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By R. H. Gautschi, F. C. Langenberg

Rare-earth additions were made to laboratory heats of Type 310 stainless to observe their effect on as-cast ingot structure, nitrogen and sulfur contents, and nonmetallic inclusions. Lanthanum had a grain-refining effect in 30-lb ingots, but results with 200-lb ingots were inconsistent. Cerium, lanthanum, and misch metal lowered the sulfur content when the sulfur exceeded 0.015 pct and the rare-earth addition was greater than 0.1 pct. The rare-eardh content in the metal dropped very rapidly within the first few minutes after the addition. The size, shape, and distribution of nonmetallic inclusions was not changed in 30-lb ingots, but changes were noticed in larger ingots. RARE-earth* additions have been made to austenitic Cr-Ni and Cr-Mn steels to improve their hot workability. The high alloy content of these steels often results in a considerable resistance to deformation and inherent hot shortness at rolling temperatures, particularly in larger ingots. Rare earths in the metallic, oxide, or halide form are usually added to the steel in the ladle after deoxidation although they can be added in the furnace prior to tap or in the molds during teeming. The literature- indicates that the effects of rare-earth treatments on these stainless steels are not consistent, and sometimes even contradictory. Since no mechanism has been presented which satisfactorily accounts for the claimed improvements, the effects of rare earths are a qualitative matter. The work described in this paper was initiated to expand the knowledge of the effects of rare-earth additions on melting variables such as ingot structure, chemical analysis, and nonmetallic inclusions. REVIEW OF LITERATURE Ingot Structure—Rare-earth additions to stainless steels have been reported to cause a change in primary ingot structure in that there are fewer coarse columnar grains. However, the results are inconsistent. While one investigation1 has shown a large reduction in coarse columnar crystals, another2 has been unable to observe this effect, particularly when small ingots were poured. Post and coworkers3 observed ingot structures for a number of years and found that the columnar type of structure is not definitely a cause of any particular trouble in rolling or hammering, provided the alloy is ductile. Knapp and Bolkcom4 found rare-earth additions to be quite effective in preventing grain coarsening in Type 310 stainless steel. Chemical Analysis—Many effects of rare-earth treatment on chemical analysis have been claimed in the literature. Russell5 observed that some sulfur is removed by rare-earth metals, and that a high initial sulfur content improved the efficiency of sulfur removal. Lillieqvist and Mickelson6 report that rare-earth treatment causes sulfur removal in basic open-hearth furnaces, but not in basic lined induction furnaces. Knapp and Bolkcom found no sulfur removal in acid open-hearth and acid electric furnaces, probably because the acid slag can not retain sul-fides. snellmann7 showed that sulfur could be lowered apprecfably with rare-earth additions; however, a sulfur reversion occurred with time. Langenberg and chipman8 studied the reaction CeS(s) = Ce(in Fe) + S(in Fe), and found the solubilit product [%Ce] [%S] equal to (1.5 + 0.5) X 10-3'at 1600°C. Results in 17 Cr-9 Ni stainless were about the same as those in iron. Beaver2 treated chromium-nickel steels with 0.3 pct misch metal and observed some reduction in the oxygen content. He also noted an inconsistent but beneficial effect of rare earths when tramp elements were present in amounts sufficient to cause difficulty in hot working. It is not known whether rare earths reduce the content of the tramp elements or change the form in which these elements appear in the final structure. No quantitative data are available concerning a possible effect of rare-earth treatment on hydrogen and nitrogen contents. However, Schwartzbart and sheehan9 stated that additions of rare earths had no effect on impact properties when the nitrogen content was low (0.006 pct), but served to counteract the adverse effects of high nitrogen content (0.030 pct) on these properties. Knapp and Bolkcom4 analyzed open-hearth heats in the treated and untreated conditions and found the nitrogen content (0.006 pct) to be unaffected. These two results lead to the speculation that rare-earth additions can reduce the nitrogen content to a certain level. Decker and coworkers10 have observed that small amounts of boron or zirconium, picked up from magnesia or zirconia crucibles, increased high-tem-

