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By A. H. Geisler, F. Keller

Although the subject of precipitation from solid solution appears to be one of the more profitable fields in metallurgy for study with the electron Microscope, few comprehensive studies have yet been made. Occasionally electron micrographs have been published that illustrated alleged precipitation in various alloys, but frequently the apparent size, shape and distribution of the particles do not fully agree with those expected from theory or from observations of the Precipitate when the particles have grown to a size resolvable with the light microscope. The presence of a Widmanstatten pattern for submicroscopic precipitate particles has been demonstrated for only a few aged a1loys.l The initial problem has been the development of suitable techniques for applying the transmission-type instrument to a field that has been inherently associated with reflection-type microscopes. The various techniques have been the subjects of numerous publications, and instead of describing them individually here it will sufficc to say that the oxide film method has proved to be the most satisfactory method yet found for studying the microstructure of aluminum alloys with the electron microscope. This method has the definite characteristic advantage that the actual surface layer of the specimen is examined and not a plastic or silica replica. Doubtless suitable methods for forming and removing the oxide film could be developed for alloys of other metals. The purpose of this report is to point out the characteristics of the oxide film method that have been observed during the studies of numerous aged aluminum alloys and to present the results of these studies. Preparation OF Specimens The oxide film method for preparing specimens of aluminum alloys for examination in the electron microscope has been described in detail previously,¹,² Briefly, the procedure consists of preparing the metallographic specimen, forming the film by anodic oxidation and removing the film from the prepared surface of the oxidized specimen, The specimen is polished accordillg to the usual procedure for microscopic examination.³ he specimen may then be etched to remove flowed metal but etching to attack the alloy constituents or to leave them in relief as in the replica processes is not necessary. Electrolytic polishing is not generally recommended, Deep-etched specimens are used frequently, however, since they provide information that is not revealed by polished specimens and frequently present the same information more clearly than do the polished specimens, The surface preparation of specimens to be deep-etched is not important, since specimens that have been subjected to the first wet PoliShing operation are generally used, but frequently the as-rolled surface is Suitable. These specimens are then etched using a suitable macroetching reagent.

Jan 1, 1947

By F. Keller, A. H. Geisler

Although the subject of precipitation from solid solution appears to be one of the more profitable fields in metallurgy for study with the electron Microscope, few comprehensive studies have yet been made. Occasionally electron micrographs have been published that illustrated alleged precipitation in various alloys, but frequently the apparent size, shape and distribution of the particles do not fully agree with those expected from theory or from observations of the Precipitate when the particles have grown to a size resolvable with the light microscope. The presence of a Widmanstatten pattern for submicroscopic precipitate particles has been demonstrated for only a few aged a1loys.l The initial problem has been the development of suitable techniques for applying the transmission-type instrument to a field that has been inherently associated with reflection-type microscopes. The various techniques have been the subjects of numerous publications, and instead of describing them individually here it will sufficc to say that the oxide film method has proved to be the most satisfactory method yet found for studying the microstructure of aluminum alloys with the electron microscope. This method has the definite characteristic advantage that the actual surface layer of the specimen is examined and not a plastic or silica replica. Doubtless suitable methods for forming and removing the oxide film could be developed for alloys of other metals. The purpose of this report is to point out the characteristics of the oxide film method that have been observed during the studies of numerous aged aluminum alloys and to present the results of these studies. Preparation OF Specimens The oxide film method for preparing specimens of aluminum alloys for examination in the electron microscope has been described in detail previously,¹,² Briefly, the procedure consists of preparing the metallographic specimen, forming the film by anodic oxidation and removing the film from the prepared surface of the oxidized specimen, The specimen is polished accordillg to the usual procedure for microscopic examination.³ he specimen may then be etched to remove flowed metal but etching to attack the alloy constituents or to leave them in relief as in the replica processes is not necessary. Electrolytic polishing is not generally recommended, Deep-etched specimens are used frequently, however, since they provide information that is not revealed by polished specimens and frequently present the same information more clearly than do the polished specimens, The surface preparation of specimens to be deep-etched is not important, since specimens that have been subjected to the first wet PoliShing operation are generally used, but frequently the as-rolled surface is Suitable. These specimens are then etched using a suitable macroetching reagent.

Jan 1, 1947

By Fred C. Bond

COMPRESSION TESTS THE standard method of determining the crushing resistance of rocks consists of crushing prepared shapes under slow compression, and expressing the ultimate crushing resistance at the load causing failure in pounds per square inch of crossectional area perpendicular to the crushing force, with the height approximately equal to the diameter. One-inch cubes or cylindrical drill cores are commonly used. Cubes and drill cores are cut by a high-speed steel disk with diamond dust embedded in the edges, and running under a water spray. Such a saw will cut one square inch or more of hard stone per minute. An oiled, spherical, swivel compression block of small diameter should be used to equalize the pressure. Each sample is crushed between sheets of cardboard or blotting paper extending about one-half inch beyond the edges of the stone. A cloth is wrapped around it to prevent dangerous explosive shattering. It is probably preferable to place the swivel block below the specimen, with either a rigid head or another swivel block above. Whatever the arrangement, the conditions should be selected that will develop the maximum crushing strength of the specimen, even though its top and bottom planes may not be precisely parallel. The cardboard pads may be dispensed with if the ends of the specimens are polished smooth. The use of lead pads was discontinued because of the observed tendency to split the material. The samples are weighed and measured before breaking, and the density is calculated. Cubes that contain bedding planes or veinlets are usually placed with these vertical and parallel to the crushing force, in order to develop the maximum resistance possible. A number of compression tests were made on Canadian ores, by Forrest Nagler, of the Allis-Chalmers Manufacturing Co., and are listed alphabetically in Table 1. These tests were made on one inch cubes or on diamond-drill cores approximately one inch in diameter and one inch long. The drill cores represent virgin rock, while the cubes may have been previously weakened by explosives. Compression tests have been made in the Allis-Chalmers Milwaukee Laboratory on a number of ores and other materials. These are listed alphabetically in Table 2. In test No. 1339, on limestone from the Hanna Coal Co., comparison was made between 2 by 2-in. diamond-drill core segments and one-inch cubes cut from the cores in the same strata. Results for the cylinders are tabulated directly below those for the cubes. The bedding planes were normal to the compressive force in breaking the cylinders and parallel in breaking the cubes, which accounts for the lower strength obtained from the cylinders. The percentage of net linear compression at the ultimate pressure was measured in test No. 1055 for Fontana TVA quartzite as 0.30 for cube A, and 0.37 for cube D.

