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By G. R. Gardner, D. H. Davis

Increasing realization of the importance of dust control, and the recommendations of various agencies, have led the mining industry to become actively concerned with this problem. The background and necessity for adequate dust-suppression measures have been discussed in a number of publications, including those of the U. S. Bureau of Mines, and the use of spray water to reduce dust at the face and on roadways has been recommended. The problem resolves itself into obtaining adequate dust reduction at a reasonable cost. Inasmuch as the term "adequate dust suppression" has never been clearly defined, nor have permissible limits of dustiness (in terms of dust count) been established, it is apparent that any method selected may be required to meet additional demands. Until the industry has been given some indication of permissible limits of dustiness, no permanent solution is possible. Progress will be somewhat handicapped until such information is available. In addition, dust reduction must be obtained without the addition of any excessive moisture to the coal, since consideration must often be given to: I. Quality standards, particularly reduction in heat value. 2. Handling characteristics, particularly in regard to unloading from railroad cars and bins. 3. Application of dry methods of coal cleaning. 4. Necessity for fine screening within specified limits of oversize and undersize. Little detailed information is available as to the advantages and disadvantages of the several methods of water distribution, the location and protection of sprays, operating data on pressure, quantity of water, and so forth, and results obtained. In 1940 an investigation was undertaken to determine and evaluate the principal factors involved. This paper constitutes a progress report on this work and cannot in any way be regarded as complete on any one of the several phases. Classification of Dust Sources The various sources of underground dust may be classified as primary or secondary. A primary source is one associated with appreciable degradation of size, that is, where the greater part of the actual fines capable of becoming air-borne dust are produced. A secondary source may be considered as one in which the greater part of the fines have been produced at some previous operation and are in such condition that they can be dispersed as air-borne dust. These conceptions appear to be of practical significance, as experience indicates that when dust is controlled at the primary sources the importance of secondary sources is minimized. For these reasons, investigations to date have been concerned principally with the primary sources of dust, and this paper is concerned particularly with one of these—namely, undercutting. In accord with the foregoing definitions, the sources to which the following opera-

Jan 1, 1942

By G. R. Gardner, D. H. Davis

Increasing realization of the importance of dust control, and the recommendations of various agencies, have led the mining industry to become actively concerned with this problem. The background and necessity for adequate dust-suppression measures have been discussed in a number of publications, including those of the U. S. Bureau of Mines, and the use of spray water to reduce dust at the face and on roadways has been recommended. The problem resolves itself into obtaining adequate dust reduction at a reasonable cost. Inasmuch as the term "adequate dust suppression" has never been clearly defined, nor have permissible limits of dustiness (in terms of dust count) been established, it is apparent that any method selected may be required to meet additional demands. Until the industry has been given some indication of permissible limits of dustiness, no permanent solution is possible. Progress will be somewhat handicapped until such information is available. In addition, dust reduction must be obtained without the addition of any excessive moisture to the coal, since consideration must often be given to: I. Quality standards, particularly reduction in heat value. 2. Handling characteristics, particularly in regard to unloading from railroad cars and bins. 3. Application of dry methods of coal cleaning. 4. Necessity for fine screening within specified limits of oversize and undersize. Little detailed information is available as to the advantages and disadvantages of the several methods of water distribution, the location and protection of sprays, operating data on pressure, quantity of water, and so forth, and results obtained. In 1940 an investigation was undertaken to determine and evaluate the principal factors involved. This paper constitutes a progress report on this work and cannot in any way be regarded as complete on any one of the several phases. Classification of Dust Sources The various sources of underground dust may be classified as primary or secondary. A primary source is one associated with appreciable degradation of size, that is, where the greater part of the actual fines capable of becoming air-borne dust are produced. A secondary source may be considered as one in which the greater part of the fines have been produced at some previous operation and are in such condition that they can be dispersed as air-borne dust. These conceptions appear to be of practical significance, as experience indicates that when dust is controlled at the primary sources the importance of secondary sources is minimized. For these reasons, investigations to date have been concerned principally with the primary sources of dust, and this paper is concerned particularly with one of these—namely, undercutting. In accord with the foregoing definitions, the sources to which the following opera-

Jan 1, 1942

By Worthen Bradley, R. G. Hall

THIS paper will attempt to show how a metallurgical problem at one California quicksilver mine was solved, and how the solution was applied successfully at another mine. The pronouns "we" and "our," as used below, refer to the Bradley Mining Co. of San Francisco. The term "concurrent firing" for the purpose of this paper can be defined as feeding and firing a rotary kiln at the same end-that is, of course, the upper end. This is as opposed to "counter-current firing," the orthodox method, in which a kiln is fed at the upper and fired at the lower end. The terms "quicksilver" and "mercury" are used interchangeably. EARLY REFERENCES The earliest work on nonferrous metallurgy, we believe, was The Pirotechnia of Vannocio Biringuccio,1 its first edition having been printed in Italy in 1540. Quoting from its chapter entitled "Concerning Quicksilver and Its Ore": Quicksilver . . . is one of the gods and has divine strength in itself, and also, to the annoyance of the alchemists, it is winged. Hence, when it sees that it is in gravest danger, it loosens itself from . . . every bond . . . and flies away into the heavens, escaping from the hands of those who crucify it. Almost laughing, it leaves all its adversaries mocked and scorned, with their phials and filters empty . . . How thorough a job, under certain conditions, it can do of mocking its adversaries and leaving their phials and filters empty, was found out four centuries later at the Sulphur Bank mine, on the east shore of Clear Lake, in Lake County, California. The other mine mentioned in the title is the Reed, in Yolo County, California, 35 miles by road southeast of Sulphur Bank. Reed and Sulphur Bank ranked respectively fifth and seventh in U. S. production in 1943. The earliest direct reference we can find to furnacing troubles at these mines was by Thomas Egleston in 1890.2 Speaking of Sulphur Bank, Egleston says: Sometimes there is more sulphur than cinnabar in the ore, which is a detriment to both . . . making the sulphur impure, and rendering the cinnabar difficult to work on account of the soot. In some of the early . . . furnaces the accumulation of soot from the excess of sulphur has been known to penetrate as far as the fan blower at the end of the . . . condensers, and completely prevent its revolution. In order to get rid of the inconvenience of this accumulation . . . , as well as to get a commercial value from the sulphur, it (the sulphur) is now separated by steam and sold. It is claimed that the sulphur alone pays all the expenses of . . . the mine. The mine was first worked for sulphur, and the cinnabar it contained was considered to be an inconvenience, and was carefully picked out and thrown away. as its richness and value were not