Jan 1, 1961

By John A. Ruppert, John E. Conley

LIGHTWEIGHT aggregates have been in use for many years in the United States but are now receiving more and more attention by manufacturers and users of concrete shapes. These shapes comprise building blocks, special forms, such as door sills, lintels, floor slabs, and beams. Lightweight aggregate also is adapted for monolithic construction. The increased building activity since termination of the war, together with the widespread shortage of cinders resulting from a general trend toward the use of oil and pulverized-coal fuels, has aggravated the situation. In some localities? new producers of lightweight aggregates have been stimulated to increased efforts to supply the demand. In addition, various estab- lishments of the United States Government have recently given attention to this problem. The National Bureau of Standards, in the Commerce Department, and the Bureau of Reclamation, in the Interior Department, have completed a series of tests on concretes made from some of the available commercial aggregates in order to evaluate their qualities. The tests have been made to focus attention on the desirable properties of good aggregates. This work was done at the request of the Technical Office of the National Housing Agency and Housing and Home Finance Agency. Some time previously, the former office had conducted a survey of the locations where lightweight aggregates are produced.' A study of this information discloses that the producing centers are widespread and that certain areas, notably the region east of the Mississippi River and especially the southeastern states in the sections along the Atlantic Coast, have only a limited number of such plants. The situation has been alleviated to some extent with new plants having been erected near Richmond, Va., and Lansford, Pa. Experiment Stations of the Federal Bureau of Mines at Tuscaloosa, Ala., Norris, Tenn., and College Park, Md., have investigated types and sources of potential raw materials such as clays, shales, and slates, as well as methods and procedures for utilizing these materials for their conversion into aggregates, and have published the data as a Bureau of Mines report.' Structural Uses of Lightweight Aggregates: Production of masonry blocks in the United States has averaged close to a billion units a year for the past three years, and of these it is estimated that more than 40 pct consisted of the lightweight type. It is anticipated that the future will witness an increase in this percentage in view of the superior insulating properties, decrease in dead weight, and ease of handling, transporting, and laying units of this type. Lightweight aggregates are used extensively in multistoried buildings in which the weight of the walls and floors is carried by a structural steel framework. The substitution of a lightweight concrete for normal concrete in a building of this type has brought about in many instances some or all of the following advantages:

Jan 1, 1951

By D. Harker, M. J. Murphy

The mechanism by which age-hardening takes .place is still not completely understood. The principal theories range from the extreme of "precipitaiion-hardening" to that of "order-hardening," with many intermediate gradations. In the hope of obtaining new data on which to base a choice among the many theories, the authors have made electron micrographs of formvar replicas taken from metallic specimens at various stages of age-hardening. The results so obtained on an alloy of 2 per cent beryllium in copper and one of 20 per cent molybdenum in iron will be described in the following pages, as well as the technique used in preparing the replicas. Preparation of Formvae. Replicas of Metallic Specimens This section is concerned with the techniques that have roved successful in preparing formvar replicas for studying the microstructure of metals with the electron microscope. Because of its simplicity and accuracy, the formvar replica1 method developed in the General Electric Research Laboratory has been used exclusively, since it is much simpler than the silica replica method of Heidenreich and Peck2 and produces as good results. The formvar method to be described requires a technique acquired only by practice, and no foolproof set of rules can be given. it is a rapid method and a replica can be obtained in less than five minutes under favorable conditions. This does not mean that perfect replicas can be produced every five minutes, but rather that one can well afford to take several strippings* in order to produce a replica of high quality. The metallographic technique required for replica work—very fine polishing and etching with very dilute solutions—is described here. It can be said, in general, that almost any surface that has been carefully prepared for a photomicrograph at 1000 or more diameters can be used to obtain a replica for the electron microscope. Preparation of Metallographic Specimens The preparation of the metallographic specimens is somewhat more exacting than that usually given to samples to be used for inspection under the light microscope. After much experimentation, it was concluded that the best method consists in polishing the metal through to the coarse cloth, then etching and repolishing on final cloth until the layer of distorted metal is removed. After this procedure has been completed, a dilute etch—to approximately the depth necessary for a micrograph at 1000 diameters—usually produces a sur-