Jan 1, 1946

By T. E. Tietz, J. E. Dorn

Activation energies for creep of copper at intermediate temperatures, where crystal recovery was negligible, were determined by the simple technique of rapidly alternating the test temperature between and T2 (T2 = TI + about 10°K) throughout a constant stress creep test. The activation energy for creep H was found to be 37,000± 3,000 cal per mol, independent of stress and strain. The same creep laws as have been previously established for high temperature creep were found to be valid for creep at intermediate temperatures. But the AH was found to be lower than that for self-diffusion in the intermediate temperature range whereas it is known to be equal to that for self-diffusion at high temperatures. IT is now well established that creep at high temperatures can be correlated by the functional relationship'-" e = f(?) s = constant [I] where E is the total plastic strain, f is the function that depends on the stress, ? = f e -- dt, t is the duration of test, e is the base of natural logarithms, AH is the activation energy for creep, R is the gas constant,T is the absolute temperature, and s is the stress. Thus, identical values of are achieved during creep under a given stress at two alternate temperatures at the same total strain. At the same strain therefore where subscripts refer to the two alternate temperature conditions of test. Consequently, the activation energy for high temperature creep is readily obtained with the aid of Eq. 2. Activation energies so obtained have been observed to be insensitive to the creep strain at which they are evaluated, the applied stress, grain size, minor alloying additions,'-' cold worked state, and the presence of thermally stable dispersions of intermetallic compounds in an a solid solution matrix Furthermore, the activation energy for high temperature creep is very nearly equal to that for self-diffusion in all cases where adequate data are available for comparison." " The apparent identity of the activation energies for high temperature creep and self-diffusion strongly suggest that high temperature creep arises from a dislocation climb process. This hypothesis is further strengthened by the fact that the energy of activation for high temperature creep is insensitive to the applied stress," and by the observations that the correlation suggested by Eq. 1 cannot be ex- tended to temperatures below those for rapid crystal recovery. When using the activation energy for self-diffusion, Eq. 1 fails to give the required correlations between creep curves at various intermediate temperatures.' This suggests that the dislocation climb mechanism for creep might be superseded by some alternate mechanism in the intermediate range of temperatures. This investigation was initiated in a preliminary attempt to ascertain the type of creep law that might be valid in the intermediate range of temperatures. Special consideration, however, was given to the determination of the activation energy for creep in this range because the Becker-Orowan', " and the Mott-Nabarro10 theories for transient creep suggest that the activation energy should increase

Jan 1, 1957

By J. A. Bartnik, Gerald D. Rose, William H. Benson

New techniques in the magnetite and heavy media beneficiation industries demand more efficient magnetic dispersion and flocculation of the finely ground particles. Demagnetizing coils must produce several major effects, such as improving classification and screening efficiency, decreasing moisture content in filter cake and improving separation selectivity and green pellet properties. Likewise, magnetic flocculators must increase filtering rates and the settling rates of solids, improve magnetite recovery and produce cleaner water. To improve the design of equipment and to conduct tests leading to the optimization of such dispersion and flocculation, a program was initiated at Eriez Magnetics. The major conclusions reached are: 1. Laboratory and plant scale tests conducted on magnetite products show that a demagnetizing force of 450 rms oersteds at 60 cycles for 1/20- second duration will depolarize natural magnetite particles coarser than approximately 10 microns. This has been found satisfactory for most applications. 2. Effective flocculation of magnetite was obtained when a slurry with more than one percent magnetite was exposed for a period of approximately 1/15 second to a 600-gauss field. 3. The cost of demagnetizers (or flocculators) increases rapidly for larger diameter pipes. In order to reduce the cost, narrow rectangular sections are recommended for magnetic flocculators. 4. For minimum operating cost, permanent magnetic flocculators are ideal, chiefly because they do not require any maintenance and have no operating cost. 5. A newly designed electro-demagnetizing coil with high heat dissipation and a nonmetallic core provides high efficiency and long life. 6. To select the correct magnetic flocculator (or demagnetizing coil) the following information is necessary: a. Magnetic product susceptibility b. Magnetic product coercive force c. Percent of magnetic product d. Flow rate e. Viscosity f. Structure of magnetic product

