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By AIME AIME

CONCIDENT with what promises to be a record-breaking year of activity in the world's greatest iron-ore district is the announcement of plans to hold the regional meeting of the American Institute of Mining & Metallurgical Engineers at Duluth, Aug. 12 to 15 in¬clusive. More than 25 open-pit mines will be in operation in Minnesota's great iron-ore district this year, affording to those attending the convention an unusual op¬portunity of viewing practically side by side the interesting activities of power-shovel operations, railway haulage, truck haulage, conveyor-belt haulage, tower-excavator operations, iron-ore concentration, and underground mining. The ore can be followed from the mines to washing and concentrating plants and to the docks and lake carriers on Lake Superior, where an average of one boat of 10,000 tons' capacity will be loaded and depart every 15 minutes, day and night, during the 1941 shipping season.

Jan 1, 1941

Jan 1, 1940

By J. D. Prater, H. R. Spedden, E. E. Malouf

With the expansion of copper leaching of the various mine wastes at the Kennecott properties, additional copper recovery facilities have been required. A research and development program has been pursued to determine a suitable economic approach to the processing of the additional leach solutions contemplated. lnvestigations on laboratory and pilot plant scales covered electrowinning, solvent extraction, launder and vat type cells, activated launders, precipitation drums, and precipitation cones. This paper contains information on the development and use of a new precipitation-cone-type copper recovery plant, which provides many advantages over older systems. The application of research findings to the old art of leaching copper from copper-bearing mine waste has resulted in a significant contribution of copper to over-all copper production. For example, at the completion of the current expansion program at the Kennecott properties in the United States, copper produced from waste dump leaching will amount to about 25% of the total production. Formerly only 2% was derived from this source. This planned expansion of copper leaching focused attention on the problem of developing more efficient methods for the recovery of copper from greatly increased volumes of copper-bearing solutions.1 The detailed investigations which have been made in laboratory pilot plant and plant tests for the recovery of copper from copper-bearing solutions have included electrowinning, solvent extraction, ion exchange and cementation with iron in launders, precipitation drums, activated launders, and precipitation cones. The results of these investigations have led to the development of a new precipitation cone-type copper recovery system providing many advantages over older methods. ELECTROWINNING OF COPPER FROM COPPER-BEARING SOLUTIONS The direct electrowinning of copper from relatively dilute solutions of copper-bearing mine water, namely solutions containing 10 to 20 lbs of copper per 1000 gal, has always been an attractive possibility.2,3 By this method, high-purity copper powder can be recovered with a power consumption of 3.5 kwh per Ib of copper. However, once the solution strength de-

Jan 1, 1967

By Charles A. Ashburner

At the Philadelphia meeting of the Institute, held in February, 1881,I had the honor of reading a paper on "A New Method of Mapping the Anthracite Coal Fields of Pennsylvania."* At that time the State appropriation for the Second Geological Survey had just expired, and, as a new appropriation was not assured, no detailed plan had been adopted by Professor Lesley, State Geologist, for the practical examination of the mines, and the solution of the geological structure of special localities, or the representation in sections, vertical and columnar, of the general structure of the coal basins and coal beds. I had merely proposed a plan of mapping, as the material for the construction of maps was most available, and it was at that time uncertain what money the Survey would have to enable it to extend the surface and underground explorations, in order to make the examinations complete. After a continuation of the Survey was authorized until January, 1884, by the legislature, in May, 1881, the Anthracite Survey was regularly organized, and a plan adopted for a systematic and exhaustive geological and mine examination of the region. This plan provided for such work, other than that of mapping, as was necessary for a complete and practical geological and mining survey of a coal field. To do any geological work, of however general a character, it was absolutely. necessary that the members of the Survey Corps should obtain unrestricted access to all the mining records of the operators, which have been made with great care and accuracy and at an enormous expense during the past thirty years and more. The unanimous and generous support of the individual and corporate coal operators, of the plan of carrying on the Survey, was promptly assured, on condition that the results should be of such a character as to render them of practical utility to the property-owners and those directly interested. It was hoped