Jan 1, 1945

By A. G. Roach

THIS paper deals with a plant built under joint agreement between the Canadian and United States Governments to supply the strategic mineral, corundum, at a time when African production was dwindling and war demands still increasing. The operation began in September 1944, retreating the tailings from a former mill by gravity methods, and is still in production (Sept. 1946). In 1942, when it became apparent that South African production would be insufficient to meet mounting wartime requirements of corundum, a survey was made of Canadian sources of the mineral, at the request of the Foreign Economic Administration of the U. S. Government. The investigation1 indicated that the quickest and cheapest supply would be obtained by reworking the tailings deposit at Craigmont, Ontario. Sampling of the dump by Canadian Government engineers revealed that 125,000 tons of tailings, averaging 2.96 pct corundum, was available for retreatment. Ore-dressing tests on representative samples of the deposit were conducted by the writer in the laboratories of the Industrial Minerals Section of the Department of Mines and Resources at Ottawa; and gravity concentration on tables was indicated as the most suitable method of treatment. Decision to proceed with the project was deferred until May 9, construction was begun on May 18, and tune-up operation of the plant begun on Sept. 15, 1944. CORUNDUM-ITS PROPERTIES AND USES Corundum is an oxide of aluminum having the formula A1203. Its outstanding characteristic is its great hardness; 9 in the Mohs scale. In this respect it is second only to the diamond. It usually occurs in barrel-shaped crystals in nepheline syenites and other feldspathic rocks deficient in silica. It has a specific gravity of 3.95 to 4.1 and is insoluble and infusible. In color it ranges from white, through red and green, to black. Ruby and sapphire are gem varieties of corundum. Corundum is supplied to industry as closely graded grain.2 The coarser products (10 to 24-mesh) are used largely for snagging wheels in the steel-castings industry, while the finer grades (from 70-mesh down to flours) find a wide application in the polishing of lenses and for other uses in the optical trade. All sizes of corundum grain are in close competition with synthetic abrasives such as carborundum and alundum. In some fields of application the artificial product is superior to the natural grain but not in all. The shape of the particle and its behavior under conditions of actual use determine its sphere of employment. The United States is the largest consumer of corundum, annual consumption in peacetime approaching 3000 tons; during the war this figure was roughly doubled. During the years 1902 to 1913, the bulk

Jan 1, 1946

By Boyd Guthrie, J. D. Lankford

A progress report on the oil-shale and shale-oil processing research program at the U. s. Bureau of Mines Oil-Shale Demonstration Plant. Legislation providing for the program and aims are briefly noted. The remoteness and rugged nature of the terrain at the plant site are important factors in construction and operations. Large-scale units now in operation are the crushing plant and two 40-ton N-T-U retorts. These are described in detail. Under construction are several retorting pilot plants and a 200 bbl per day refinery. The refineiy incorporates several types of thermal operation, three-stage low-temperature acid treating, doctor sweetening and rerunning. Data are presented on typical N-T-U retort runs. Yields of 90 to loo pct of assay are realized on 30 gal to the ton shale with a retort cycle time of 18 hr. Data also are presented showing a comparison of a Mid-Continent petroleum and N-T-U shale oil. This comparison indicates that shale oil has a high pour point, low API gravity, and contains about 0.8 pct sulphur and 2 pct nitrogen. The naphtha fraction contains 3 pct tar acids, 9 pct tar bases and jo pct olefins. The problems involved in refining shale oil into usable products are discussed in detail. Introduction The Bureau of Mines oil-shale program now under way at Rifle, Colo., was begun in July 1944 under the provisions of the Synthetic Liquid Fuels Act, which was passed in the spring of that year under the sponsorship of Senator Joseph C. O'Ma-honey of Wyoming and Congressman Jennings Randolph of West Virginia, aided by Michael W. Straus, former Assistant Secretary of the Interior, and others. The oil-shale plant is only a part of the Office of Synthetic Liquid Fuels, Bureau of Mines, which has under way projects to develop synthetic liquid fuels from coal and other solid materials at Pittsburgh and Bruceton, Pa., Morgantown, W. Va., Louisiana, Mo., as well as the Petroleum and Oil-Shale Experiment Station at Laramie, Wyo., and the oil-shale demonstration plant at Rifle. The oil-shale program is entirely experimental. It is not intended that oil will be produced in great quantities. Production will be limited to the volume obtained from plant-scale experimental operations, which will be kept to the minimum size needed to develop techniques and processes and to demonstrate costs. After the passage of the enabling act in the summer of 1944 a survey of the oil-shale resources of the Nation was made to determine the most suitable general area in which to establish the demonstration plant. The most suitable area was found to be in the Rifle-De Bequearea in Garfield County, western Colorado. Bureau of Mines field parties covered this entire area thoroughly