Jan 8, 1968

By Shiou-Chuan Sun

THIS paper presents the design and operation of a frothmeter capable of measuring the frothing characteristics of pine oils and other frothing reagents. The experimental data show that the froth-ability of pine oil is governed by: 1—rate of aeration, 2—time of aeration, 3—height of liquid column, 4—chemical composition of pine oil, 5—pH value of solution, 6—temperature of solution, and 7—concentration of pine oil in solution. The effect of mineral particles on the behavior of froth also was studied, and the results can be found in a separate paper.' The results also show that the relative froth-abilities of pine oils in the frothmeter generally correlate with those in actual flotation, provided that other factors are kept constant. In addition to pine oils, the other well-established flotation frothers were tested, and the results are included. In this paper, compressed air frothing is the frothing process performed by means of purified compressed air, whereas sucked air frothing is the frothing process accomplished by purified air sucked into the glass cylinder by a vacuum system. The term vacuum frothing denotes that froth was formed by degassing of the air-saturated liquid under a closed vacuum system. Apparatus The frothmeter, shown in Fig. 1, is capable of re-producibly measuring the volume and persistence of froth as well as the volume of air bubbles entrapped in the liquid and is capable of being used for compressed air frothing, sucked air frothing, and vacuum frothing. Fig. la shows that for compressed air frothing, the apparatus consists of an airflow regulating system, 1-3; a purifying and drying system, 4-8; a standardized flowmeter to measure the rate of airflow from zero to 500 cc per sec, 9; and a graduated glass cylinder, 13; equipped with an air regulating stopcock, 10; an air chamber, 11; and a fritted glass disk to produce froth, 12. The fritted glass disk, 5 cm in diam and 0.3 cm thick, has an average pore diameter of 85 to 145 microns. The pyrex glass cylinder has a uniform ID of 5.588 cm and an effective height of 63 cm. The inside cross-sectional area of the glass cylinder was calculated to be 24.53 sq cm, or 3.8 sq in. For sucked air frothing, Fig. lb shows that the apparatus for compressed air frothing is used again, with the following modifications: 1—compressed air and its regulating system, 1-3, are eliminated; and 2—a vacuum system, 16, equipped with a vapor trap, 15, and a vacuum manometer, 17, is added. The vacuum system can be either a water aspirator or a laboratory vacuum pump. Any desired rate of airflow can be drawn into the glass cylinder, 13, by adjusting the opening of the air regulating stopcock, 10. The sucked air stream is cleaned by the purifying and drying system, 4-8, before entering the glass cylinder, 13. When this setup is used for vacuum frothing, the air regulating stopcock is closed. The frothmeter has been used for almost 3 years and has proved to give reproducible results, as illustrated in Table I. With a magnifying glass and suitable illumination, the frothmeter also can be used to study the attachment of air bubbles to coarse mineral particles.' Experimental Procedures Except where otherwise stated, the data presented were established by means of the compressed air method. The volume and persistence of froth were recorded respectively at the end of 4 and 6 min of aeration at a constant rate of airflow of 29.3 cc per sec, which is equivalent to 71.6 cc per sq cm per min, or 462.6 cc per sq in. per min. The aqueous solution for each test, containing 1000 cc of distilled water and 19.2 ± 0.5 mg frothing reagent, was adjusted to a pH of 6.9 0.2. The volume of froth is expressed as cubic centimeter per square centimeter and is equivalent to the height of the froth column (the distance between the bottom and the meniscus of the froth). The volume of froth was obtained by multiplying the height of froth by the cross-sectional area of the glass cylinder, 24.53 sq cm. Before each test, the glass cylinder, 13, was cleaned thoroughly with jets of tap water, ethyl alcohol, tap water, cleaning solution, tap water, and finally distilled water. The cylinder with stopcock,

Jan 1, 1953

By Shiou-Chuan Sun

THIS paper presents the design and operation of a frothmeter capable of measuring the frothing characteristics of pine oils and other frothing reagents. The experimental data show that the froth-ability of pine oil is governed by: 1—rate of aeration, 2—time of aeration, 3—height of liquid column, 4—chemical composition of pine oil, 5—pH value of solution, 6—temperature of solution, and 7—concentration of pine oil in solution. The effect of mineral particles on the behavior of froth also was studied, and the results can be found in a separate paper.' The results also show that the relative froth-abilities of pine oils in the frothmeter generally correlate with those in actual flotation, provided that other factors are kept constant. In addition to pine oils, the other well-established flotation frothers were tested, and the results are included. In this paper, compressed air frothing is the frothing process performed by means of purified compressed air, whereas sucked air frothing is the frothing process accomplished by purified air sucked into the glass cylinder by a vacuum system. The term vacuum frothing denotes that froth was formed by degassing of the air-saturated liquid under a closed vacuum system. Apparatus The frothmeter, shown in Fig. 1, is capable of re-producibly measuring the volume and persistence of froth as well as the volume of air bubbles entrapped in the liquid and is capable of being used for compressed air frothing, sucked air frothing, and vacuum frothing. Fig. la shows that for compressed air frothing, the apparatus consists of an airflow regulating system, 1-3; a purifying and drying system, 4-8; a standardized flowmeter to measure the rate of airflow from zero to 500 cc per sec, 9; and a graduated glass cylinder, 13; equipped with an air regulating stopcock, 10; an air chamber, 11; and a fritted glass disk to produce froth, 12. The fritted glass disk, 5 cm in diam and 0.3 cm thick, has an average pore diameter of 85 to 145 microns. The pyrex glass cylinder has a uniform ID of 5.588 cm and an effective height of 63 cm. The inside cross-sectional area of the glass cylinder was calculated to be 24.53 sq cm, or 3.8 sq in. For sucked air frothing, Fig. lb shows that the apparatus for compressed air frothing is used again, with the following modifications: 1—compressed air and its regulating system, 1-3, are eliminated; and 2—a vacuum system, 16, equipped with a vapor trap, 15, and a vacuum manometer, 17, is added. The vacuum system can be either a water aspirator or a laboratory vacuum pump. Any desired rate of airflow can be drawn into the glass cylinder, 13, by adjusting the opening of the air regulating stopcock, 10. The sucked air stream is cleaned by the purifying and drying system, 4-8, before entering the glass cylinder, 13. When this setup is used for vacuum frothing, the air regulating stopcock is closed. The frothmeter has been used for almost 3 years and has proved to give reproducible results, as illustrated in Table I. With a magnifying glass and suitable illumination, the frothmeter also can be used to study the attachment of air bubbles to coarse mineral particles.' Experimental Procedures Except where otherwise stated, the data presented were established by means of the compressed air method. The volume and persistence of froth were recorded respectively at the end of 4 and 6 min of aeration at a constant rate of airflow of 29.3 cc per sec, which is equivalent to 71.6 cc per sq cm per min, or 462.6 cc per sq in. per min. The aqueous solution for each test, containing 1000 cc of distilled water and 19.2 ± 0.5 mg frothing reagent, was adjusted to a pH of 6.9 0.2. The volume of froth is expressed as cubic centimeter per square centimeter and is equivalent to the height of the froth column (the distance between the bottom and the meniscus of the froth). The volume of froth was obtained by multiplying the height of froth by the cross-sectional area of the glass cylinder, 24.53 sq cm. Before each test, the glass cylinder, 13, was cleaned thoroughly with jets of tap water, ethyl alcohol, tap water, cleaning solution, tap water, and finally distilled water. The cylinder with stopcock,