Jan 1, 1883

By Jim F. Lemons

INTRODUCTION A nickel doesn't buy much anymore. That's even true in the cost of recovering nickel -- the commodity. A 5[C] per pound (11 [c] per kilogram) increase in the nickel price won't cover a 10-percent increase in fuel costs for processing laterite ores, nor will it cover a 10- percent increase in wages for recovering nickel from a sulphide ore. It won't even cover a 5- percent increase in the capital cost necessary to mine and process ocean nodules. The basis for this statement and a quantitative analysis of the variations in costs to recover nickel from different types of nickel ores will be discussed in this paper. During the early part of the 1970's, the interest in nickel and its potential development was shifting from Canada to the Pacific Basin area. Canadian growth rate was slowing and each additional increase in nickel capacity was very expensive (Argall, G.O., 1970). Laterite ores were attractive to developers since they were easy to mine at a low labor cost, and technologies were being developed that would allow the recovery of nickel in marketable forms (Mohide, T.P., Warden, C.L., Mason, J.D., 1977). During the last decade, new laterite production was achieved in the Philippines and Botswana, and a significant increase in production from Indonesia and New Caledonia occurred. However, recent reports on nickel identify numerous problems plaguing the industry, i.e., high energy costs that are forcing shutdowns (INCO, 1980), (Mohide, T.P., Warden, C.L., Mason, J.D., 1977), high Canadian sulphide mining labor costs (Anon., 1976), and rapid inflation of nickel capital costs (Anon., 1981b). No definitive study has been made to determine how sensitive the total cost of production is to rising energy, labor, or capital costs, or to identify to what extent increased byproduct revenues could be used to offset these production costs. The purpose of this paper is to quantify the effects of increases in energy, labor, capital costs, and by-product credits on the future cost of production from nickel reserves and/or resources. METHODOLOGY OF ANALYSIS In order to evaluate the sensitivity of nickel production costs to changes in energy, labor, and capital costs, and in byproduct revenues, an analysis was made of existing and proposed nickel operations, their costs, and their sensitivity to change. The data for these analyses were obtained from numerous sources including international govern¬ment and university publications, professional journals, company reports, private communications, U.S. Bureau of Mines contracts, and estimates by Bureau of Mines personnel. These data were collected, in part, as an ongoing effort of the U.S. Bureau of Mines Minerals Availability System (MAS) to systematically measure and classify identified mineral resources according to their respective extraction technologies, economics, and commercial availability. The MAS Program is currently evaluating the present and potential availability of nickel to the United States in relation to mining, beneficiation, smelting, refining, leaching, transportation, infrastructure, environment, land use, labor, productivity, technology efficiencies, operating capacities, deposit life, and political factors. As a summary of this data, the following briefly describes nickel ore types as each relates to energy, labor, capital, and byproducts. Sulphide Operations Nickel is currently available from sulphide deposits. Roughly 55 percent of the current world nickel production in market economy countries is from sulphide ores, although only about 20 percent of the known land-based nickel reserves and/or resources are sulphides (INCO, 1981). In 1979, the Western World sulphide reserves were estimated at about 9.2 million metric tons of nickel (Little, A.D., 1979). Sulphide ores are typically mined underground, thus resulting in high mining costs; however, these ores can often be upgraded by flotation prior to final nickel recovery and require about one-third of the energy required to recover nickel from laterites (Anon., 1981c). In addition, nickel in sulphide ores may be associated with economically recoverable byproducts, which include copper, cobalt, gold, silver, and other precious metals. Laterite Operations Forty-five percent of current nickel production is from laterite deposits. Laterite deposits account for 80 percent of the known land-based nickel reserves and/or resources (INCO, 1981). In 1979, the Western World laterite reserves were estimated at over 35 million metric tons of nickel (Little, A.D., 1979). Nickeliferrous laterites are residual soils formed by weathering, typically under tropical or near tropical conditions. They can be easily mined by open-cut methods, but generally cannot be beneficiated; thus, recovery of nickel must entail processing of the total mined ore. Usually, these ores have high moisture content (20 to 30 percent by weight) that result in additional fuel costs to dry the ore. Nickel silicates, garnierites, are, processed by pyrometallurgical methods; limonite nickel oxides are normally leached. Byproduct cobalt is not recovered from most ferronickel operations, and is only recovered to a limited extent from many leach operations.