Jan 1, 1949

By J. H. Richards, G. Derge, W. Peifer

A WIDE Variety of metallurgical defects in steel have commonly been attributed to the presence of excessive amounts of hydrogen. These defects include flakes in rails and forgings, cracks in welds, and blisters in enameled ware, They have been related to hydrogen largely by circumstantiat evidence because the proper sampling and analysis of steel for hydrogen has been known to be difficult and because no general agreement has existed with regard to the relative suitability and accuracy of available methods. The need for a direct approach to these problems has been widely recognized. This general situation has been well described in the publications of the British committee on the Heterogeneity of Steel Ingots,' and current approaches to the problem were reviewed in a recent symposium of the AIME.I2 The plans described by the present authors at that meeting have now matured satisfactorily and will form the basis of this paper. The principal object of this paper will be to describe the methods of sampling and analysis which have been developed and to illustrate the usefulness and limitations of these methods by citing their application to a specific problem, The first problem selected for investigation was the behavior of hydrogen in rail steel. This was chosen because the occurrence of shatter cracks in rails has received a great deal of study over a long period of time. The defect can be controlled by the expensive procedure of slow in However, it may be hoped that a better understanding of the factors influencing the hydrogen content of rails will lead to a more efficient control of this problem. Rails provide a good starting point for a more general study of hydrogen in steel because they provide a cross-section large enough to develop cracks, Yet small enough for convenient handling and sampling. Rails were also selected because they arc made from plain carbon steel and it was felt that the initial work should not be complicated by the effects introduced by alloying elements. The considerations which determined the original planning of this study should be reviewed. The inherently complex nature of most hydrogen problems requires that a large amount of data must be collected for any particular case. This in turn means that any analytical procedure should be as rapid and simple as possible. The same objective of speed is indicated by the fact that it may finally become desirable to use hydrogen analysis in process control. It is also known that hydrogen is highly fugitive and that any procedure which facilitat~s early analysis of the sample without prolonged or irregular storage has distinct advantages. The most important previously reported methods of analysis may be classified into three general groups: (I) Vacuum fusion, (2) Vacuum extraction (without melting), (3) Total combustion.

Jan 1, 1949

By G. Derge, W. Peifer, J. H. Richards

A WIDE Variety of metallurgical defects in steel have commonly been attributed to the presence of excessive amounts of hydrogen. These defects include flakes in rails and forgings, cracks in welds, and blisters in enameled ware, They have been related to hydrogen largely by circumstantiat evidence because the proper sampling and analysis of steel for hydrogen has been known to be difficult and because no general agreement has existed with regard to the relative suitability and accuracy of available methods. The need for a direct approach to these problems has been widely recognized. This general situation has been well described in the publications of the British committee on the Heterogeneity of Steel Ingots,' and current approaches to the problem were reviewed in a recent symposium of the AIME.I2 The plans described by the present authors at that meeting have now matured satisfactorily and will form the basis of this paper. The principal object of this paper will be to describe the methods of sampling and analysis which have been developed and to illustrate the usefulness and limitations of these methods by citing their application to a specific problem, The first problem selected for investigation was the behavior of hydrogen in rail steel. This was chosen because the occurrence of shatter cracks in rails has received a great deal of study over a long period of time. The defect can be controlled by the expensive procedure of slow in However, it may be hoped that a better understanding of the factors influencing the hydrogen content of rails will lead to a more efficient control of this problem. Rails provide a good starting point for a more general study of hydrogen in steel because they provide a cross-section large enough to develop cracks, Yet small enough for convenient handling and sampling. Rails were also selected because they arc made from plain carbon steel and it was felt that the initial work should not be complicated by the effects introduced by alloying elements. The considerations which determined the original planning of this study should be reviewed. The inherently complex nature of most hydrogen problems requires that a large amount of data must be collected for any particular case. This in turn means that any analytical procedure should be as rapid and simple as possible. The same objective of speed is indicated by the fact that it may finally become desirable to use hydrogen analysis in process control. It is also known that hydrogen is highly fugitive and that any procedure which facilitat~s early analysis of the sample without prolonged or irregular storage has distinct advantages. The most important previously reported methods of analysis may be classified into three general groups: (I) Vacuum fusion, (2) Vacuum extraction (without melting), (3) Total combustion.

Jan 1, 1949

By B. N. Bose, M. F. Hawk

SINCE Davenport and Bain' introduced the isothermal transformation technique for the study of austenite decomposition in steels, a new field of investigation has opened up. Extensive research has been carried out on many different steels, but relatively little work has been done on eutectoid transformations in analogous alloy systems. The researches of Smith and Lindlief,² Mack,³ and Klier and Grymko²0 on the beta-phase transformation in copper-aluminum alloys, of Hibbard, Eichelrnan, and Saunders4 and Smith5 on the kappa-phase transformation in copper-silicon alloys, of Chaudron and Forester6 on the decomposition of "FeO," and of Wasserman7 on similarities between the iron-carbon, copper-aluminum, copper-tin, and copper-beryllium systems essentially comprise the field. The iron-nitrogen system, in view of its remarkable similarity to the iron-carbon system, is particularly attractive for the study of eutectoid decomposition. The present investigation is concerned with the study of isothermal transformation, proceeding by the familiar nucleation and growth processes, and of martensitic transformation characteristics of pure iron-nitrogen alloys. The kinetics of transformation and the morphology of the transformation products have been investigated, for these must be the factors determining the properties and behavior of the final product. The Iron-Nitrogen System he binary iron-nitrogen phase diagram has been a matter of considerable disagreement among vari01.1s investigators. However, the phase diagram according to Eisenhut and Kaupp8 and Lehrer10 is now considered essentially correct as reproduced in fig. 1. The important values, 2.35 pct nitrogen and 591°C, for the co-ordinates of the eutectoid point (obtained from this diagram and used in the re- search to be described) were confirmed in a concurrent study of Paranjpe, Cohen, Bever and Floe." The eutectoid decomposition involves the transformation of the ? face-centered cubic interstitial solid solution of nitrogen in iron to the a body-centered cubic interstitial solid solution of nitrogen in iron and the ?' nitride of iron. This nitride is essentially the compound Fe,N; it also possesses a face-centered cubic lattice but a considerably larger one than the ?; the nitrogen atoms in ?' are arranged in an ordered way in the centers of the unit cubes.8,10,11 A martensitic structure has also been reported8,12 in iron-nitrogen alloys and was studied in the research to be described here. Materials and Methods The specimens used in this investigation were prepared by nitriding "pure" iron. This iron was supplied by the Westinghouse Research Laboratories and is the product bearing their trade name "Puron"; it contains about 0.04 wt pct total impurities, the major portion of which is oxygen. Specimens were ribbons several inches long, a tenth of an inch wide, and 0.125 mm thick; this was the