Jan 1, 1953

By H. M. O?Harra

Experiments have shown that the use of enriched air would be of particular benefit in the roasting of zinc ores for the manufacture of sulfuric acid. Enriched air increases capacity of furnace, decreases fuel consumption, and increases SO2 content of roaster gas. THE work here described had for its purpose the procuring of data from which some quantitative estimate might be made of the results obtainable by using oxygen-enriched air in roasting zinc ores on a commercial scale. The principal metallurgical advantages of using enriched air in roasting zinc ores would be: 1. The rate of roasting would be increased, with consequent gain in the capacity of the roasting furnace. 2. As less air would be required for roasting, the volume of hot gases leaving the furnace and the heat carried out of the furnace as sensible heat in these gases would be less per ton of ore roasted; partly for this reason and partly because of the increased quantity of heat generated in the furnace by the larger amount of ore that could be roasted, the consumption of fuel by the furnace would be lessened; and by the use of air sufficiently enriched with oxygen the necessity of using fuel might be entirely obviated. 3. Roaster gas having a higher SO2 content could be produced; this would make possible greater capacity and more economical operation of the sulfuric-acid plant. Certain phases of the application of enriched air to roasting can be worked out only by experimenting with a furnace of commercial, or at least semicommercial, size. Thus the precautions necessary to secure proper distribution of heat in the furnace;1 the volume of enriched air,

Jan 3, 1924

* The greatest and richest iron ore body in the world was discovered by U. S. Steel in Venezuela in April 1947, and is disclosed for the first time in this issue (p. 178), One solid mountain of ore, Cerro Bolivar, will furnish more tonnage than the famous Hull Rust pit at Superior has, or can produce. Total resources are on the order of 2 billion tons plus. Big Steel is now moving with great speed on construction to bring out this ore, and 10 million tons are scheduled for shipment into Baltimore and Birmingham by late 1952. This ore will arrive at, Pittsburgh at a price lower than present natural ores from Superior. The Venezuelan properties will be completely mechanized. •U. S. Steel and independent companies are embarking on a taconite beneficiation program of tremendous proportions, which must be speeded to completion in the 1950's (see p. 185). By 1960 over $l.2 billion dollars will be spent on Venezuela, taconite, and Labrador to solve the United States iron ore crisis. In addition, U. S. Steel will spend another $300 million plus for a new steel mill at Trenton, N. J., before 1955. •The Deister Concentrator Co. gave $500 to the 1950 Coal Division Scholarship Fund. •Howard N. Eavenson, in analyzing the bituminous coal situation (see p. 193), suggests that anti-trust laws be extended to labor unions, disinterested trustees to administer pension funds, begin pension funds now and stop the collection of all "check-offs" for union dues or funds. •Minerals and metals worth 13.9 million dollars were produced in the United States in 1949, Secretary of the Interior Oscar L. Chapman announced. Although this value was 11 pct less than in 1948, it was the second greatest in history. Nonmetallics was the only major group that in 1949 equaled the 1948 production high. Mineral fuels decreased 12 pct and metals 15 pct. • Prospects for making gas from coal are seen to be unattractive by the Pittsburgh Consolidated Coal Co. because the success of operation depends on price and supply of coal which presently are not attractive. The company has shut down its gasification plant at Library, Pa. * Economic prospects for the immediate future in the United States are good and business probably will continue at its present high levels throughout at least the early part of 1950, Secretary of Commerce Charles Sawyer said in his year-end report to the White House based on his personal survey of business conditions. •A 467-ft well 34 miles north of Rock Springs, Southwestern Wyoming, is said to be flowing a 5 pct solution of nearly pure trona (sodium carbonate) at the rate of 10,000 barrels a day. Trona, natural soda ash, is mined for the chemical trade at Searles Lake, Calif., and from about 1500 ft underground near Green River, Wyo., and has been in short supply. •The AEC is "very much interested" in a discovery of radioactive material that has been made in Baraga County bordering Lake Superior in the Upper Peninsula of Michigan, reported F. G. Pardee, Michigan State mining engineer. The material has been identified as uranium oxide in the form of pitchblende or uraninite. The discovery, made by a geologist of the Jones & Laughlin Ore Co., is the only instance in which the commission has certified samples of Michigan rock.

Jan 2, 1950

By W. F. Holbrook, C. E. Wood, E. P. Barrett

The high-frequency laboratory induction furnace with a rotating liquid crucible enables research workers to conduct certain investigations heretofore very difficult or impossible to realize because vessels are not obtainable that are capable of resisting the physical conditions or the chemical actions to which they are subjected. Applications for patents covering commercial uses of centrifugal liquid crucibles were filed in the United States in 1919,' in France in 1925, in the United States and Germany in 1926,2 and in France in 1927.3 In 1928, Schuette and Maier,4 of the Bureau of Mines, reported the construction of a whirling table beneath a high-frequency induction furnace. Shape and Size of Centrifugal Liquid Crucibles When a vessel containing a liquid is rotated, the inner surface of the liquid takes the shape of a paraboloid under the simultaneous action of centrifugal force and gravity. The internal dimensions of the paraboloid rotating liquid crucible are governed by the diameter of the container and its speed of rotation. Melted Wood's metal was poured into cylinders 2 1/2 in. in diameter, which were rotated at 180, 300, and 468 r.p.m. When the metal was solid, a slurry of plaster of Paris was added, and rotation continued until the plaster had set. Fig. 1, a photograph of sections of the cylinders, shows the effect of speed of rotation of the containers upon the shape of the inner surface of the rotating liquid crucibles. Types of Furnaces Three types of high-frequency induction laboratory furnaces using liquid-metal crucibles were designed and constructed by the Blast