Jan 1, 1982

By D. Swan

Industrial research may be defined as a critical and exhaustive investigation to create new and better ways of doing things. The results of industrial research are new and improved products, processes, and techniques. This broad definition, of course, covers investigation of all subjects by either individuals or groups of people, and this chapter aims to examine the purpose (what research tries to do), and methods (or how research is done) as applied in the mineral industries. Concepts and History The idea or concept of organized research probably originated in the universities of Europe. There, groups of scholars banded together for discussion and application of their particular specialty to a common problem. Publication of the conclusions drawn from such investigations gave scholars in other areas the opportunity to review and criticize the work of their colleagues, and one of the hallmarks of scientific research work is the publication and criticism of the results of the investigation. It was not until the late nineteenth century that the concept of organized research for the profit of industry was recognized. During the late nineteenth and early twentieth centuries, a large number of industrial enterprises sponsored organizations to study the application of the physical sciences with the aim of making discoveries that would result in profit to the sponsoring organization. The tangible benefits accruing from these activities were so great that they, in turn, fostered several other methods for the support of organized research activities. For the large problems involving public interest, United States Government scientific re- search laboratories were set up. As the demand of smaller enterprises for research activities increased, research institutes and consulting laboratories were organized. In Europe the idea of common industry sponsorship of research centers grew and many large research organizations there were sponsored by associations of manufacturers. Finally, in the United States

Jan 1, 1959

By Persifor Frazer

At a time when all those interested in the iron trade are carefully scanning the horizon for new sources of the raw material, a few words concerning a field, which though not new, has not been hitherto fruitful of statistical information, may be deemed appropriate at this meeting. The district alluded to is the belt of the Middle James River, or in other words, that portion of the ferriferous belts of Virginia lying between Josua Falls and the little settlement of Norwood, in the counties of Amherst and Nelson, and on the left bank of the James River. This region shows unmistakable signs of developing a very considerable market for iron ores and for iron in the future, as well as a tempting appearance of possible productiveness in the former. It, is extremely hazardous to deal in generalizations as to the productiveness or non-productiveness of these measures without a more thorough development than has yet been attained. It is true that they probably constitute an horizon whence comes a part of the marvellous mineral wealth of the northern peninsula of Michigan. But

Jan 1, 1883

By D. L. Rainey, E. R. Goter, W. R. Hudspeth

THE area in which spodumene-bearing pegmatites occur extends from Gaffney, S. C., in a northerly direction to Lincolnton, N. C., a distance of about 16 miles. The zone averages 2 miles in width. Interest in this area was first aroused by the discovery of small amounts of cassiterite in the pegmatites and in greissen which occurs on the walls of some of the pegmatites. Attempts were made from 1880 into the 1920's to mine and concentrate cassiterite, but there were no successful operations. In 1935 L. M. Williams became interested in the area and began prospecting by trenching and sinking several small shafts. He gradually gained control of a considerable acreage south of the city of Kings Mountain, N. C. Mr. Williams states that he produced some ore from a shaft which he shipped to the Maywood Chemical Co. in the late 1930's. In 1937 G. H. Chambers of the Foote Mineral Co. visited the area and examined several properties, but the lithium market was too small to support the necessary concentrating plant.

Jan 9, 1953

By B. G. Klugh

In a paper before the Institute at Wilkes-Barre, Pa., June, 1911,' Mr. James Gayley discussed the application of this process to iron-bearing materials. The same author² described the results of operations at the plant at Birdsboro, Pa. The purpose of the present paper is to present further discussion of some techuical details involved in the operation of this plant, and of the theoretical and practical relations of this product to blast-furnace practice. Since Oct. 1, 1911, the Birdsboro plant has been in operation at the blast-furnace of the E. & G. Brooke Iron Co. The results have been highly satisfactory, although the material treated, being chiefly the flue-dust currently made by the furnace or taker] from the accumulated stock-pile, was excessively high, and yet not uniform, in carbon, so that the desirable control or regularity of the amount of fuel in the mixture treated could not be maintained. Nothing could more forcibly demonstrate the flexibility of the process than the fact that, under these conditions, the sinter produced was, in all cases, of excellent quality. The Dwight & Lloyd process, as such, slid its present highly-developed mechanical appliances were described by Mr. Gayley in the paper above mentioned. While the repetition of some particulars will be unavoidable in this paper, it will be confined to features bearing upon the metallurgical principles involved. According to the principle of the process, the finely-divided iron-bearing material to be sinterecl is intimately nlixed with