Jan 1, 1945

Jan 1, 1934

By J. C. Williams

THE operations described in this paper are those of the flotation plant of the Valley Forge Cement Co. at Conshohocken, Pa., and concern the use of a particular cationic reagent-namely, DP-243. The role of this reagent in this plant may be better understood by first considering the purpose of beneficiating cement rock in general and the specific problems at the Valley Forge plant. The ultimate purpose of beneficiating cement rock is to obtain a kiln feed of the desired chemical composition in a form suitable for the most efficient kiln operation. The chemical composition is governed by the type of cement to be made. Before government restrictions (the purpose of which is to simplify operations during wartime) limited the types of portland cement a manufacturer is permitted to produce, five principal types of cement were generally recognized by the industry. They are based upon chemical and physical specifications proposed by the American Society for Testing Materials, federal and other governmental agencies, state highway departments, water boards and other users of large quantities of cement. The physical as well as chemical specifications for any particular type of cement necessitate proper proportioning of the major components-that is, the silica, alumina, iron and lime-and it is necessary to establish and maintain definite limits for each in the raw mix. The manufacturer must then prepare a kiln feed of a composition that will yield a final product that will fulfill the desired specification. This step is further complicated for kilns using coal as fuel, by the amount and analysis of the ash introduced. The amount and nature of the dust lost during burning will also affect the composition of the kiln feed. The problem of preparing a kiln feed of the desired chemical composition is not a simple one, and it is the final product that governs the methods used to obtain such a feed. For example, in starting with a material deficient in lime for the mix sought, it may not be sufficient to raise it to the required lime content. The other constituents must also be present in the proper proportions. In some cases, it may be necessary to raise the lime content to a point greatly exceeding that of the final mix, then, by addition of one or more other materials lower in lime, obtain the mix. The rock used at the Valley Forge plant is a metamorphosed argillaceous limestone of the Jacksonburg formation, the same formation as that of the Lehigh Valley cement rock (which occurs approximately 50 miles north), and its oxide composition is similar to that of the latter. The only practical differences between the two are that, as a result of metamorphosis, crystallization of the Valley Forge rock is considerably coarser and it contains less carbon than the Lehigh Valley rock as well as slightly more magnesia in the form of magnesian mica. The calcium carbonate content of the various strata in the Valley Forge quarry ranges from about 65 per cent to over 85 per cent, the average for the entire quarry being somewhat under the requirement for manufacture of cement, which usually is from 75 to 76 per

Jan 1, 1946

By F. J. Deadrick, A. L. Ramirez, R. J. Lytle

This article describes the evaluation of a new geophysical technique used to map fractures between boreholes: electromagnetic geotomography used in conjunction with salt water tracers. An experiment has been performed in a granitic rock mass. Geotomographic images have been generated and compared with borehole geophysical data: neutron logs, acoustic velocity logs, caliper logs and acoustic televiewer records. Comparisons between the images and the geophysical logs indicate that clusters of fractures were detected but single fractures were not.