Jan 1, 1939

By W. F. Holbrook, C. E. Wood, E. P. Barrett

The high-frequency laboratory induction furnace with a rotating liquid crucible enables research workers to conduct certain investigations heretofore very difficult or impossible to realize because vessels are not obtainable that are capable of resisting the physical conditions or the chemical actions to which they are subjected. Applications for patents covering commercial uses of centrifugal liquid crucibles were filed in the United States in 1919,' in France in 1925, in the United States and Germany in 1926,2 and in France in 1927.3 In 1928, Schuette and Maier,4 of the Bureau of Mines, reported the construction of a whirling table beneath a high-frequency induction furnace. Shape and Size of Centrifugal Liquid Crucibles When a vessel containing a liquid is rotated, the inner surface of the liquid takes the shape of a paraboloid under the simultaneous action of centrifugal force and gravity. The internal dimensions of the paraboloid rotating liquid crucible are governed by the diameter of the container and its speed of rotation. Melted Wood's metal was poured into cylinders 2 1/2 in. in diameter, which were rotated at 180, 300, and 468 r.p.m. When the metal was solid, a slurry of plaster of Paris was added, and rotation continued until the plaster had set. Fig. 1, a photograph of sections of the cylinders, shows the effect of speed of rotation of the containers upon the shape of the inner surface of the rotating liquid crucibles. Types of Furnaces Three types of high-frequency induction laboratory furnaces using liquid-metal crucibles were designed and constructed by the Blast

Jan 1, 1939

The Sub-committee on Coal Mining, since its appointment, has been collecting data about subsidences in coal mines in this country, and thinks that almost all of the available data about occurrences of this sort in bituminous mines has been collected. Similar data is being compiled for the anthracite regions, which it is hoped will be ready for the 1927 meeting. As most of the bituminous seams are nearly level, the records obtained give the problem in its simplest form, without complications due to the pitch of the seam. Copies of the questionnaire, Appendix A, were mailed to all of the coal operators' associations, to most of the large operating companies and to many engineers, with the request that any data on the subject be returned to the committee, or that advice of any subsidences known be given: the replies to most of the questionnaires were general, although some specific cases were given. Many of the companies were unable to reply to all questions, as they lacked the necessary data, but in nearly every case where accuratc data was available, it was cheerfully furnished, and any additional information requested was secured. All specific cases of subsidence were followed up by correspondence, and in several cases by personal inspection. Figs. 1 to 31 were made from the information furnished. Table 1 gives measurements of elevations taken in one case at intervals from October, 1913, to May, 1918. With one exception, where the evidence cannot be released on account of a lawsuit, it is believed that the cases submitted with this report include practically all that have happened in bituminous coal mining in this country of which actual measurements were secured. Some of these have been published by Young and Stoek,l and some have been secured from other publications. In collecting these data, the subcommittee had the Engineering Societies Library extend its bibliography to date; this list is given in Appendix B. To assist in the study of the problem, all of the subsidence literature in English was examined for cases in which spccific measurements were given, and the essential data for each case are shown in Appendix C.

Jan 1, 1927

By A. G. Guy

IN the course of a research on steady-state diffusion it became necessary to make diffusion calculations for a finite solid. This problem was found to be sufficiently different from the corresponding problem for the semi-infinite solid for an entirely new approach to be necessary in obtaining a useful solution. The assumption of an exponential variation of the diffusion coefficient with concentration' was no longer a practical necessity, so that the new solution offered the possibility of handling diffusion in semi-infinite solids for arbitrary variations of the diffusion coefficient with concentration. In discussing the principle on which this method of calculation is based, it is convenient to consider the relatively simple problem of one dimensional diffusion into a matrix that initially contains none of the diffusing substance. The solution of the set- ond Fick Law,?C/?t=D0?2C/?x2, for diffusion into a semi-infinite solid is3 C/C=1-F(x/2vD0t [1] where C is the concentration of the diffusing substance at a depth x cm below the surface after dif- A. G. GUY, Member AIME, and M. GOLOMB are Professor of Metollurgicol Engineering and Professor of Mathematics, respectively, Purdue University, Lafayette, Ind., A. S. YUE, formerly with Purdue University, is now with the Research Laboratory, Dow Chemical Co., Midland, Mich. TP 4505E. Manuscript, July 18,1956. fusion has occurred for t seconds; C, is the concentration of the diffusing substance at the surface of the matrix; Do is the diffusion constant, expressed in sq cm per sec; and + represents the Gauss error function. The corresponding solution for diffusion into a finite solid of thickness, 1, is conveniently written for the change in concentration, C+, at a point midway through the matrix and for times, t, great enough for the following equation to be used4 c1/2/C1=(1/2-2/?e-?2D0t/l2) [2] In Eqs. 1 and 2 the diffusion coefficient is represented by the symbol Do (rather than by D) to emphasize that these equations are valid only for constant values of D. To understand how these equations can be modified to take account of actual variations of D, such as that shown in Fig. 1, first consider the fact that for a given time of diffusion theconcentration at a given point is determined, not by the D value alone, but by the ratio x/vD0 in Eq. 1 and by a similar ratio, l2/D0 in Eq. 2. Even though in fact D varies, it is possible to keep this ratio constant by using a special coordinate system, x,, that varies with D in the appropriate manner. The necessary character of this special coordinate system can be easily visualized by imagining that