Jan 1, 1951

By J. W. Hickman, E. A Gulbransen

The physical and chemical structure of the oxide films formed on metals and alloys is of interest in our understanding of their protective properties. According to Pilling and Bedworth,¹ if the specific volume of the oxide is equal to or greater than that of the metal, a compact or continuous structure results; if the volume of the oxide is less, a cellular or porous structure forms. With the cellular type of coating the surface layer of oxide offers no impedance to oxidation; at a given temperature the rate of oxidation is quite constant. On the other hand, the compact type of coating acts as an effective barrier to oxygen and the rate of oxidation will follow a parabolic law. The recent work of Gulbransen2 and of Leontis and Rhines3 on the oxidation of magnesium indicates that it is not necessary for the volume of the oxide to be greater than that of the metal in order that the oxidation may follow a parabolic rate law. One exception to the rule of Pilling and Bedworth¹ is noted by Scheil;4 namely, tungsten. At 500° and 700°C long-time oxidations indicate a linear rate law with time. However, Dunn's6 0xidation measurements from 700°to 1000°C indicate that a parabolic rate law is followed. The oxide is mainly yellow WO a with a thin layer of the blue oxide. Preliminary results on the oxidation of tungsten6 in the temperature range 400° to 500°C indicate that the oxidation does proceed according to a parabolic rate law. Irrespective of the actual rate law that tungsten may obey, it is of interest to compare the results obtained on the oxidation of tungsten in the thin film region with those found when the metal is scaling. A time-temperature study of the oxides formed on both molybdenum and tungsten may indicate whether there exist any peculiarities in the oxide structures of the thin film region compared with those of the scaling region of oxidation. In a recent paper the authors7 presented an investigation of the structures of the oxide films formed on the metals iron, cobalt, nickel, chromium and copper. The results of these studies are presented in graphical form as existence diagrams of the oxides on a time-temperature scale. The existence diagrams of the oxides occurring on some of the metals are simple and show few chemical transitions, but there are many cases in which the physical state of the oxide surface changes as a function of time and temperature, as evidenced by the appearance or disappearance of orientation effects and sharpness of patterns. In general an increase in temperature results in an increase in

Jan 1, 1947

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

The physical and chemical structure of the oxide films formed on metals and alloys is of interest in our understanding of their protective properties. According to Pilling and Bedworth,¹ if the specific volume of the oxide is equal to or greater than that of the metal, a compact or continuous structure results; if the volume of the oxide is less, a cellular or porous structure forms. With the cellular type of coating the surface layer of oxide offers no impedance to oxidation; at a given temperature the rate of oxidation is quite constant. On the other hand, the compact type of coating acts as an effective barrier to oxygen and the rate of oxidation will follow a parabolic law. The recent work of Gulbransen2 and of Leontis and Rhines3 on the oxidation of magnesium indicates that it is not necessary for the volume of the oxide to be greater than that of the metal in order that the oxidation may follow a parabolic rate law. One exception to the rule of Pilling and Bedworth¹ is noted by Scheil;4 namely, tungsten. At 500° and 700°C long-time oxidations indicate a linear rate law with time. However, Dunn's6 0xidation measurements from 700°to 1000°C indicate that a parabolic rate law is followed. The oxide is mainly yellow WO a with a thin layer of the blue oxide. Preliminary results on the oxidation of tungsten6 in the temperature range 400° to 500°C indicate that the oxidation does proceed according to a parabolic rate law. Irrespective of the actual rate law that tungsten may obey, it is of interest to compare the results obtained on the oxidation of tungsten in the thin film region with those found when the metal is scaling. A time-temperature study of the oxides formed on both molybdenum and tungsten may indicate whether there exist any peculiarities in the oxide structures of the thin film region compared with those of the scaling region of oxidation. In a recent paper the authors7 presented an investigation of the structures of the oxide films formed on the metals iron, cobalt, nickel, chromium and copper. The results of these studies are presented in graphical form as existence diagrams of the oxides on a time-temperature scale. The existence diagrams of the oxides occurring on some of the metals are simple and show few chemical transitions, but there are many cases in which the physical state of the oxide surface changes as a function of time and temperature, as evidenced by the appearance or disappearance of orientation effects and sharpness of patterns. In general an increase in temperature results in an increase in

