive control over cross travel that is supplied by the wash and feed water.

Jan 1, 1929

By H. J. French

Within the past few years, particularly because of the rapid growth of the airplane industry during the war, considerable attention has been paid to the manufacture of light-wall cold-drawn seamless and welded steel tubing for structural purposes. While the manufacture of such tubing is not, in itself, a difficult matter, some difficulties have been encountered in producing the same under specifications requiring definite physical properties. It is the purpose of this paper to describe the methods of manufacture and the properties that may be obtained by such methods for tubing coming within about 1/2 to 2 in. (12.7 to 50.8 mm.) outside diameter and 10 to 22 Birmingham wire gage (0.134 to 0.028 in. wall thickness). Such tubing is largely used as structural material in the aircraft industry, and it is of the utmost importance that the physical and chemical properties should be known, and also that the various factors entering into the manufacture should be under such control as to allow these properties to be varied and held within definite limits. In general, tubing may be divided into four classes: namely, specialty tubing, such as riveted-sheet or plate, lock jointed, etc.; brazed tubing; welded tubing; and seamless tubing. Welded tubing may be divided into hot product, such as lap welded and butt welded, and cold product, such as acetylene and electric welded. Seamless tubing may be hot rolled or cold drawn. Specialty Tubing The first two classes present mainly mechanical or structural engineering problems. A simple form of tube is made by riveting together the overlapping edges of rolled sheets or plates formed into a cylinder. Because of the nature of its construction, such a tube is necessarily limited to relatively large sizes. Lock-jointed tubing is produced by passing low-carbon strip through a forming machine having suitable rolls and dies, its manufacture is almost entirely a question of design of the forming machine and its satisfactory operation. The chief application of such tubing is in the manufacture of bedsteads.

Jan 1, 1920

By H. R. Aldrich

This paper is not a treatise on the theory and practice of magnetic surveying. It presents a diagram upon which have been plotted observations taken with the simplest form of magnetic instrument, the lowly dip needle, over a large area astride the Lake Superior syncline of northern wisconsin. The exposures of the underlying formations are not sufficiently great in number nor fortunate in distribution to have provided the fuller understanding of the geology which has been secured by the use of the magnetic observations as an auxiliary tool or accessory in the hands of the geologist. The diagram (Fig. 2) in large part speaks for itself if studied in connection with the geological map (Fig. 1) for which it is the main control. It is presented to demonstrate the extent to which the use of such methods may aid in the solution of geological problems in a covered country. The diagram is probably unique in assembling the expression of such a wide range of formations, affected by so wide a range of secondary processes, and deformed by so many different structures in terms of magnetic variation. Few geologists outside of the Lake Superior country have had any first-hand experience in the taking of magnetic observations and the interpretation of the results in terms of geological conditions; nor have the Lake Superior men gone with the methods far afield from the mere tracing of iron formations. In more recent years the oil companies have gone heavily into investments in magnetometers, balances, and dip needles in the quest of concealed structural anomalies which are the favorable loci of petroleum accumulation. But these geophysicists come back from the fields with their collections of observations facing the question of interpreting the geological meaning of their magnetic anomalies. It is considered probable therefore, and certainly it is the hope of the writer, that the appended charts, or magnographs, which show how character of the country rock and its changes, structural strike and dip and their changes, depth of burial and its variation, contact metamorphic

Jan 1, 1929

By Charles Fulton

EXPERIMENTAL work on the process was begun on a laboratory scale at Cleveland, Ohio, in 1914, and transferred to East St. Louis, Ill. in 1916, where a commercial sized furnace was in technical operation until January, 1918. The essential steps of the process are as follows: Oxidized zinc ore or roasted zinc concentrate is mixed with crushed coke and coal-tar pitch and formed into briquets 9.25 in. (23.5 cm.) in diameter and 21 in. (53 cm.) long in a manner similar to that used in the manufacture of graphite or carbon electrodes, except that much less care and time are required. The composition varies with the nature of the ore; in one case, the composition was 100 parts ore, 70 parts coke, and 18 to 20 parts pitch. These briquets maintain their form and volume during and after the distillation of the zinc. This object is gained by using coke as the matrix and coal-tar pitch as the binder; this pitch becomes coke on heating and unites the ore particle and the original coke particle into a continuous mass. The briquet is an electrical conductor but only to such, a degree that it can be used as a resistor. The size of the ore, as in the present practice of zinc metallurgy, ranges from fine material, such as flotation concentrate, to coarse table and fine jig concentrate. The process is not restricted to any particular kind of ore, but is applicable to pure high-grade ores, ores high in iron, and complex zinc lead ores, since the residue from the distillation is held immovably in place within the briquet. In the case of complex zinc-lead ores, the distillation is conducted with a carefully regulated temperature so that a high percentage of lead is retained in the distilled briquet, which may then be smelted for its lead content. In present zinc smelting practice, the reduction fuel is from 40 to 50 per cent. of the weight of the ore. In the briquet, it is from 60 to 85 per cent. of the ore; but unless the ore is exceptionally high in residue, the distilled briquet