Jan 1, 1982

By M. J. Duggin

Structural similarities between the E, X, and iron carbides are illustrated. Experimental evidence regarding phase transformations occurring during ternpering reactions in finely divided carbides, thin-film carbides, and carbides which occur in steels is considered and possible mechanisms for the E — x and x — 9 transformations proposed. HOFER1 has shown that within the appropriate temperature ranges carbon monoxide will react with finely divided a iron to form either iron carbide or x iron carbide. He has shown that at an elevated temperature the E iron carbide will transform to the x iron carbide (Hagg carbide) which, upon further elevation of temperature, will transform to 9 iron carbide (cementite). Jack,2,3 using X-ray diffraction methods, has observed that during the tempering reactions occurring in steel the E iron carbide formed in the first stage of tempering passes into two-dimensional platelets of 0 iron carbide during the second stage of tempering. The three-dimensional form of the 0 carbide is formed during the third stage of tempering. Jack suggested2 that the two-dimensional platelets of 0 carbide could be related to the faulted x iron carbide. Okada and Arata4 investigated a Swedish steel containing 1.05 wt pct C and approximately 1.0 wt pct Mn using permeability measurements at low field strength. A Curie point of 360°C was observed in the quenched steel, which indicated the presence of E iron carbide. On tempering at 400°C the specimen developed a Curie point at 230°C, indicating the presence of x iron carbide, and on tempering at 700°C the specimen developed a Curie point at 190°C which was assigned to 0 iron carbide. The carbides were extracted electro-lytically and the use of X-ray diffraction techniques4r5 indicated the carbide with a Curie point of 230°C to be x iron carbide. The Curie points of the carbides are 10 to 22°C lower than the accepted values which is probably due to the presence of manganese in the carbides, since it has often been observed (e.g., Ref, 6) that a partial substitution of manganese for iron in cementite will lower the Curie point of this carbide. Hofer' summarizes additional evidence of the tempering reactions in steel in which E iron carbide, formed during the first stage of tempering, transforms to x iron carbide during the second stage of tempering. During the third stage of tempering, the x carbide disappears as the 0 carbide is formed. By carburizing thin iron films in a CO gas stream, ~a~akura' has been able to produce the E, X, and 0 iron carbides. He found that below 250°C the E iron carbide was formed; between 250" and 350°C the x iron carbide was formed and above 350°C the 0 iron carbide was formed. He has shown that the E iron carbide transforms to form x iron carbide at 380" to 400°C and that the x ir°n carbide transforms to form the 0 iron carbide at approximately 550" C; both of these phase transformations are irreversible. Hofer' presents a review of evidence to show that the sequence of reactions occurring during tempering processes subsequent to the formation of E iron carbide formed by the direct carburization of finely divided a iron is the same as the sequence of reactions which occur during the tempering processes subsequent to the formation of E iron carbide in steel during the first stage of tempering. It is evident from Nagakura's work that identical tempering reactions are found in thin films of iron which have been carburized to form iron carbide. The purpose of this paper is to discuss the structural similarities between the E, X, and 0 carbides and to suggest a possible mechanism by which regions of the E carbide, formed during the first stage of tempering, may transform to the x carbide during the second stage of tempering. For the finely divided or thin film carbides a mechanism will be proposed for the transformation of the x carbide to the 0 carbide during the third stage of tempering, although it will be suggested that there is evidence that such a transformation may not occur in steels. STRUCTURAL DATA OF THE E, X, AND 0 IRON CARBIDES € Iron Carbide. It is evident from X-ray diffractions and electron diffraction', investigations that the metal atoms in the E iron carbide form an hcp structure with lattice constants ah = 2.752A, ch = 4.3534, using electron diffraction, reports the lattice paramet$rs of the superlattice cell to be a = 4.767A, c = 4.354, c/a = 0.9134. He finds that the carbon atoms occupy the octahedral voids in the metal atom structure so as to form a hexagonal stacking sequence with its basal plane parallel to that of the metal atoms. Considerable long-range disorder occurs in the positioning of the carbon atoms, however, which is in agreement with the possible range of composition Fe2C-Fe3C discussed by Hofer.' Barton and ale" have made X-ray diffraction measurements on a sample of E iron carbide extracted from a catalyst in an organic process. Although there were few reflections recorded on the obtained X-ray powder diffraction pattern, they have proposed that the structure could belong to one of the three possible space groups p3m1, P63/mmc, or Pbcn if one assumed the composition to be Fe2C. Nagakura, using electron diffraction data, suggests a space group of P 6322 for a specimen of c iron carbide of apparent composition Fez.&. x Iron Carbide. The x iron carbide has been studied by Duggin and Hofer" and by Jack and wild,' who