Jan 1, 1913

By E. G. Williams

Manganese-ore has been found upon the Isthmus of Panama throughout' a region of nearly three hundred square miles, over the greater part of which, however, it is known only in small bodies without commercial value. Only six mines, controlled by two companies, have actually shipped ore, although a large area has been taken up in miningelaims. The ore-bearing region extends along the coast of the Carib. bean Sea, beginning on the west near Puerto Bello and extending easterly about 35 miles toward Point San Blas. Ore has been discovered in the interior, at a maximum distance of about 10 m. from the coast. Fig. 1 is a map of a portion of the Isthmus

Jan 1, 1903

By Frank J. Markewicz, William Lodding

Greensand, greensand marl, and green earth are names given to sediments rich in the bluish green to greenish black mineral known as glauconite by the mineralogist. The word glauconite is from the Greek word glaukos, meaning bluish green. The term "greensand" as a rock name for a glauconite-bearing sediment is more appropriate than "greensand marl," a term that has been doggedly perpetuated in the literature. Because of its potash and phosphate content, greensand was dug and marketed as a fertilizer and soil conditioner for more than 100 years. The advent of prepared fertilizers with adjustable nutrient ratios led to the decline of green- sand for agricultural application. The material has since been recognized for use in water treatment. Unfortunately, in spite of large reserves and worldwide distribution, the mineral has not been utilized to any significant commercial extent because no major application has been found for a substance with its chemical composition and properties. This lack is probably due to a paucity of research on its potential commercial application. Extraction of potash received considerable attention during and just after World War I. Because of relatively high extraction costs and generally low potash content (up to 8%), glauconite lost its appeal as a source of this commodity. Historical Background Greensand was used as a fertilizer in New Jersey in the latter part of the 1700s. During the early 1800s its use became more common; applications of up to 100 tons per acre were sometimes made, although recommendations for agricultural use suggested 20 to 50 tons per acre (Tedrow, 1957). Many crops, especially the forage type, were said to improve with greensand application; however, because of slow release of potash, large quantities were required. Certain greensands that contain sulfur and sulfide minerals are harmful to plant growth, and these were classified as "poison," "burning," or "black marls." The availability of higher-grade potash salts from other mineral sources, and the manufacture of prepared fertilizers, displaced the agricultural use of green- sand during the later 1800s. During the mid-1800s the domestic greensand industry, centered in a small section of the eastern United States, grossed more than $500,000 per year. Toward the end of the century, annual production had dwindled to less than $100,000. By 1910 there were only six or eight greensand producers, grossing less than $5000 (Tyler, 1934). There was a small revival in the industry during World War I because of the curtailment of foreign potash, especially from Germany. During the later 1940s and early 1950s greensand was again recommended as a food nutrient for plants and farm crops. Agronomic studies discussed its potential as a soil additive that gradually releases potash and many trace- element nutrients essential for plant growth (Tedrow, 1957). Greensand was sold with the idea that it would condition soil and absorb and hold water while its base-exchange properties would release trace elements. For a short time glauconite was utilized in certain parts of New Jersey as a binding additive in the brick industry, and in the 1800s for making green glass (Cook, 1868). In the early 1900s the base-exchange property of glauconite was recognized for water treatment, and the mineral gained acceptance as a water softener. Mansfield ( 1922) does not mention base-exchange; however, the base ex-

Jan 1, 1975

By Homer Turner

THE nature and comparative features of anthracite and bituminous coals have been discussed by the writer in two previous papers.1 Although this paper is offered as a further contribution to the subject, it seems desirable at the outset to repeat some of the descriptive matter of the early works in order to show the actual connection between various constituents of both coals and the new photomicrographs and other physical and chemical properties.