Jan 9, 1919

By E. C. Bain, E. S. Davenport

When annealed carbon, or low-alloy, steels are suitably heated the ferrite (alpha iron solid solution) and the carbide, of which they are composed, react together to form a single solid solution of carbon (and other elements) in gamma iron (austenite). This reaction may begin only at a certain minimum temperature called the eutectoid temperature. The first ferrite and carbide thus to react together do so in definite proportions known as the eutectoid composition. With further heating the original constituent that is present in excess is dissolved in the austenite until exhausted. Whether the excess constituent be ferrite (hypoeutectoid steels) or carbide (hypereutectoid steels) the procedure is much the same, and upon slow cooling the homogeneous austenite expels the excess of either (proeutectoid ferrite or carbide) until the eutectoid composition is reached. Thus the reaction upon heating is strictly reversed upon cooling and accordingly an equilibrium diagram of this process may be constructed. Such an equilibrium diagram concerns itself only with the temperatures involved and with the proportions and compositions of the phases developed under conditions that suffice to permit equilibrium. Specifically it has no concern for the type or mode of distribution of these constituents nor with any extra-equilibrium conditions such as undercooling, which is almost universally encountered in metals. Actually, however, of great importance is the sluggishness toward equilibration caused by the not inconsiderable time involved in diffusion. Thus instead of the theoretical transformation point AF, we find for a certain rate of heating or cooling the use of the designations Ar and Ac (transformation temperature found on cooling and upon heating). These figures obviously have no particular meaning except as measured and expressed for a definite heating or cooling rate, and represent the apparent temperature displacement caused by an inadequate time allowance. In this paper are presented the results of a study of the time required for the transformation of austenite to ferrite and carbide at a variety of temperatures and also of the time required for the reaction austenite? martensite at the temperatures at which this reaction occurs instead of

Jan 1, 1930

By Lewis T. Wright

(Pittsburg Meeting, March, 1910.) I HAVE long been aware that ferruginous copper furnace slags if fused in the electric arc will yield metallic iron containing copper, and in order to confirm this knowledge, and to obtain further information of the behavior of such slags in the high temperature and reducing conditions of the electric furnace, a number of samples of slag were fused in an experimental electric furnace. The results obtained, given in Table I., show that a very large amount of metallic iron was produced, and that this iron carried with it practically all the copper, gold, and silver, and more than 50 per cent. of the sulphur, of the original slag. The metallic buttons formed in the electric furnace were clean, hard, but not brittle.