Jan 1, 1969

By L. Delisle

This work represents the first step of an attempt to test the applicability of the electron microscope to the study of subgrain structures in copper. Observations on annealed and deformed single crystals and polycrystalline samples of copper are described. IN the course of study of the structure of fine tungsten wires and tungsten rods with the electron microscope, well defined subgrain structures were observed. The size, size distribution, and orientation uniformity of the etch figures varied widely in different samples. Figs. 1 and 2, electron micrographs of a tungsten wire and of a tungsten rod, respectively, are illustrations of the difference in size and size distribution of the etch figures in different samples of the same metal. The observed differences, as pointed out in a previous paper,' appeared to be related to the heat and mechanical treatments of the samples. They were also consistent with the results reported in the literature on the mosaic structure of metals.' For that reason a program of research was initiated in an effort to obtain more systematic evidence of the possible relation of heat and mechanical treatments to the subgrain structure of metals as observed in the electron microscope. The purpose of this paper is to present observations made on the effect of cold work on the subgrain structure of copper. Procedure Starting Materials: Copper was the metal studied because it can be obtained in a high degree of purity, much information is available in the literature on its properties and its response to cold work and heat treatment, it shows no allotropic change, and it is sufficiently hard to be handled without great difficulty. Two groups of specimens were used: 1—single crystals cast from spectroscopically pure copper and 2—polycrystalline samples of oxygen-free high conductivity copper. Single crystals were studied because it was hoped that the elimination of a number of variables, such as grain boundaries, orientation differences, degree of purity, would simplify the problem and perhaps permit a better understanding of the phenomena that would be observed. The polycrystalline samples were designed to give a general picture of the changes considered. The single crystals were made of copper which analyzed spectroscopically to better than 99.999 pct Cu. They were cast in vacuum, by the Bridgman method, in crucibles made of graphite with a maximum ash content of 0.06 pct. The mold design is shown in Fig. 3. It permitted casting crystals of the size and shape required for the experiments, so that the danger of introducing cold work in the original samples by cutting or other machining would be eliminated. The polycrystalline samples were pieces, 3/4 in. long, cut from a rod of oxygen-free high conductivity copper, % in. in diameter. A flat surface, 1/4 in. wide, was milled along the rods, polished, and etched. The samples were then annealed in vacuum at 850°C for 1 hr. Polishing and Etching: Work previously done on tungsten,' polished mechanically and etched chemically," had shown that: 1—the general appearance of the etch figures of a given sample was not altered by repeated polishings and etchings under similar conditions; 2—variations in the time of etching and the concentration of the etchant changed the definition of the etch figures, but did not alter their general size nor orientation distribution within the limits of observation. Further work confirmed the reproducibility of the subgrain structures observed in, 1—single crystals and polycrystalline samples of copper when polishing and etching were repeated under similar conditions, and 2—specimens of tungsten and polycrystalline copper when electrolytic polishing and etching were substituted for mechanical polishing and chemical etching, respectively. On the strength of these observations, it was felt that, if conditions of polishing and etching were kept constant, changes observed in the subgrain structure of a sample upon deformation and annealing would be attributable to such treatments. For that reason the conditions of polishing and etching were kept as constant as possible. The single crystals were polished electrolytically in a bath of orthophosphoric acid in water, in the ratio of 1000 g of acid of density 1.75 g per cc to 1000 cc of solution, under a potential drop of 1.6 to 1.8 V. Electrolytic polishing was selected to prevent the formation of distorted metal in polishing. The same samples were etched by immersion in a 10 pct aque-

Jan 1, 1954

Jan 1, 1944

By M. L. Fuller

DURING the last several years many papers have appeared dealing with the structure of highly polished metal surfaces. The awakening of interest in this subject is due to the applicability of the electron diffrac-tion technique to the study of surfaces. The original theory of Beilby1 considered the surface of polished metals as of the nature of a super-cooled liquid or a vitreous, amorphous solid. The electron diffraction effects from polished metals have been interpreted by many to be a direct experimental proof of the correctness of the Beilby theory. This inter-pretation has been strongly opposed by others, so that at the present time the subject is in an uncertain and controversial state. In the present paper new, and hitherto unpublished, electron diffrac-tion effects from polished zinc are described. These observations indicate that the polished surface of zinc is crystalline.

Jan 1, 1938

By G. S. Ansell

RCENTLY, in investigating the high-temperature creep properties of an aluminum, SAP-type alloy, MD 2100, fabricated by Professor F. V. Lenel of Rensselaer Polytechnic Institute, Ansell and Weertman1 found unusually low creep rates. These creep rates are 4 or 5 orders of magnitude lower than is predicted by the slowest creep mechanism based upon dispersion-hardened alloy theory. They ascribed these results to a lack of both normal active dislocation sources and a continuous three-dimensional dislocation network. If one couples these results with the following factors of production and microstructure: 1) The compacted and sintered aluminum powder compact is hot-extruded, with an extrusion ratio of 25:1.2 2) The alyminum oxide particles are approximately 140A units thick, and have a spacing varying from 0.05 to 1.5 1. 3 3) The alloy has plate-shaped grains with minor axes of about 5 X 10 -3 mm and major axes several orders of magnitude greater than this.'

Jan 1, 1960

By Thomas Fraser

BECAUSE of the present interest in the subject of sulfur in coal and its removal, such information as is available in the coal-washing literature on the various factors that determine the adaptability of a coal for wash- FIG. I.-COAL-WASHING TABLES OF ONE-FOURTH COMMERCIAL SIZE. ing have been collected and are presented here together with some observations based on results of experimental work carried out in the coal-washing laboratory of the mining department of the University of Illinois, and investigative work at Illinois washeries in connection with the work on reduction of the sulfur content of coal, being carried on at the Urbana Station of the.U. S. Bureau of mines. This investigative