Jan 1, 1947

By A. G. H. Anderson, A. W. Kingsbury

Silicon bronzes containing ken are used to a considerable extent in industry, under the trade name of P.M.G. alloys. Various classes of wrought alloys fall in the composition range 1.5 to 3.5 per cent silicon, and 0.5 to 2.5 per cent iron. Castings may contain as much as 6 per cent silicon and 3 per cent iron at present. The constitutional diagrams of these alloys are thus of considerable practical importance. Copper-silicon-binary alloys have been thoroughly investigated by a number of workers, the latest reports being those of C. S. Smith1 and of A. G. H. Andersen.2 Although much work has been done on iron-copper alloys,3 recorded investigations on the copper-rich copper-iron binary constitutional diagram are not numerous. Tammann and Oelsen4 etermined the solubility limits of iron in copper by means of magnetic measurements, and found that the solubility of iron in copper amounts to a fraction of one per cent at 400°C., increasing slowly to one per cent at 800°C. From 800°C., the solubility increases rapidly and attains 4 per cent at iioo°C. Hanson and Ford,5 using electrical resistivity measurements and the microscope, determined a somewhat different solubility limit. of earlier X-ray works on the copper-iron system, very little has been published. The work by Bradley and Goldschmidt6 on copper-iron-aluminum alloys includes some information on the copper-iron binary. These investigators conclude that substitution of iron in the copper lattice decreases the spacings, which is contrary to the evidence of the present work. Hanson and West? have investigated the ternary alloys of copper with iron and silicon. Although their diagrams are valuable contributions to the understanding of these alloys, they did not recognize the kappa phase,l,2,7,8 and their diagrams do not everywhere conform to the phase rule. The present work contains a check by means of X-rays of the solid solubility limit of iron in copper, and an X-ray investigation of the ternary-phase diagram, which, owing to present conditions, it became necessary to curtail considerably. Preparation of Samples Castings weighing about 75 grams were melted under vacuum. The charges were made up of ingot iron, copper cathodes from Laurel Hill, and refined silicon supplied by the Electrometallurgical Co. Alundum crucibles were generally used. The exceptions were alloys 77 and 78, which were melted in graphite crucibles. The ingots were annealed at 800°C. for one week, then samples were cut for chemical analysis. Longitudinal sections of the binary alloy ingots were hammered into plates 1/8 in. thick. Wherever possible, these plates were homogenized at temperatures ensuring

Jan 1, 1943

By A. G. H. Anderson, A. W. Kingsbury

Silicon bronzes containing ken are used to a considerable extent in industry, under the trade name of P.M.G. alloys. Various classes of wrought alloys fall in the composition range 1.5 to 3.5 per cent silicon, and 0.5 to 2.5 per cent iron. Castings may contain as much as 6 per cent silicon and 3 per cent iron at present. The constitutional diagrams of these alloys are thus of considerable practical importance. Copper-silicon-binary alloys have been thoroughly investigated by a number of workers, the latest reports being those of C. S. Smith1 and of A. G. H. Andersen.2 Although much work has been done on iron-copper alloys,3 recorded investigations on the copper-rich copper-iron binary constitutional diagram are not numerous. Tammann and Oelsen4 etermined the solubility limits of iron in copper by means of magnetic measurements, and found that the solubility of iron in copper amounts to a fraction of one per cent at 400°C., increasing slowly to one per cent at 800°C. From 800°C., the solubility increases rapidly and attains 4 per cent at iioo°C. Hanson and Ford,5 using electrical resistivity measurements and the microscope, determined a somewhat different solubility limit. of earlier X-ray works on the copper-iron system, very little has been published. The work by Bradley and Goldschmidt6 on copper-iron-aluminum alloys includes some information on the copper-iron binary. These investigators conclude that substitution of iron in the copper lattice decreases the spacings, which is contrary to the evidence of the present work. Hanson and West? have investigated the ternary alloys of copper with iron and silicon. Although their diagrams are valuable contributions to the understanding of these alloys, they did not recognize the kappa phase,l,2,7,8 and their diagrams do not everywhere conform to the phase rule. The present work contains a check by means of X-rays of the solid solubility limit of iron in copper, and an X-ray investigation of the ternary-phase diagram, which, owing to present conditions, it became necessary to curtail considerably. Preparation of Samples Castings weighing about 75 grams were melted under vacuum. The charges were made up of ingot iron, copper cathodes from Laurel Hill, and refined silicon supplied by the Electrometallurgical Co. Alundum crucibles were generally used. The exceptions were alloys 77 and 78, which were melted in graphite crucibles. The ingots were annealed at 800°C. for one week, then samples were cut for chemical analysis. Longitudinal sections of the binary alloy ingots were hammered into plates 1/8 in. thick. Wherever possible, these plates were homogenized at temperatures ensuring

Jan 1, 1943

By R. I. Jaffee, J. G. Dunleavy, H. R. Ogden, Webster Hodge

INTRODUCTION EARLY in 1946, at the instigation of the U. S. Army Signal Corps, the authors made an extensive survey of the available literature covering high-strength, high-conductivity alloys. For the purposes of the Signal Corps, the minimum tensile strength to be considered was 150,000 psi, together with at least 50 pct IACS conductivity. No single alloy was found to be in production, or mentioned in the literature, which had this combination of properties. The constitution diagram for the iron-copper alloys is not well established in the respect to the two-liquid region. Fig I, taken from the 1939 Ed. of the ASM Metals Handbook, shows a two-liquid system existing above the liquidus temperature, but disconnected from it. Although Ruer and Fick1 and Ruer and Goerens2 definitely established the fact that two liquid layers could occur in the system, Ruer3 was not convinced that the line off immiscibility was closed in the center. Maddocks and Claussen4 found no liquid immiscibility at temperatures up to 1570°C in alloys containing almost no carbon. Although the diagram would indicate age hardening of the copper-iron alloys is possible, Hanson and Fords found that little hardening effect could be obtained. However, Gordon and Cohen6 reported that the response is better if the quenching is very efficient. Although iron has a potent effect on the conductivity of copper, Hanson and Ford5 have shown that, when hot-rolled copper iron alloys are aged at 1200°F, the electrical conductivity decreases sharply with iron contents up to 0.2 pct Fe, and then levels off at conductivities between 60 to 70 pct IACS with compositions to 2.1 pct Fe. They also found that aging did not increase the tensile strength, although increasing iron content gave a moderate improvement in strength. High-strength copper-iron alloys, usually containing about 60 pct iron, had been reported by Smith and Palmer.7 They found that an alloy containing 56.4 pct copper, 0.21 pct magnesium, balance iron, would give a maximum tensile strength of 170,000 psi and an electrical conductivity of slightly over 35 pct IACS. The alloy could also be processed to have 150,000 psi tensile strength, and about 41 pct IACS conductivity. Decreasing the iron content increased the electrical conductivity, but the long mushy range during freezing of the alloy containing 10 to 20 pct iron made the production of good castings difficult, In spite of the difficulty encountered by Smith and Palmer with alloys of around 20 pct iron, it was decided to make a rather complete investigation 0f this type of alloy. As a result 0f this investigation, a method of alloying and fabricating copper alloys containing 10 to 15 pct iron was developed