Mar 1, 1910

By R. J. Fruehan

The oxygen activity and concentration were measured in Fe-Cr-0 melts in equilibrium with an oxide phase at 1600°C (2912°F). The activity was determined by ,use of the following solid oxide -electrolyte galvanic cell CY-Cr8,(s) I ZrOz(CaO) I Fe-CY-G(saturated)(l) The oxygen concentration decreases with increasing Cr concentration to about 270 ppm 0 at about 7pct CY and then increases gradually. The activity coefficient of oxygen (fo) decreases with increasing Cr. In melts containing up to about 20 pct Cr, log f is approximately a linear function of wt pct Cr with a slope (e q 2) of —0.037. The activity of chromium was calculated and found to exhibit a small negative deviation from Raoult's law. From the activity and solubility data for low chromium melts, the free energy of formation of chromite, FeCr204, was found to be -79.8kcal per mole where pure liquid chromium and oxygen at I wt pct in Fe are the standard states. ThE effect of chromium on the chemical behavior of dissolved oxygen in liquid iron is of great importance in controlling the deoxidation of steels containing a significant amount of chromium. Chen and chipman' equilibrated Fe-Cr melts in the presence and absence of slag with hydrogen-water vapor mixtures. They concluded that at 1595°C chromite was the oxide phase in equilibrium with Fe-Cr alloys containing less than 5.5 pct Cr while at higher chromium concentration Cr,O, was the stable phase. In the composition range 0 to 10 pct Cr they found that the interaction coefficient, was equal to -0.041. Turk-dogan,' Schenck and Steinmetz,, and pargeter4 measured egr) in a similar manner and found the value to be -0.064,-0.04, and -0.052, respectively. McLean and Be11 evaluated egr) from their data on the equilibrium of Fe-Cr-Al-0 alloys with H2/H20 mixtures and found it to be -0.058. However, McLean and Bell's value should only be considered an estimate because the effect of aluminum on the activity coefficient of oxygen is about a hundred times greater than that of chromium. Consequently, an error in the value of egl) used, which at the present time is not well-known, or an error in aluminum analysis, which is present in very small quantities, will result in a significant error in egr). Fischer et a1.6 determined the interaction coefficient (eEr) in Fe-Cr-0 melts not in equilibrium with an oxide phase and containing less than 18 wt pct Cr at 1600°C electrochemically. They determined a value of -0.031 for egr). Hilty et aL7 measured the oxygen content of Fe-Cr melts in equilibrium with an oxide phase containing up to 50 pct Cr. They found that the solubility of oxygen decreased as the chromium content increased to about 6 pct Cr and then increased gradually. They concluded that the equilibrium oxide phase was chromite below 3 pct Cr, distorted spinel from 3 to 9 pct Cr, and Cr,04 above 9 pct Cr. Adachi and lwamotoa also investigated this system, but did not find Cr30,. They X-rayed the equilibrium oxide phases and did not find the presence of Cr,O,. They also X-rayed the oxide phase extracted from a 65 pct Cr melt which was heat treated and did not find metallic chromium as would be expected if Cr3O4 were the equilibrium oxide phase as indicated by the reaction : 3Cr3O4 — 4Cr2O:, + Cr [lj It was the purpose of the present investigation to determine the effect of chromium on the activity coefficient of oxygen in Fe-Cr melts by measuring the activity and solubility of oxygen equilibrated with an oxide phase in the composition range 0.18 to 50.5 wt pct Cr at 1600°C (2912°F). The activity of oxygen in the melts was determined by use of the following galvanic cell: The relationship between the partial pressure of oxygen in equilibrium with the melt and the reversible electromotive force of the cell (E) is where 11 = 4, F is the Faraday constant, pb, is the oxygen pressure in equilibrium with the meit and is the oxygen pressure in equilibrium with Cr203 as determined from the free energy data compiled by Elliott et al? The oxide phase in equilibrium with pure chromium was assumed to be Cr If Cr30, were the equilibrium phase the activities derived would be approximately the same, since the best estimated free energy of formation of Cr,O,, if it does exist, is approximately % the free energy of formation of The activity of chromium in Fe-Cr alloys at 1600° C was also determined from the measured electromotive force. The activity of chromium (aCr) is related to the electromotive force as follows: , The oxide phase in equilibrium with pure chromium and Fe-Cr melts from 10 to 52 pct is assumed to be Cr203 so that n equals three. If future work proves the existence of Crs04 in equilibrium with Fe-Cr melts and pure chromium, the experimental results can be reevaluated using a value of $ for n in Eq. 141. A value of ^ for n will make the activities about 10 pct higher. In order for Eqs. 131 and [4J to be valid the electrolyte, ZrOa(CaO), must exhibit predominantly ionic conduction at the temperature and oxygen partial pressure of its use. Previous work1' has demonstrated that ZrOz(Ca0) is predonlinantly an ionic conductor