Jan 9, 1919

By C. W. A. Newey

I would like to make the following points in connection with the studies of the deformation of NiAl reported in the recent paper by Wasilewski, Butler, and Hanlon. 1) Much of their paper is concerned with demonstrating that slip occurs on either {110)(001) or {100)(001) systems. In their discussion they state "the existence of (001) as the basic slip direction can thus be considered established." This fact was established by the earlier studies of Ball and Smallman.32 Ball and Smallman also concluded that the slip plane was of the type (110) and they showed that cross slip or pencil glide on orthogonal (110) planes could produce macroscopic slip on planes of the (001) zones, e.g., (100). Wasilewski et al. refer to this paper by Ball and Smallman but not in connection with the slip system determinations. 2) Wasilewski et a!. eliminate the possibility of (111) slip in NiAl on dubious grounds. Their statement that ('the very high yield strengths of the (100) oriented crystals", in which (001) slip is constrained, "immediately ruled out the possibility of {110)(111) slip" cannot be accepted unequivocably; it would be reasonable if the crystals were completely brittle but they are not, as Wasilewski et al. and others33734 have shown. Their elimination of the possibility of (111) slip in a crystal compressed along [227] is misleading since there is no obvious reason why (111) slip should occur in a crystal of this orientation. In fact, from an analysis of the macroscopic surface markings on deformed (100) stoichiometric crystals, Pascoe and Newey34 have deduced that slip occurs on systems of the type {211)(111) and {321)(111). 3) Polycrystalline NiAl is known to undergo general deformati~n.Having emphasized that general deformation is impossible if only (100) slip occurs, it is a pity that Wasilewski et al. do not attempt to account for the disagreement between theory and their experimental results. Of course, (111) slip can provide the additional independent systems required for general deformation.

Jan 1, 1969

By Robert Sisselman

Saving time and energy at Consolidation Coal Co.'s Rowland mine is realized by exploiting its coal deposits via three mining methods. Surface, auger and underground techniques are uniquely combined with specialized transport vehicles to coax the coal from seams unduly protected by topography and lithology. These factors account for what is believed to be the swiftest and most economical means of working the Beckley, W. Va., property.

Jan 1, 1970

By C. G. Dunn, P. K. Koh

THE primary recrystallization texture in cold-rolled silicon iron, which is the matrix texture for developing the Goss texture or the cube-on-edge texture by secondary recrystallization at temperatures near 900°C,1-5,21 has not been adequately described. Thus from the present available information, it is not possible to explain satisfactorily both the grain-growth selectivity of the matrix and the often observed magnetic torque curve, which itself provides some information on the texture. Also lacking is information on the special annealing texture that develops in this material when the annealing temperature is 1200°C or higher and the rate of rise to temperature is extremely rapid. From the work of May and Turnbull5 and from unpublished work, it was known that isothermal annealing near 1200°C tends to reduce the extent of secondary recrystallization and that a much weaker cube-on-edge texture results if appreciable normal grain growth replaces secondary recrystallization. Koh and Dunn6,7 have obtained additional information on complex primary recrystallization textures from further studies made after normal grain growth. In these instances the initial textures were retained during normal grain growth. A similar result reasonably could be expected in the present study except for the presence of a grain growth ihibitor1-5,8,9.21 and its tendency to allow only a few grains to grow. However, any information on the orientations of grains in the special annealing texture, even if far from representative of the initial matrix texture, would provide useful information on the nature of the matrix texture. In the present texture study the method of Newkirk and Bruce,10 which is based on the methods of Geisler" and Schwartz, 12 is used to obtain a complete (110) pole figure of the primary recrystallization texture. The high-temperature annealing texture is determined simply from the orientations of a large number of selected grains. The kinetic nature of the process that produces the annealing texture is treated elsewhere13 and it is shown that a form of secondary recrystallization with a very high rate of nucleation occurs during rapid annealing at high temperatures. EXPERIMENTAL PROCEDURE Commercial 0.014-in. cold-rolled silicon iron strip (3.16 wt pct Si), prepared by two stages of cold rolling with an intermediate short anneal, was given a decarburizing 3-min anneal at 800°C. Me-tallographic studies indicated complete recrystallization. Short-time anneals at 900° C and at higher temperatures proved that secondary recrystallization had not begun at 800°C, in fact, the short additional anneals were still in the induction period of secondary recrystallization. A rapid rise to an annealing temperature of 1260°C (2300°F) was obtained in a BaC12and NaCl fused salt bath. The structures that resulted from anneals in the range 12- to 1000-sec duration were relatively finegrained, even though the growth was a form of exaggerated grain growth13 or secondary recrystallization with a high nucleation frequency.= Many of the grains were large enough for an X-ray study using a 5-mil X-ray beam. A transmission Laue Camera and an optical-mechanical stage for moving the grains into the X-ray beam were used. A total of 325 grains were X-rayed in this manner and the grain orientations determined. Complete (110) pole figures were obtained for the primary recrystallization texture using CoKa radiation at 30 kv in the back-reflection range, such as (220) for (110) poles, as described recently by Newkirk and Bruce.10 The low voltage serves to reduce the spurious white radiation to a minimum. A filter of 0.001-inch iron foil was located in front of the detector slit for transmission and in front of the beam slit for back reflection. A new and improved specimen holder extended the useful tilting angle range for transmission to 70 deg instead of 60 deg as previously reported.' A torque magnetometer was used to obtain the magnetic torque curves for a number of l-in. diam disk specimens. RESULTS The (110) pole figure of the material after recrystallization at 800°C is shown in Fig. 1. The positions of the pole concentrations are found to be