Jan 1, 1958

By S. Nakajima, H. Okazaki

Quantitatiue studies of the deformation texture in drawn tungsten wives were made by the X-vay dif-fractottletetr. Experimental results show that the diffraction Intensities are equal to tilose pvedicted from the (1 10). fiber lexlure but the angxla), spreads of. diffraction peaks in the pole distribution curres are different for different diffraction planes and directions. For this reason a modified (110) fiber lextuve model, in which a kind of anisotropy is assumed, is proposed to explain the results. According to this model the poles lying on a line directing front the (110) to the (110) poles in the (1 10) standard stereograpllic projection should show spreads which are different from those lyitlg on a line directing from the (001) to the (001) poles, which is confirmed by the experiments. The anisolvopy and the spveads of the pole positions are large at the outer part of the wires and decrease gradually lowards the inside of the wire. The possibilily of occurrence of such anisolropy in irrelals with fcc stvuctures is discltssed. THE deformation texture of drawn tungsten wires has been assumed by different investigators to be the simple ( 110) fiber texture.' Recently, however, Leber2,3 has shown that a swaged tungsten rod has a cylindrical texture. It changes gradually to the (110) fiber texture by drawing through dies. However, even after drawing to 0.25 mm in diam, the cylindrical texture can still be found in wires together with the (110) fiber texture. This was deduced from the pole figures obtained from the longitudinal section of these wires. Use was made also of quantitative measurements of the pole distribution curves. Leber stated that the angular spread of the pole distribution curves (henceforward called dispersions) are quite different for (400) 45 deg and (400) 90 deg: the former is always larger than the latter. This inequality is accompanied by deviations of the diffraction intensities from the theoretical values for the ( 110) fiber texture. Bhandary and cullity4 have reported similar results on iron wire and explained them by assuming a cylindrical texture. Both Leber3 and Bhandary4 used only the results of the (400) reflection for the determination of the dispersion. The pole figures found by Leber3 and by Rieck5 are largely different. The model given by Leber to explain the effects is in the authors' opinion in some respects unsatisfactory, especially if one looks at other than the (400) reflections. Intensities and dispersions of diffraction peaks are conclusive factors for the determination of the fine structure in wire textures. For this reason we studied them extensively to come to a model which is more suitable to fit the facts. In the following, after giving the experimental set-up, we report about measurements of X-ray diffraction on drawn tungsten wires. Different models to describe the experimental results will be discussed. EXPERIMENTAL GO-SiO2-A12O3 doped tungsten wires drawn to 0.18 mm in diam were used for the measurements. The wires were chemically etched to various diameters down to 0.03 mm. Measurements were carried out for the different wires in order to determine the dependence of the texture on the radius. The wires were cut to pieces of 10 mm length and fixed with paste closely against each other on a flat, polished glass plate. Parallelism of the wires with the surface of the glass plate should be adequate. For the diffraction studies three different X-ray sources were applied, respectively, giving the CuK,, FeK,, and FeKp emission. The measurements were carried out with a diffrac-tometer with a GM counter. The latter was fixed to a certain diffraction angle 20hkl and the diffraction intensity was recorded as a function of the angle of rotation of the specimen around the axis, lying in the specimen surface and perpendicular to the wire axis, as shown in Fig. 1. Measurements were also done with the detector at angles slightly deviating from the diffraction maxima The measured intensities in this case were taken to be equal to the background level. The deviations were chosen as small as possible but large enough to eliminate the influence of the diffraction maxima. The useful range of the rotation angle x of the specimen is generally limited by the wavelength of the X-rays. We have: where and cp is the angle between the wire axis and the normal of the diffraction plane. Intensity measurements were made to find the necessary corrections for counting loss of the GM counter and for distortion resulting from such effects as absorption of X-rays and from inclination of the reflection plane under study with respect to the surface of the specimen. The counting loss was esti-

Jan 1, 1968

By J. Birkinbine

Extended discussions, by inviting attention to problems affecting the conservation of natural resources, have encouraged investigations as to their sufficiency, with the general result that the more thorough the examination, the less cause appears for anxiety as to the exhaustion or serious depletion of these resources.