Jan 1, 1948

By E. F. Ketterer, D. B. Collyer, A. B. Wilder

AISI constructional alloy steels are a series of steels in which a numbering system signifies the chemical composition limits. SAE (Society of Automotive Engineers) and AISI (American Iron and Steel Institute) use basically the same numbering system. The steels contain, in part, alloy additions of chromium, molybdenum, nickel, and vanadium. They are used widely in the automotive industry but have not been adopted for high temperature service. The purpose of this investigation was to study changes in microstructure observed in typical AISI constructional alloy steels in the welded and un-welded conditions after exposure for 34,000 hr at 900" and 1050" and, in several instances, 1200°F. The tensile and creep rupture properties after exposure for 10,000 hr were also evaluated. The investigation is a continuation of the work previously discussed. Little was known concerning the existence of graphite in medium or low carbon steels before 1943. It is important to note that continued exposure at elevated temperature is required in order to develop graphite in steels. Interest in the presence of graphite in steel, and also in changes in the properties of steels after long service at elevated temperatures, developed after 1943 when a failure of a welded joint of high temperature piping was associated with the graphitization of a relatively low carbon content steel with 0.50 pct Mo,8,0 Numerous investigations have beeen made in recent years studying the relationship of this type of failure to changes in properties. Attempts have been made to evaluate the performance of a number of steels, particularly in the heat-affected zone of welds. It was the unfortunate failure of a weld-heated zone in high temperature piping in the steam-power industry which focused attention upon possible failures, and upon the need for improved steels for high temperature piping service. Investigation by the National Tube Div., U. S. Steel Corp., Lorain Works, has included a wide variety of steels in an attempt to learn the effects of numerous factors and elements upon the long time performance of steels, although many of the compositions studied will never be used at elevated temperatures.1,4-7 Included were the well established AISI steel series, which offered opportunity to test moderately high carbon content steels as well as observe the effect of nickel, chromium, molybdenum, etc., upon the properties of these well known steels. The properties of the AISI steels were also studied for comparison with the previously reported properties of the Cr-Mo steels, now used by the steam-power industry.5,7 Materials and Testing Procedure The AISI alloy steels in Table I were exposed for 10,000 and 34,000 hr at 900°, 1050°, and 1200°F.

Jan 1, 1958

By A. A. Smith, J. S. Smart

THE controlled amounts of phosphorus, arsenic, sulphur or selenium found in commercial coppers perform a variety of highly useful functions. Indeed, a large segment of modem copper technology is essentially dependent upon the presence of one or more of these elements. Consequently, the literature contains many references to their effects but the scope is broad and has been only partly covered. New data are presented herewith directed toward a better understanding of the basic behavior of these elements in copper, with particular emphasis on the composition range 0 to 0.05 per cent. These data are a part of a general program of research on the effects of impurities on the properties of oxygen-bearing and oxygen-free copper, other portions of which have been reported previously.1-2-3 Schematically, the behavior of individual elements is determined from measurements of conductivity and softening temperature,1, 2 and the binary alloys employed are synthesized from high-purity copper in order to eliminate interference from the effects of extraneous impurities. Alloys of selected composition were first prepared in the oxygen-free form by continuously casting the melts in the form of 3/8-in. diameter rod. Oxygen was added subsequently to portions of the alloys, either by remelting or by diffusion at 850°C. from a surface scale. Test wires were drawn one B. and S. number per pass, using four 30-min. 600°C. anneals at o.3125, 0.257, o.204 and o.162 in., and a final cold reduction of 95 per cent t0 0.081 in. Oxygen-bearing slugs made by remelting were hot-rolled to 5/16 in., drawn to 0.162 in., annealed for 30 min. at 600°C. and cold-drawn 95 per cent to 0.081inch. The alloys containing phosphorus, having been compounded very early in the program, were prepared in the form of 5/16-in. rod, and processed to wire with only the last three intermediate anneals listed above, all of these having been conducted in commercial nitrogen. In addition, the conductivity anneals on these alloys were also performed in the same atmosphere, and the small amount of oxygen present as an impurity in the gas resulted in some loss of accuracy at temperatures of 700° to 800°C., as will be shown later. Subsequently, the anneals for all oxygen-free alloys were conducted in hydrogen to prevent oxidation, and purified nitrogen was employed only for oxygen-bearing samples. All conductivity anneals were of one hour duration followed by a rapid quench in 10 per cent H2SO4. EFFECT OF PHOSPHORUS The widespread use of phosphorus as a deoxidant has resulted in universal appreci-