Jan 1, 1929

By R. M. Larsen

The Rocky Mountain region is defined with some variations for different purposes or by different organizations. For oil and gas development, Wyoming, Montana, Colorado, northwestern New Mexico, and Utah are included in the order of their apparent importance. Portions of adjoining states, such as North and South Dakota, Nebraska, Arizona, Nevada, and Idaho, arc attributary to this region, but have little or no oil or gas production. Nebraska and New Mexico are considered separately (see pp. 412 and 415), and most of the discussion in this report will be confined to Colorado, Montana, and Wyoming. Utah has produced about 200,000 bbl. of oil from the San Juan and Virgin fields, which are isolated and shut in at present. The Clay Basin field in northeastern Utah produces natural gas and distillate, and the Farnham field in central Utah produces carbon dioxide gas. Other Utah areas of some interest are listed in Table I. The Cedar Creek (Baker-Glendive) field in southeastern Montana extends into North Dakota, but is listed under Montana. The other states are in the main wildcat areas, and exploration in 1944 was at a minimum. However, geological and geophysical parties are reviewing them for further testing. Oil production in Colorado, Montana and Wyoming was 459,000 bbl. more than in 1943. Increases of 713,000 bbl. in Colarado and 731,000 bbl. in Montana offset a loss of 985,000 bbl. in Wyoming. This was the first decline in Wyoming since 1938. Field production figures and state totals are given in Table I. Total drilling activities in these three states and Utah increased from 687 wells making 1,442,511 ft. of hole in 1943 to 916 wells making 2,245,803 it. in 1944. Wildcat drilling increased from 163 wells making 331,193 ft. of hole in 1943 to 171 wells making 389,144 it. in 1944. These figures include all drilling wells making footage, not starts or completions, and represent an all-time high in drilling. The year 1944 witnessed the greatest concentration of seismograph activity that the region has had. The Rocky Mountain Oil Scouts Association reported that in 1943, the previous peak year, 91 crew months of work were performed; in 1944, the time was 254 crew months. About 67 per cent of the work was in Wyoming, 18 per cent in Montana, and 12 per cent in Colorado. Twenty-three blocks totaling 400,000 acres were reported assembled in Colorado, and 161 blocks totaling 4,000,000 acres in Wyoming. Information about other states was not given. Fourteen unit agreements were approved by the Department of the Interior, as compared with 13 in 1943. The 1944 agreements were all in Wyoming. In five of the unit areas, oil or gas discoveries were made, four were dry, and five were drilling Or pending' Oil companies find it advantageous to unitize blocks containing any proportion of public domain. Units for

Jan 1, 1945

By J. J. Rutledge

On Sept. 4, 1914, Mine No. 1 of the Union Coal Co., Adamson, Oklahoma, suddenly caved, entombing thirteen miners whose bodies were never recovered. The seam of coal mined, the Lower Hartshorne, averaged 5 ft. in thickness and dipped at an angle varying from 22" to 30n. The strata overlying the coal seam were sandstones and shales. The mine was worked by the pillar-and-room method, the rooms being driven directly up the dip of the seam. All coal was blasted off the solid. Rooms were turned on short centers and room pillars were thin and irregular, as shown in Fig. 1. Fig. 2 is a cross-section of the form; showing the mine workings. Some cracks had been observed on the surface, it is said, at least a month before the squeeze occurred, but the collapse of the mine workings came very suddenly. As is usual when squeezes occur on such steep dips and the pillars fail, the crush progressed rapidly down the dip until it reached solid coal; there was a line of break, or draw, over in the solid coal. Several well-defined cracks appeared on the surface, after the mine had squeezed, but there was no appreciable subsidence of the surface, the weight seemed to be thrown entirely to the dip. About one year after the squeeze, and after the workings of the adjoining mine, NO. 4, had been retimbered and made safe, the writer inspected the tenth north (right) entry, or lift, off of No. 4 slope, which was below and fairly near the lowest caved portion of mine No. 1. The roof shale was composed of thin layers, which had been bent in somewhat the same manner as the leaves of a book having flexible covers are bent when the book is folded or rolled up in the hands. Though the mine workings are immediately beneath the streets and buildings of the mining town of Adamson, business was not disturbed by the squeeze, so far as any subsidence of the surface was concerned. No surface monuments were available and no elevations were taken, but the mine workings had been accurately surveyed and traversed, and the streets of the town overlying the mine workings had been carefully platted on the mine map, so that it was possible to locate accurately the cracks on the surface.