Jan 1, 1915

By S. A. Mersol, C. T. Lynch, F. W. Vahldiek

The room-temperature microhardness of as-grown and annealed MoaC single crystals was measured on the (0001), {2110), and1012) planes using Knoop and Vickevs indenters at loads ranging front 25 to 1000 g. The orientatimz dependence of hardness with respect to crystal axes was also studied. The average random hardness of as-grown crystals was determined to be 1520 kg per sq nm. Annealing to 2000°C decreased. the average hardness by 150 units. An increase in hardness after annealing at 2200 ;C was noted. Optical and electron microscopy revealed slip and twin traces on all planes studied, as produced by mi-cvohavdness indentations. Basal (0001)(2i10) slip was determined to be the primary slip system and was substantiated by electron transmission microscopy. A secondary {1010)(2110) slip was produced by mi-crohardness indentations. The lattev also produced twinning- of the {10i2)[0001] type, as proven by electron diffraction. Electrical resistivity and elastic-modulus anisotropy were found and correlated with hardness anisotropy and Mo2C crystal structure. Elastic-modulus values were obtained by microhard-uess and ullrasonic methods. Bonding mechanism of Mo2C is discussed. ROOM-TEMPERATURE microhardness indentations are useful for studying hardness anisotropy, slip, and twinning in brittle materials. Slip has previously been produced in this manner in and WS~~.~ Recently, the authors5 reported slip of the {10i0)(11~0) type produced by high pressure and microhardness indentations on hexagonal TiBz (c/a = 1.066) single and polycrystals. This slip system was also reported by French and ~homas' and Taka-hashi and ~reise~ for hexagonal WC (c/a = 0.976) crystals. These results suggest that prismatic rather than basal slip is favored in hexagonal nonmetallic materials having a c/a ratio considerably less than the ideal (1.633). Buerger precession and cylindrical X-ray rotation patterns were previously' taken on cleaved sections of the Mo2C single crystals studied in this work. Th~y were found to be hexagonal MoaC with a. = 3.0233A, co = 4.7344A, and C/O = 1.5660. The latter ratio is close to that of the beryllium metal (c/a = 1.57), which slips primarily on the (0001) plane: but also slips on the (1010) planes.'0 ~irconium" (c/u = 1.59) and titanium12 (c/o = 1.59) deform mainly by slip on nonbasal planes which contain a close-packed direction. This is due to the fact that for these two metals the initial resolved shear stress for slip on the (10i0) prismatic planes is lower than that on the (0001) plane. The prominence of basal rather than prismatic slip in metals of high c/o ratios is shown by cadmium (c/a = 1.89), zinc (c/a = 1.86), and magnesium (c/a = 1.62) which deform mainly by basal slip. However, in case of the latter, by stressing magnesium crystals in tension or compression parallel to the basal plane, slip on (10i0) planes can also be produced.13 Several hardness values for polycrystalline Mo2C are reported in the literature: Biickle ' and Samsonov'~ give a value of 1800 and 1479 kg per sq mm, respectively, at a 100-g load; and Kieffer and Benesovsk~'~ report a value of 1950 kg per sq mm at a 50-g load. ~ott'~ reports a Vickers hardness value of 2000 kg per sq mm, with the load unspecified. A Rockwell A hardness value of RA = 88 has also been reported.'' In the present work, for comparison with single-crystal Mo2C hardness values, a Khnloo value of 1600 It 150 kg per sq mm was found on 99.6 pct pure and 99 pct dense hot-pressed Mo2C. This work was undertaken partly to explain the considerable differences in hardness values reported for polycrystalline Mo2C. EXPERIMENTAL The Mo2C single crystals investigated were prepared by a Verneuil-type process using an electric arc by the Linde Co. of the Union Carbide Corp.lg The largest specimens grown were boules 7 mm in diam by 40 mm in length. The crystals had an average density of 9.04 g per cu cm, with a Mo + C content of 99.8 wt pct. The major impurities were: 100 ppm each Na, Zr, and Ca; 85 ppm 0, 55 ppm Fe, and 10 ppm each Cr and Ta. The crystals were found to be carbon-poor, the average carbon content being 5.73 wt pct (stoichiometric value is 5.89 pct). The molybdenum content was found to be 94.08 pct, which is nearly stoichiometric. Electron-microprobe traverses of selected specimens were done with a Phillips-AMR microanalyzer. Thin-film and carbon replicas were used to prepare electron micrographs. This work was done with a JEM-6A electron microscope. Prior to optical and electron-optical studies, specimens were mounted in Lucite and polished on a vibratory polisher using diamond-paste grades ranging from 9-1 p and Linde A powder for up to 48 hr. Dilute nitric acid was used for thin-section polishing and chemical etching for 1-15 min. Electrical-resistivity measurements at room temperature were taken with a Rubicon bridge, using gold contacts. For hardness measurements, a Tukon Microhardness Tester Type FB with Knoop and Vickers indenters was used. Measurements were taken at loads ranging from 25 to 1000 g; however, the 100-g load was chosen as the standard load. All measurements were taken at room temperature. Indentations of cracking classes 1 and 2 only were considered for hardness determinations.20)21 (There are six cracking classes, ranging from "class 1" for a perfect inden-

Jan 1, 1967

By N. P. Goss

Asterism appearing in X-ray Laue diagrams is an extremely sensitive index of changes in the internal structures of individual grains of polycrystalline metals. It indicates the existence of various forms of subboundary structure or subdivision within the grain. The present viewpoint is that the grain is made up of lattice blocks having substantially the same size and shape.l-4 When these blocks all assume exactly the same orientation, the crystal is perfect and asterism is absent. Cleaves and Thompson5 observed that the hardness of iron is virtually constant over a range of grain sizes. It is quite possible that the subboundary structure caused this, and that the latter is just as important as grain size itself. While the experiments reported here are not conclusive, they do support this viewpoint. Metals can, under certain conditions, be prepared entirely free from asterism, but this preparation does not necessarily require long heating or slow cooling, as will be shown here. In this paper a distinction is made between mosaic and distorted grain structures but the difference is only a matter of degree. In a previous paper9 it was shown that the grains can become distorted even during heat-treatment. The block structure exists inherently, even in a perfect crystal; the size and shape of these crystallites, or lattice blocks, varies, depending upon a number of factors. Goetz, for example: has shown that a metal before crystallizing from the molten state must go through a paracrystalline phase with oriented groups of atoms about 10-l4 to 10-l5 c.c., or 10-15 cm. in size. These crystallites, or blocks, appear to survive the most drastic cold-working, for it has been shown, and more elaborately by Wood's recent work," that cold-working cannot reduce the size of these crystallites smaller than of the order 10-5 cm. The interesting correlation brought out by the experiments of Goetz and Wood is that the block size after severe cold-working is of the same order of magnitude as the groups that formed in the metal just before crystallizing from the molten state. The work of Ewald and Rennenger17 and the now classical experiments of Darwin and James12,13 all strongly suggest the existence of a periodic structure of crystal. lites smaller than the grain itself. Related to this effect is the appearance of veinlike markings in the microstructures. Ammer-man and Kornfeld,16 in their experiments, did not observe any evidence of veining in specimens of alpha iron annealed below A3 and believed that veining was not due to impurities in the iron, as Northcott16 suggested; veining was observed by them only in specimens annealed above A3. Hanemann,16 Schrader and Tangerding found that annealing in hydrogen did not diminish veining and so it could not be caused by oxides. They concluded that veining was due to a slight difference in the orientation of ferrite lattice blocks. This viewpoint is well supported by the evidence presented here.