Jan 1, 1970

By S. J. Matas, R. F. Hehemann

The existence of two distinct forms of bainite—upper and lower bainite—in hypoeutectoid steels is confirmed by a systematic study of the structure of the product resulting from this mode of austenite decomposition. The transition between these two forms occurs at about 650° F regardless of the alloy content of the steel and their structural differences can be interpreted in terms of the kinetics of carbide precipitation from supersaturated ferrite. In the past few years, a renewed interest has been displayed in the kinetics and mechanism of the bainite reaction in steels. Several rather divergent models for the transformation mechanism have evolved from these studies,'-' however, it is difficult to evaluate these models critically on the basis of the existing experimental data. In particular, a more detailed knowledge of the structure of bainite should be helpful in providing a framework for the construction of an appropriate model. Metallographic studies7-l4 have led to a recognition of at least two distinct forms of bainite—frequently termed upper and lower bainite. Although the morphology of bainite changes with reaction tem- perature, there appears to be a relatively sharp transition between the two forms. This occurs in a narrow temperature range near 650° F. Transformation at temperatures below about 650° F results in the presence within the bainite of small plates of carbides oriented at an angle of 60 deg with respect to the direction of growth of the plate, while at higher temperatures carbides are oriented parallel to the growth direction. There is no generally accepted view regarding the significance of this structural transition. Some authors feel that carbides precipitate from austenite at all reaction temperatures1' while others claim, at least for low-temperature bainite, that carbides precipitate from supersaturated ferrite.14.15 It was recognized many years ago that the nature of the carbide in bainite depends on the reaction temperature. The carbide hase in upper bainite is unmistakenly cementite.16-19 The exact nature of the carbide in low-temperature bainite is less certain. Magnetic measurements of lower bainite reveal no cementite Curie point21'22 and dilatometric studiesz0 produce total expansions which are larger than those predicted on the basis of a ferrite-plus cementite structure. These effects have been attributed to the

Jan 1, 1962

Jan 1, 1951

Jan 1, 1951

By Charles A. Chase

This paper, descriptive of a single mine, is presented in the belief that it may furnish useful suggestions to mine-managers encountering similar problems; and it includes the details which will enable them to estimate the value of the methods employed—especially where these depart from common practice. Tt should be added, however, that this mine is not typical of the San Juan district, but differs markedly from neighboring mines in physical conditions and metallurgical requirements. The Liberty Bell mine is situated in San Miguel county, Colo., on the west front of the San Juan mountains, 2 miles north of Telluride. The vein was discovered in 1876 by Wm. L. Cornett, who, with subsequeilt locators, took up claims along the apex. A few hundred feet of development-work was accomplished, and a few? tons of ore were smelted or milled; but profitable working proved impossible under existing

Jan 1, 1912

Jan 1, 1932

Jan 1, 1900

By Leo J. Vogel, E. D. Hummer

INTRODUCTION by E. D. HUMMER An efficient refuse-disposal system is a necessary part of the modem cleaning plant. The large-scale refuse system and disposal area, engineered for the lifetime of the plant, has become more important due to the greater tonnages of refuse produced from increased quantities of mechanically mined and prepared coal. Laws and increased government regulations have affected the design and operation of disposal systems. THE EFFECT OF MINE AND PLANT OPERATION Refuse disposal starts at the mining face. The mining system, the type of roof support, the machinery used, and the degree of discipline at the face contributes to the amount and type of refuse that must be removed through the disposal system. Economies gained through modification of the mining system or mining machinery may be partially offset by increased dilution of the mined coal with impurities from associated rock formations. In some cases the change in the mining system and equipment has reduced the dilution. In all cases the ratio of impurities that must be removed from the raw-coal feed to the plant not only affects the maintenance and operating costs of the plant, but greatly affects the design of the refuse disposal system. The design of a mine and plant should include the location and the estimated capacity of the disposal areas for the life of the property or plant. Complete evaluation of the disposal system and an estimate of its annual cost of operation over the life of the property or plant should be incorporated in the plant and mine evaluation. Plant design should be as simple as possible, consistent with the efficient production of clean coal. Material transfer points, crushing, screening and pumping operations should be kept to a minimum to reduce degradation and the subsequent increased difficulty and cost of refuse removal. The maintenance of good process control by operating management will result in a minimum of misplaced material in both refuse and clean coal. Reduction of misplaced float material in the plant refuse is an important factor in preventing combustion in the refuse storage pile. THE REFUSE DISPOSAL AREA Combustion in refuse piles occurs when air enters the pile in sufficient quantity to support oxidation. At certain rates of air in-filtration, the heat produced by the oxidation process is not dissipated and temperature rises.