Jan 1, 1923

By J. J. Rutledge

On Sept. 4, 1914, Mine No. 1 of the Union Coal Co., Adamson, Oklahoma, suddenly caved, entombing thirteen miners whose bodies were never recovered. The seam of coal mined, the Lower Hartshorne, averaged 5 ft. in thickness and dipped at an angle varying from 22" to 30n. The strata overlying the coal seam were sandstones and shales. The mine was worked by the pillar-and-room method, the rooms being driven directly up the dip of the seam. All coal was blasted off the solid. Rooms were turned on short centers and room pillars were thin and irregular, as shown in Fig. 1. Fig. 2 is a cross-section of the form; showing the mine workings. Some cracks had been observed on the surface, it is said, at least a month before the squeeze occurred, but the collapse of the mine workings came very suddenly. As is usual when squeezes occur on such steep dips and the pillars fail, the crush progressed rapidly down the dip until it reached solid coal; there was a line of break, or draw, over in the solid coal. Several well-defined cracks appeared on the surface, after the mine had squeezed, but there was no appreciable subsidence of the surface, the weight seemed to be thrown entirely to the dip. About one year after the squeeze, and after the workings of the adjoining mine, NO. 4, had been retimbered and made safe, the writer inspected the tenth north (right) entry, or lift, off of No. 4 slope, which was below and fairly near the lowest caved portion of mine No. 1. The roof shale was composed of thin layers, which had been bent in somewhat the same manner as the leaves of a book having flexible covers are bent when the book is folded or rolled up in the hands. Though the mine workings are immediately beneath the streets and buildings of the mining town of Adamson, business was not disturbed by the squeeze, so far as any subsidence of the surface was concerned. No surface monuments were available and no elevations were taken, but the mine workings had been accurately surveyed and traversed, and the streets of the town overlying the mine workings had been carefully platted on the mine map, so that it was possible to locate accurately the cracks on the surface.

Jan 1, 1923

By L. VOGELSTEIN

OUTSTANDING among the year's events in copper has been the reimposition of an import duty of 4r. per pound in this country which became effective June 21. In consequence of this action by Congress, the Ottawa Empire conference recommended a duty of 2d. per pound equivalent at normal rate of exchange to our 4c. duty, on all copper originating outside of the Empire. Lip to the middle of this year only Russia and Japan had a closed market; the import duty on copper in Russia is 30 per cent ad valoremm and in Japan about 2c. Russia's consumption has always been in excess of production and she has imported from 2(1,000 to 40,000 ton, of copper per annum. Japan, with a production of 6,000 to 7,000 tons per month, has absorbed, in normal times, its production, but during recent: sears has exported varyiug quantities in 1929. 2,200 ton-: in 1930, 2,700 tons, and in 1931. 3,600 ton-. Aside from the-e two countries, the international market has heretofore been free. It and when the British Empire duty become, effective the world's markets will be divided into four unit: 1. Russia and Japan, 2. United States. 3. British Empire. 4. Rest of the world. The world's production at present is rennin it the rate of 930.000 tons per annum. This year's production will be over 1,000,000 tons because the several curtailment did not become effective until the second quarter. consumption will be slightly in excess. Deducting from 30,000 tons Russia's and Japan's production of 121.000 tons, 806,000 tons is left divided a, follows:

Jan 1, 1932

By E. A. Gulbransen, J. W. Hickman

ONE of the important factors that determine the resistance of a metal or alloy to further chemical reaction is the structure of the superficial oxide film A thorough understanding of the physical and chemical structure as well as the stability of the oxide film formed on the surface as a function of time and temperature of the chemical reaction might furnish clues as to the nature of the reaction process and the protective nature of the film A comprehensive program has been undertaken to study these phenomena This paper summarizes the structure of the oxide films formed on the metals iron, cobalt, nickel, chromium and copper at temperatures up to 700°C Before the introduction of the electron diffraction technique, it «as necessary to use either direct chemical analyses or X-ray diffraction analyses to determine the nature of the oxide film formed on the metal or alloy Chemical analyses yields information on the percentages of the several atomic species present in the film while X-ray diffraction analyses yield information on the atomic geometry In special cases the information obtained may be identical, but in general both view-points are necessary Much of, the early work was carried out on the oxidation of bulk samples where thick films were obtained The products were identified after cooling to room temperature by X-ray diffraction and chemical analyses Although much useful information has been obtained in this manner, little could be learned about the character of the protective oxides during the period when the films were actually protective Evidence concerning the chemical structure of thin oxide films has been made possible by the development of the electron diffraction reflection technique In this method the most fruitful investigations have been made by carrying out the reaction in situ at the temperature at which the film is actually protective LITERATURE The oxidation of iron has been extensively investigated by X-ray and electron diffraction Jackson and Quarrell1 found that oxide films formed and examined at the same temperature differed considerably from those allowed to cool to room temperature The results showed that below 400°C the oxide that was stable in intimate contact with iron was Fe304, between 515° and 900°C the stable film was FeO Above the upper change point of iron the oxide was found to be Fe304 prom 400° to 515°C , FeO, Fe304 or a mixture of the two oxides was found Recrystallization of the air-formed film below 400° and above 900°C led to the formation of Fe304 In the range where thicker films consisted of FeO, the air-formed film was converted to a new hexagonal oxide not previously described