Jan 1, 1945

By K. E. Merklin, F. D. DeVaney

In the past most of the research in pelletizing has as its aim the production of a physically strong pellet. Now that this problem is solved, more attention is being paid to uniformity in grade and chemical composition. Consideration has been given in recent years to a study of additives which will make pellets partially or fully fluxed. Blast furnace tests show fluxed pellets to have advantages over both fluxed sinter and acid pellets. Lower slag volumes are used more frequently in the blast furnace and the uniformity of the charge, both physically and chemically, is becoming increasingly important. A considerable improvement can be secured by having all of the flux uniformly distributed through the pellets in a calcined state. A fluxed pellet, therefore, should be a superior product. The use of an ore burden that contains an appropriate quantity of fluxing materials is not new to the blast furnace industry. For years the Minette ores of France and Germany, the Clinton ores of the Birmingham, Ala., areas, as well as others, which are low in iron but contain calcium carbonate in sufficient quantities to give them self-fluxing properties, have proven economical. The adaption of the sintering process to the preparation of ore burdens provided a means for artifically associating the fluxstone with the iron ore prior to charging to the blast furnace. In 1944 Torpl discussed the effects of using lime in sinter made in Sweden on the sinter's metallurgical performance in a blast furnace. Hessle2 reported in 1945 on the advantages of using lime in sinter to increase the sintering plants' capacity and reduce fuel requirements. Robinson3 discussed the use of lime in Swedish sintering practice at the 1950 Blast Furnace, Coke Oven, and Raw Materials meeting. One of the suggested advantages was the combining of lime with silica to prevent the formation of a fayalite slag, which is difficult to reduce in the blast furnace. Nilson4 at the same meeting commented briefly on experimental work that had just started in the U. S. on the use of lime in sinter. The literature tends to indicate that most of this early work was directed towards improvement in sinter physical quality, and the fact that the feed to the blast furnace was partially fluxed was incidental. It was not long, however, before blast furnace advantages were being claimed. The matter was forcibly called to the attention of North American operators by reports of remarkable production records established by the Russians using fluxed sinter. The leading step was taken on this continent by the Steel Company of Canada in 1957; McMahon5 reported on the marked improvement in performance of an 18-ft blast furnace using fluxed sinter at its Hamilton works. Other North American operators quickly followed theStelco lead.

Jan 1, 1963

By Simon D. Strauss

COPPER In terms of mining activity, copper is the leading nonferrous metal. It is true that in recent years the volume of aluminum consumption in the non-Communist world has exceeded the volume of copper consumption, but virtually the entire primary aluminum supply is derived from bauxite. On the average, only four tons of bauxite need be mined to produce a ton of aluminum. By contrast, the highest-grade, large-scale copper mines now in operation (those in the Congo) must mine at least 20 tons of ore to produce a ton of copper. In the United States an average of 150 tons of ore must be mined to produce a ton of copper. This does not take into account the huge amounts of waste overburden that must be stripped from the open-pit mines to account for their steadily rising share of the world's copper output. Copper epitomizes the economic problems of the mining industry in many ways. Its price is highly volatile, considering its great economic importance. It has been a tool of mankind longer than any other of the base metals-the dawn of history has been classified as "The Bronze Age." World Copper Production Although copper is mined in many countries, in recent years 70% of the non-Communist world production has come from six countries. Two of these are industrialized countries and are large consumers-United States and Canada. The other four are developing countries with very small domestic requirements-Chile, Zambia, Zaire, and Peru. Heavily dependent on copper exports to sustain their domestic economies, these countries find themselves oscillating between prosperity and depression with the changing levels of copper prices. In an effort to control their own destiny, in 1968 they formed an organization of copper exporting countries (CIPEC) which was designed to study copper markets and possibly to intervene actively in these markets. (When this chapter was being prepared, no actual steps along such lines had been taken.) Many of the leading industrialized nations are wholly dependent on imports for their primary copper supplies. These include West Germany, the United Kingdom, France, Italy, and many others. Japan, now the non-Communist world's second largest copper consumer, produces only 10 to 15% of its requirements from domestic mines. Although the bulk of the copper output is smelted in the country where it is mined, there is a limited international trade in copper concentrates. Canada, the Philippines, Australia, and Papua-New Guinea are significant exporters of copper concentrates; Japan, Germany, the United States, and Sweden are importers. However, this trade accounted for only about 10% of the non-Communist world production of copper during the decade of the 1960s.

Jan 1, 1976

By H Pray, H. W. Russell, Paul D. MILLER

It is known that austenitic chromium-nickel steels that have free carbide in the grain boundaries are subject to intergranu-lar corrosion. It is difficult to detect such a susceptible condition in a fabricated article because present test methods require a sample section for examination and in most cases this is difficult to obtain. The question of the nature and prevention of intergranular corrosion in austenitic stainless steels has been ably discussed by Bain and co-workers1-3 and by other investigator4-10 The present methods of study subject samples to corrosive conditions in such reagents as the Strauss solution, a mixture of copper sulphate and sulphuric acid. Such tests usually require at least 72 hr. to run. Various methods of measuring the degree of sensitization have been employed, such as the measurement of electrical resistivity, magnetic measuremerits, measurement of the degree of cracking produced on bending over a malldrel, and microscopic studies. The detection of carbides at the grain boundaries by metallographic polishing and etching methods is tedious and requires a skilled operator. A recent report on such methods of carbide detection is given by the American Society for Testing Materials Subcommittee VI of Committee A.-1011 and by Arness.12 The present investigation was undertaken to develop a simple test procedure for detecting carbide precipitation or susceptibility to intergranular corrosion. The test is designed for use in the plant and for the testing of fabricated structures. Carbide precipitation, the factor leading to susceptibility to corrosion, is produced by heating the alloy in the temperature range 800° to 1600°F., as in welding, in improper annealing or in service where such temperatures are met. The connection between such precipitation and susceptibility to corrosion has been thoroughly discussed, as has been the use of stabilizing addition elements to prevent precipitation. Experimental Method A small area of the steel under test is subjected to an anodic treatment in a cell that can be 'lamped Onto a a Or an actual structure. The cell and electrical circuit used are illustrated in Fig. I. The cell C is lead, joined to the steel plate D and insulated from it by a short piece of rubber tubing E. The cell is forced tightly against the steel plate by a spring Or clamping device. The seal formed by the rubber against the steel plate is sufficient to retain the liquid bath inside the cell. The spot treated can be made any shape desired, depending on the shape of the rubber gasket. The cell illustrated polishes a circular spot about 3/8- diameter' The bath consists of 60 per cent (by weight) sulphuric acid to which is added 5 ml. per liter of Glycyrrhiza extract (U.S.P.). The cell requires about 2 to 2.5