Jan 1, 1941

By N. P. Goss

Asterism appearing in X-ray Laue diagrams is an extremely sensitive index of changes in the internal structures of individual grains of polycrystalline metals. It indicates the existence of various forms of subboundary structure or subdivision within the grain. The present viewpoint is that the grain is made up of lattice blocks having substantially the same size and shape.l-4 When these blocks all assume exactly the same orientation, the crystal is perfect and asterism is absent. Cleaves and Thompson5 observed that the hardness of iron is virtually constant over a range of grain sizes. It is quite possible that the subboundary structure caused this, and that the latter is just as important as grain size itself. While the experiments reported here are not conclusive, they do support this viewpoint. Metals can, under certain conditions, be prepared entirely free from asterism, but this preparation does not necessarily require long heating or slow cooling, as will be shown here. In this paper a distinction is made between mosaic and distorted grain structures but the difference is only a matter of degree. In a previous paper9 it was shown that the grains can become distorted even during heat-treatment. The block structure exists inherently, even in a perfect crystal; the size and shape of these crystallites, or lattice blocks, varies, depending upon a number of factors. Goetz, for example: has shown that a metal before crystallizing from the molten state must go through a paracrystalline phase with oriented groups of atoms about 10-l4 to 10-l5 c.c., or 10-15 cm. in size. These crystallites, or blocks, appear to survive the most drastic cold-working, for it has been shown, and more elaborately by Wood's recent work," that cold-working cannot reduce the size of these crystallites smaller than of the order 10-5 cm. The interesting correlation brought out by the experiments of Goetz and Wood is that the block size after severe cold-working is of the same order of magnitude as the groups that formed in the metal just before crystallizing from the molten state. The work of Ewald and Rennenger17 and the now classical experiments of Darwin and James12,13 all strongly suggest the existence of a periodic structure of crystal. lites smaller than the grain itself. Related to this effect is the appearance of veinlike markings in the microstructures. Ammer-man and Kornfeld,16 in their experiments, did not observe any evidence of veining in specimens of alpha iron annealed below A3 and believed that veining was not due to impurities in the iron, as Northcott16 suggested; veining was observed by them only in specimens annealed above A3. Hanemann,16 Schrader and Tangerding found that annealing in hydrogen did not diminish veining and so it could not be caused by oxides. They concluded that veining was due to a slight difference in the orientation of ferrite lattice blocks. This viewpoint is well supported by the evidence presented here.

Jan 1, 1941

By F. Keller, A. H. Geisler

ALTHOUGH the subject of precipitation from solid solution appears to be one of the more profitable fields in metallurgy for study with the electron microscope, few comprehensive studies have yet been made. Occasionally electron micrographs have been published that illustrated alleged precipitation in various alloys, but frequently the apparent size, shape and distribution of the particles do not fully agree with those expected from theory or from observations of the precipitate when the particles have grown to a size resolvable with the light microscope. The presence of a Widmanstätten pattern for submicroscopic precipitate particles has been demonstrated for only a few aged alloys.1 The initial problem has been the development of suitable techniques for applying the transmission-type instrument to a field that has been inherently associated with reflection-type microscopes. The various techniques have been the subjects of numerous publications, and instead of describing them individually here it will suffice to say that the oxide film method has proved to be the most satisfactory method yet found for studying the microstructure of aluminum alloys with the electron microscope. This method has the definite characteristic advantage that the actual surface layer of the specimen is examined and not a plastic or silica replica. Doubtless suitable methods for forming and removing the oxide film could be developed for alloys of other metals. The purpose of this report is to point out the characteristics of the oxide film method that have been observed during the studies of numerous aged aluminum alloys and to present the results of these studies. PREPARATION OF SPECIMENS The oxide film method for preparing specimens of aluminum alloys for examination in the electron microscope has been described in detail previously.1,2 Briefly, the procedure consists of preparing the metallographic specimen, forming the film by anodic oxidation and removing the film from the prepared surface of the oxidized specimen. The specimen is polished according to the usual procedure for microscopic examination.3 The specimen may then be etched to remove flowed metal but etching to attack the alloy constituents or to leave them in relief as in the replica processes is not necessary. Electrolytic polishing is not generally recommended. Deep-etched specimens are used frequently, however, since they provide information that is not revealed by polished specimens and frequently present the same information more clearly than do the polished specimens. The surface preparation of specimens to be deep-etched is not important, since specimens that have been subjected to the first wet polishing operation are generally used, but frequently the as-rolled surface is suitable. These specimens are then etched using a suitable macroetching reagent.

Jan 1, 1946

By Susasn Leiter

THAT oxygen in copper has been a source of trouble is well known and that that trouble has been real in the commercial world has been shown by Fuller.1 Moore and Beckinsale's paper2 at the annual meeting of the Institute of Metals in London, 1921, called forth considerable discussion. Prof. T. Turner expressed the opinion that it was not necessary to have cuprous oxide present in sufficiently large quantities to form either globules or seams in order to produce a bad effect if the copper were gassed. This brought up the question of the solubility of oxygen in copper and the authors desired to know whether there were any evidence of such solubility, because their experience was that whenever there was any oxygen in copper it was present in the form of free cuprous oxide, .which was practically always in the form of globules. Later Hanson, Marryat, and Ford3 stated that for all practical purposes cuprous oxide may be regarded as insoluble in copper. However, they found particles of the eutectic to coalesce to form much larger particles. They suggested that cuprous oxide was actually slightly soluble in copper, for it was diffi-cult otherwise to understand the mechanism by which such coalescence could take place. W. E. Ruder, in discussing that paper, said that his experiments had led him to conclude that a slight solubility must exist to allow for the ready coalescence of oxide particles, but conductivity tests convinced him that that solubility was very small. Nevertheless, there appeared to be a state of admixture of oxide with copper that closely resembled a colloidal mixture which at first was mistaken for a true solution and which usually existed at the grain boundaries.

Jan 2, 1926