Jan 1, 1961

By F. Twyman, D. M. Smith

Those chemists (they are still greatly in the minority) who use the spectroscope, use it very often, and find it almost indispensable. As a means of detecting minute quantities of the metals it is unrivalled. A metal can be readily distinguished in the presence of any other element, compound, or mixture without the necessity of separation. The qualitative analysis of the metallic constituents of a substance, which the spectroscope gives so easily, is a sure basis for planning a chemical analysis. As the determination of each element proceeds the purity of precipitates may be checked as often as desired. If, possessing these advantages, the spectroscope has been neglected in general chemistry, it is not surprising that it was neglected in metallurgical chemistry; for many of the impurities which are of industrial interest, even when they are present in a metal or alloy in small quantities, are not then always easily detected by the examination of their visible spectrum. The history of the development of the art has been given in Bureau of Standards 19cientific Paper No. 444. The Development of Analysis by Spectrogbaphy Fig. 1 shows, by means of photographs taken with a quartz spectro-graph, what a valuable region of the spectrum is excluded if one has a visual instrument only. Wave length 4023 is about the end of the visible spectrum, the region from 3800 to 1854 being invisible. It is easy to understand then how it is that the vigorous resuscitation of spectrum analysis which has commenced in the last few years has been associated with the use of the quartz spectrograph; notwithstanding that the most useful instrument for the general inorganic chemist to have at his elbow, after the balance, is a good visual spectrometer.(1) 1 The revival of spectrum analysis is to be attributed chiefly to the work of W. N. Hartley with his co-workers, and to A. de Gramont. Hartley,

By John D. Wiebmer

Kansas, with its thin seams and tough overburden, may not be anyone's first choice for a coal mining operation. But there are operators making it pay through careful attention to mining techniques and aggressive marketing in the local region. One of the few Kansas coal operators is Bill Patch, who has been in the business for 28 years. Beginning with a single dragline operation near his home in Welch, Okla., Bill's Coal Co. weathered some lean times during the "soft" coal market of the 1950's and 1960's. But his tenacity paid off when new markets began opening up, and the company has grown by leaps and bounds in recent years. In 1975, the Fort Scott mine opened in Bourbon County, Kansas; in 1976, the Porter mine began production in Wagoner County, Okla.; in 1977, the Fulton mine opened near Fulton, Kansas. In addition, the original Welch mine in Oklahoma is still a producer, and this year the company will open a new mine at Chetopa, Kansas.

Jan 9, 1978

[ ] For President-Elect Leo F. Reinartz has been nominated for the Presidency of AIME in 1954. Mr. Reinartz is now vice-president, special operating development, Armco Steel Corp. He was born in East Liverpool, Ohio, and graduated from the Carnegie Institute of Technology as metallurgical engineer. He joined Armco in 1909 as a chemist and then became open hearth foreman; assistant superintendent, open hearth dept.; superintendent, open hearth dept.; assistant general superintendent; works manager, East works; manager, Middletown div.; and assistant vice-president, successively. Mr. Reinartz has been active in many technical societies and delivered papers before several. He has been the recipient of the Alumni Award from Carnegie and holds life honorary membership in the AIME National Open Hearth Conference. One of the organizers of the National Open Hearth Conference, Mr. Reinartz was Chairman, Executive Committee (1927 to 1946) and is presently Chairman of its Finance Committee. In October 1951 he was an American Conferee at the First World Metallurgical Congress held in Detroit. An AIME member since 1925, Mr. Reinartz has been active on numerous committees of the Institute.