Jan 1, 1941

By H. W. Russell, H Pray, Paul D. MILLER

It is known that austenitic chromium-nickel steels that have free carbide in the grain boundaries are subject to intergranu-lar corrosion. It is difficult to detect such a susceptible condition in a fabricated article because present test methods require a sample section for examination and in most cases this is difficult to obtain. The question of the nature and prevention of intergranular corrosion in austenitic stainless steels has been ably discussed by Bain and co-workers1-3 and by other investigator4-10 The present methods of study subject samples to corrosive conditions in such reagents as the Strauss solution, a mixture of copper sulphate and sulphuric acid. Such tests usually require at least 72 hr. to run. Various methods of measuring the degree of sensitization have been employed, such as the measurement of electrical resistivity, magnetic measuremerits, measurement of the degree of cracking produced on bending over a malldrel, and microscopic studies. The detection of carbides at the grain boundaries by metallographic polishing and etching methods is tedious and requires a skilled operator. A recent report on such methods of carbide detection is given by the American Society for Testing Materials Subcommittee VI of Committee A.-1011 and by Arness.12 The present investigation was undertaken to develop a simple test procedure for detecting carbide precipitation or susceptibility to intergranular corrosion. The test is designed for use in the plant and for the testing of fabricated structures. Carbide precipitation, the factor leading to susceptibility to corrosion, is produced by heating the alloy in the temperature range 800° to 1600°F., as in welding, in improper annealing or in service where such temperatures are met. The connection between such precipitation and susceptibility to corrosion has been thoroughly discussed, as has been the use of stabilizing addition elements to prevent precipitation. Experimental Method A small area of the steel under test is subjected to an anodic treatment in a cell that can be 'lamped Onto a a Or an actual structure. The cell and electrical circuit used are illustrated in Fig. I. The cell C is lead, joined to the steel plate D and insulated from it by a short piece of rubber tubing E. The cell is forced tightly against the steel plate by a spring Or clamping device. The seal formed by the rubber against the steel plate is sufficient to retain the liquid bath inside the cell. The spot treated can be made any shape desired, depending on the shape of the rubber gasket. The cell illustrated polishes a circular spot about 3/8- diameter' The bath consists of 60 per cent (by weight) sulphuric acid to which is added 5 ml. per liter of Glycyrrhiza extract (U.S.P.). The cell requires about 2 to 2.5

Jan 1, 1941

By W. R. Hibbard

Although extensive pole figure studies have been reported by Brick1 and others2,3 showing preferred orientations in rolled and annealed 70-30 alpha brass, and by Hermann and Sachs4 in 70-30 alpha brass cups, comparatively little information has been published on textures in drawn 70-30 alpha brass tubes. Crampton5 reported a (110) , [111] texture in drawn brass tubes based on selected individual X ray photograms following the method of Norton and Hiller,6 but the extent and ease of developing this texture and the annealing texture have not been reported and pole figures of these structures were not found in the literature. The present investigation was further stimulated by the possible influence of textures on the mercury stress-corrosion cracking of brass tubes. According to Snoek,7 iron-nickel alloy sheet with a strong cubic texture was more resistant to corrosion than a randomly oriented sheet. Crampton5 reported that single crystals of 70-30 alpha brass drawn into tubes did not crack after 24 hr in a standard mer-curous nitrate test. Edmunds12 found that single crystals of 70-30 alpha brass did not crack in a standard mercurous nitrate test but did crack when subjected to ammoniacal vapor. Wasserman11 reported a similar failure of a single crystal of brass in ammonia. A tube with a strong texture might approach single crystal behavior and tend to resist mercury cracking if the differences in orientation between adjacent grains were sufficiently slight. Preparation OF Specimens Crampton's5 tubes drawn 28 pct reduction in area developed a slight degree of preferred orientation while in tubes drawn 48 pct it was more marked. Based on this information, in order to obtain specimens with markedly different degrees of preferred orientation but with the same final draw, two sets of 70-30 alpha brass tubes were made following the mill schedules shown in Table I. The final draw involved a large reduction in outside diameter, and a ratio of reduction in area to reduction in outside diameter similar to that reported by Crampton,5, 10 to cause mercury cracking of brass tubes. The brass contained 71.31 pct copper, 0.01 pct lead, 0.01 pct iron and zinc by difference. Determination of Pole Figures A 6-in. length from each tube was rotated rapidly by an electric stirrer in 25 pct nitric acid until the gauge was reduced to 0.003-0.005 in. The tubes were carefully cut longitudinally and the walls gently flattened. They were further etched in 25 pet nitric acid to 0.0015 in. thickness and (111) pole figures were determined using copper K-alpha radiation in the manner described by Brick.' The three general types of pole figures

Jan 1, 1949