Jan 1, 1946

By J. W. Hickman, E. A. Gulbransen

One of the important factors that determine the resistance of a metal or alloy to further chemical reaction is the structure of the superficial oxide film. A thorough understanding of the physical and chemical structure as well as the stability of the oxide film formed on the surface as a function of time and temperature of the chemical reaction might furnish clues as to the nature of the reaction process and the protective nature of the film. A comprehensive program has been undertaken to study these phenomena. This paper summarizes the structure of the oxide films formed on the metals iron, cobalt, nickel, chromium and copper at temperatures up to 700°C. Before the introduction of the electron diffraction technique, it was necessary to use either direct chemical analyses or X-rav diffraction analyses to determine the nature of the oxide film formed on the metal or alloy. Chemical analyses yields information on the percentages of the several atomic species present in the film while X-ray diffraction analyses yield information on the atomic geometry. In special cases the information obtained may be identical, but in general both viewpoints are necessary. Much of the early work was carried out on the oxidation of bulk samples where thick films were obtained. The products were identified after cooling to room temperature by X-ray diffraction and chemical analyses. Although much useful information has been obtained in this manner. little could be learned about the character of the protective oxides during the period when the films were actually protective. Evidence concerning the chemical structure of thin oxide films has been made possible by the development of the electron diffraction reflection technique. In this method the most fruitful investigations have been made by carrying out the reaction in situ at the temperature at which the film is actually protective. Literature The oxidation of iron has been extensively investigated by X-ray and electron diffraction. Jackson and Quarrelll found that oxide films formed and examined at the same temperature differed considerably from those allowed to cool to room temperature. The results showed that below 400°C the oxide that was stable in intimate contact with iron was Fe³O4; between 515° and 900°C. the stable film was FeO. Above the upper change point of iron the oxide was found to be Fe³O4. From 400' to 515°C., FeO, Fe³O4 or a mixture of the two oxides was found. Recrystallization of the air-formed film below 400' and above 900°C. led to the formation of Fe3O4. In the range where thicker films consisted of FeO, the air-formed film was converted to a new hexagonal oxide not previously described.

Jan 1, 1947

By E. A. Gulbransen, J. W. Hickman

One of the important factors that determine the resistance of a metal or alloy to further chemical reaction is the structure of the superficial oxide film. A thorough understanding of the physical and chemical structure as well as the stability of the oxide film formed on the surface as a function of time and temperature of the chemical reaction might furnish clues as to the nature of the reaction process and the protective nature of the film. A comprehensive program has been undertaken to study these phenomena. This paper summarizes the structure of the oxide films formed on the metals iron, cobalt, nickel, chromium and copper at temperatures up to 700°C. Before the introduction of the electron diffraction technique, it was necessary to use either direct chemical analyses or X-rav diffraction analyses to determine the nature of the oxide film formed on the metal or alloy. Chemical analyses yields information on the percentages of the several atomic species present in the film while X-ray diffraction analyses yield information on the atomic geometry. In special cases the information obtained may be identical, but in general both viewpoints are necessary. Much of the early work was carried out on the oxidation of bulk samples where thick films were obtained. The products were identified after cooling to room temperature by X-ray diffraction and chemical analyses. Although much useful information has been obtained in this manner. little could be learned about the character of the protective oxides during the period when the films were actually protective. Evidence concerning the chemical structure of thin oxide films has been made possible by the development of the electron diffraction reflection technique. In this method the most fruitful investigations have been made by carrying out the reaction in situ at the temperature at which the film is actually protective. Literature The oxidation of iron has been extensively investigated by X-ray and electron diffraction. Jackson and Quarrelll found that oxide films formed and examined at the same temperature differed considerably from those allowed to cool to room temperature. The results showed that below 400°C the oxide that was stable in intimate contact with iron was Fe³O4; between 515° and 900°C. the stable film was FeO. Above the upper change point of iron the oxide was found to be Fe³O4. From 400' to 515°C., FeO, Fe³O4 or a mixture of the two oxides was found. Recrystallization of the air-formed film below 400' and above 900°C. led to the formation of Fe3O4. In the range where thicker films consisted of FeO, the air-formed film was converted to a new hexagonal oxide not previously described.

Jan 1, 1947

Jan 1, 1932