Jan 1, 1968

GOD the Almighty has all things well ordered; in G particular, the effects and attributes of the seven planets whose reign and course (by the grace of God) determine for the most part not only our own life and death but also the growth and decay of vegetable and mineral life, so that the aforesaid planets generate and develop in a wondrous way the ores of gold and other metals in minerals, rocks, and earths. Specifically, the Sun develops the ores of gold, the Moon the ores of silver, Venus the ores of copper, Saturn the ores of lead, Jupiter the ores of tin and bismuth, Mars the ores of steel and iron, and so on. Since, however, no ore is made alone but each is made and wrought so that it is associated with other ores, it is necessary to know the art of separating the thus-made ores after they have become metals; as for instance, silver from lead and copper; gold from silver, and so on. [2]* If this is to be done usefully, you must be able to assay and must understand everything that is needed in connection therewith. It is obviously true and clear as light of day that some kinds of copper contain silver and some kinds of silver contain gold. In order that you may be able to separate them, so that each is obtained by itself and can be worked with profit and re ward you need first of all a true assay for the values of such metal. The assay, by revealing how great they are, whether the pure has been obtained separate from the worthless matter, and what the admixture is, advises you whether it would be worth the expense and the effort to start mining operations. Assaying also indicates how much silver there is in a centner of ore or how much copper and lead there are in

Jan 1, 1949

Jan 1, 1902

By K. L. Komarek, P. F. J. Landler

Synthetic polycrystals of wustite were reduced ilz H2-H2O mixtures over limited roncentration ranges wiltun the wustite. field and the weight changes were continuously followed with a McBain quartz spiral balance. The reduction was. found to be controlled by a combined surface plus solid-state diffusion reaction. The solid-state diffusion had an activation energy of 38 kcal. Self--diflusioities of iron decreased with itzcreasing vacancy concentration. The activation energy of. the surface reaction runs different tor- different samples. The surface reaction-rate constan increased with increasirzg vacancy concentration. THE reduction of the oxides of iron has been studied for many years. Edstroem' has summarized the early work and has provided much information on the reduction of magnetite and hematite by hydrogen and carbon monoxide. More recent summaries are those by smeltzer2 and Themelis and Gauvin.3 Most investigators have reported that the iron metal which forms the outer layer during gaseous reduction is rather porous. According to Kohl and Engel14 the formation of such a porous iron layer depends on the properties of the underlying wiistite layer, on the reaction of the gas with the wustite surface, and on the transport of matter through the wustite layer. McKewan, Quets, Wadsworth, and Lewis, and Knacke 10 have found that, if a porous iron layer is formed, a surface reaction between gas and wustite at the bottom of the pores controls the rate of reaction. Seth and ROSS 11 and Warner 12 have pointed out that the influence of the gaseous pore diffusion through the porous iron layer cannot be neglected. It has further been shown that the wiistite layer formed during reduction is dense and that transport of matter across the layer occurs only by solid-state diffusion of iron ions.13,14 The solid-state diffusion rates observed by Edstroem and Bitsianis 14 and the surface reaction rates observed by Quets eta1.' show that an interaction of the two steps in controlling the reaction rate has to be considered. In this investigation the reduction of wustite was studied with respect to the interaction of the two steps, isolated from any other effects, by reducing wustite within the wustite field from higher to lower oxygen concentrations with H2-H2O gas mixtures. A similar study with CO-CO2 mixtures has been performed by Levin and wagner.15 Fused synthetic wustite polycrystals were reduced in steps of 0.4 wt pct from 24.4 to 23.2 wt pct 0 and over a temperature range from 700" to 1050°C. A few tests were also conducted with reduction steps from 24.4 to 23.6 wt pct 0 and 24.5 to 23.2 wtpct0. The Fe-O phase diagram is shown in Fig. 1 where the composition of the gas phase in equilibrium with the condensed phases is plotted as pct H2 vs the temperature. A careful study of the literature led to the conclusion that the fully drawn equicomposition curves (in wt pct O) in the wustite field used by Edstroem 1,16 and other authors needed some correction. Based on results by Darken and Gurry17 (shown as open circles) and on some of our own data, four corrected curves for 23.2, 23.6, 24.0, and 24.4 wt pct O were calculated (drawn as dashed lines in Fig. 1) which should replace the fully drawn equicomposition curves. MATERIALS AND APPARATUS Materials and Specimen Preparation. Wustite was prepared from iron sulfate (Fisher Scientific Co., New York) which had a purity of over 99.92 pct, with small amounts of manganese, copper, and zinc adding up to 0.03 pct. From the aqueous solution iron oxalate was precipitated and decomposed to magnetite according to Economos. 18 The magnetite powder was pressed into cylinders and sintered in vacuum at 900°C for several hours. The sintered compacts were placed in a platinum crucible of 2.5 cm diam which was fitted into a high-purity alumina crucible and then inserted into the center of the graphite heating element of an electric resistance furnace.lg The furnace was evacuated to below 1 p Hg and the magnetite sample was slowly heated. The evolution of gases during heating deter-