Jan 1, 1952

By S. R. B. Cooke, W. Philippoff, Donald E. Cadwell

THE importance of contact angles in flotation has long been recognized, but little has been done to get quantitative relationships between the surface coverage of the mineral by the reagent, the length of the hydrocarbon chain, and the contact angle. It is well known that for a complete monolayer on the surface of a mineral the contact angle 8 is determined only by the reagent1 and principally by the chain length of the hydrocarbon radical. Although for flotation the monolayer usually is regarded as being complete, early experiments of Wark and Cox&apos; showed that at very small concentrations of potassium ethyl xanthate the contact angle on galena changed in a continuous way from 0&apos; to the equilibrium value of 60". Further, Gaudin and Vincenta showed a similar continuity using heptylic acid and sphalerite. This shows that with probably incomplete monolayers, 0 varies with the degree of surface coverage. At the time these experiments were made it was impossible to measure the actual amount of surface coverage, especially since the decrease of the collector concentration in the liquor could be influenced by chemical side reactions. Through the use of the radioactive tracer method for the measurement of the amount of collector adsorbed on the surface of the mineral, Gaudin and Bloecher&apos; were able to determine accurately the actual surface coverage of dodecylamine acetate on quartz, but they did not measure any contact angles. It is believed that the relationship between the surface coverage and the contact angle is extremely important in flotation, especially as Gaudin and Bloecher showed that a 95 pct recovery is possible with a coverage of only 5 pct. Theoretical Considerations The work of adhesion W is the energy bound (in ergs per sq cm) when an interface is formed. It is determined by the difference of the free surface energies (surface tensions) of the respective phases 7j and yZ before contact and the interfacial free surface energy y, after contact. The definition of the contact angle permits the elimination of the unknown surface energy of the solid and hence the calculation of W from the surface tension of the liquid y and the contact angle 8: W = y (1 + COS0) [1] Consider a surface consisting of two components, identified as 2 and 3, 1 being the liquid. The amount of 2 in the composite surface is x, where 0 < x < 1. The respective contact angles with 1 and air are 8, and 8.. The total work of adhesion of such a surface is the sum of the values of the components multiplied by their respective areas. A formal relation can be written: Wm = x-W2+ (l-x)-W, [2] in which W, is the work of adhesion of the composite surface. Eq 1 can be introduced into Wt and Wa, but in the case of W, some discussion is needed. If the two components are segregated, each component forming an integral part of the composite surface there is no physical meaning for a contact angle 8m calculated from W,, by using eq 1. If, on the other hand, the area of each patch of the components is small in comparison with, say, the diameter of the bubble used in measuring, it could be expected that 0m would have a physical significance, because of the action of the surface tension of the liquid-gas interface tending to smooth out sharp corners. How small these patches would have to be is difficult to predict, but by using composite surfaces with microscopically

Jan 1, 1953

By Charles W. Sweetwood

THE Western phosphate field, virtually ignored for 40 years, has been undergoing a rapid climb to economic importance. Until World War II there seemed to be no reason for developing the phosphate rock region of the Intermountain Empire. But the tremendously increased demand for food production and the needs of many branches of the chemical industry changed all that. Quite suddenly a report made by the U. S. Geological Survey at the turn of the century became important. The survey showed that 60 pet of the nation&apos;s phosphate reserves were in the western phosphate field. Simplot Fertilizer Co. was one of the first to become actively interested in the development of the area. In August, 1945 the company began exploration of the Phosphoria Formation on the Fort Hall Indian Reservation. The result was the Gay Mine, about 18 miles east of Indian Agency Headquarters at Fort Hall, Idaho, developed to supply high grade phosphate rock for processing into superphosphate fertilizer at the company&apos;s Pocatello plant. Six ft of high grade oolitic phosphate rock (ranging from 32.5 to 34.5 pet P2O5) were discovered at the base of the Phosphoria Formation by diamond drilling and dozer trenching. High quality and thickness, plus the fact that the formation lay flat and near the surface made strip and open pit mining possible. In one year of mining, starting June 1946, a total of 53,000 tons of main bed oolitic phosphate rock was hauled to Pocatello for processing into supersulphate. The first year&apos;s operation was in

Jan 1, 1952