Jan 1, 1967

By David E. Hyatt

The chemical attributes of cyanides have long been exploited in ore pro- cessing schemes for the recovery of copper, molybdenum, gold, silver, and other metal values. Blast furnacing operations are significant unintentional producers of cyanides which find their way into process waters. Many of the more than 20,000 electroplating facilities in the United States utilize cyanide plating baths and generate cyanide containing wastes. As social, political, and economic pressures for water quality attainment, maintenance, and preservation grow, the requirements for the development of treatment technology to control cyanide levels in wastewater become increasingly apparent. Just as the chemistry of the cyanide ion 1s an integral part of its industrial applicability, so must this chemistry be a fundamental part of any decomposition or removal technology used to control its level in effluent or recycled waters. The complexity of this chemistry is substantial and it cannot be considered in a superficial or cursory manner if control system design is to be both efficient and reliable.

Jan 1, 1975

By S. W. Kennedy, M. Cohen, L. D. Calvert

A high-temperature X-ray diffraction method has been used to study the composition and the kinetics of formation of oxide scales at 800 °C on iron and pure iron-nickel alloys containing 25.6, 75, and 84 pct Ni. This technique has been combined with chemical analysis, and metallographic examination, and determination of weight-gain time curves. The 75 and 84 pct Ni alloys form a three-layer scale consisting of porous NiO next to the metal, a spinel layer, and a -Fe203 on the outside. The 25 pct Ni alloy produces a scale of spinel and Fe,O,, in which, however, traces of FeO and NiO are observed near to the metal. On all the nickel alloys the Fe20, is orieqted with the (107) plane parallel to the surfaces. The exposed surface of the Fe20, is in the form of needles whose axis is perpendicular to the specimen surface. Although the alloys show nonuniform oxidation rates as determined from weight-gain measurements, the X-ray data indicate that the total scale and individml scale layers grow uniformly and parabolically. Deep subscale formation is observed in the 25 pct Ni alloy only. This appeared to be associated with cracking of the scale and penetration of the oxygen along the grain boundaries. ALTHOUGH film formation has been investigated by high-temperature electron-diffraction techniques, for example by Gulbransenl and Hickman,' there have apparently been no investigations of scaling by methods permitting study of the scale during formation at the reaction temperature. Methods involving quenching of scales are based on the working assumption that no significant changes take place on cooling. In general, however, compounds may disproportionate, and the different thermal expansions of constituents may cause disruption of the scale on cooling. In particular, some scales cannot be quenched without spalling. These difficulties are avoided by X-ray diffraction examination at the temperature of formation. High-temperature diffraction procedures also provide a method of determining the kinetics of formation of each phase separately in a multicom-ponent scale. The scaling of binary iron-nickel alloys Containing up to 30 pct Ni at a temperature of 800°C has been studied by Benard and Moreau using cooled specimen~,~ whilst Foley, Druck, and Fryxel14 made an electron-diffraction study of cooled oxide films formed on an iron 42 pci Ni alloy. In the present work the scaling of three iron-nickel alloys containing 25.6, 75, and 84 pct by weight of nickel, at 800°C in oxygen at atmospheric pressure was investigated by X-ray diffraction techniques using a Norelco Geiger-counter diffrac-tometer. The oxidation of iron was investigated for comparison. In addition normal metallographic examinations and chemical and X-ray analyses were made, and weight-gain time curves obtained. EXPERIMENTAL Materials Used—The analyses of the alloys were as follows: Percent by Weight Nickel 25.6 pct 75.4 pct 83.2 pct Aluminum 0.004 None found 0.002 Cobalt — 0.05 0.05 Chromium — — — Silicon — 0.01 None found Carbon All less than 0.05 pct The chemical analysis of the iron was: Al— 0.002 i 0.001 pct, C—0.007 pct, Cr less than 0.001 pct, Cu—0.002 ± 0.001 pct, Mn—0.003 ± 0.001 pct, N—0.0002 pct, 0-0.013 pct, P—less than 0.0002 pct, Pb—not detected, S—0.0017 pct, Si—0.0095 pct, Sn—none detected. This iron was the same as that used to make the alloys and was obtained from the same source-Vacuum Metals Corp. One specimen of pure iron from The British Iron and Steel Research Association was used for preliminary investigation. Specimens were machined to shape from cast rod, polished (the final polish being with 600 Sic paper), degreased in trichlorethylene, washed, and etched. The etching and neutralizing procedure adopted by

Jan 1, 1960