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By T. Prof. Egleston

IF we may characterize the aim of metallurgists twenty years ago by any one point towards which their efforts were especially directed, we should say it was the idea of adapting "waste products" to some useful purpose, while the energy of to-day seems rather to take the direction of so arranging processes as to have no " waste products." The iron-master of this decade no longer speaks of the waste gases

Jan 1, 1873

By W. C. Winegard, W. J. Bratina

Internal friction characteristics and temperature dependence of the torsion modulus for iodide zirconium containing 2.4 pct Hf were investigated, using a low frequency pendulum technique. The internal friction curve consists of a background which increases as the temperature increases, a maximum at 860°C apparently a background due to the al-lotropic transformation, a maximum due to grain boundary relaxation with an associated heat of activation of 58,000 cal per mol, and an anomaly below 350°C which may be associated with a precipitation perphenomenon, Oxygen in below small amounts reduces the grain boundary maximum substantially. The variation of the torsion modulus at 20°C was found to be 3450 Kg per mm2 for the zirconium used in the present work. IT is well known that small amounts of certain solutes materially affect the ductility of zirconium. Lely and Hamburger,&apos; as early as 1914, found that high purity zirconium exhibited a remarkable ductility, while Fast&apos; has shown that oxygen and nitrogen can cause substantia1 embrittlement. Treco" has recently demonstrated that the ductility decreases sharply with the oxygen content, and that 2 atomic pct O2 embrittles zirconium to such an extent that cold working is impossible. The marked decrease in ductility is difficult to understand in view of the fact that Domagala and McPherson4 report the solid solubility of oxygen in zirconium to be 29 atomic pct at 500 °C. Another metal which behaves much the same as zirconium in this respect is titanium. Pratt et al." investigated the internal friction characteristics of titanium and the effect of oxygen on the internal friction values. It is evident that internal friction measurements are of value for studying grain boundary segregation, as shown by Pratt et al. for oxygen in titanium, by Pearson for oxygen in copper, and by Maringer and Schwope for oxygen in molybdenum. With this in view, the internal friction characteristics of zirconium and the qualitative effect of oxygen on the grain boundary relaxation phenomenon were investigated. Materials and Experimental Procedure The zirconium used in the present work was supplied by the Foote Mineral Co. in the form of wire 0.05 in. diam. The analysis supplied by the manufacturer indicates the amount of hafnium as 2.4 pct, less than 0.01 pct O less than 0.01 pct N,, less than 0.02 pct H,, and less than 0.001 pct C. Additional spectro-graphic analysis indicates the other main impurities as follows: 0.01 pct Fe, 0.05 pct Si, 0.008 pct Cu, <0.005 pct W, <0.001 pct Al, <0.05 pct Mg, <0.001 pct Ni, <0.02 pct Ca, and <0.01 pct Ti. Microscopic examination of the material in the as received condition revealed very fine grains with numerous twins. Specimens were annealed either in situ in the internal friction apparatus or in evacuated silica tubes in an auxiliary furnace. When the specimens were annealed in the auxiliary furnace, they were wrapped in identical zirconium wire to prevent contamination by the container. Metallographic sections were taken in all cases. Some were taken from the specimens used for internal friction measurements after completion of the experiments, while others were taken from control specimens at intermediate stages of the experiments. lnternal friction values were obtained by measuring the free decay of a low frequency torsion pendulum (1 cycle per sec), the suspension of which was

Jan 1, 1957

By D. K. Crampton, H. l. Burghoff, J. T. Stacy

The study of copper alloys of the age-hardening type has received considerable attention, and, among the alloys which the authors have, considered, those containing small amounts of nickel and phosphorus as essential constituents seem especially interesting. Such alloys have attractively great capacity for being hardened and also have relatively high electrical and thermal conductivity in the hardened state. In addition, it has been found that the increase in hardness and strength imparted by aging can be greatly augmented by cold-working, so that excellent combinations of conductivity and strength are obtainnble. In view of the possible importance of the alloys, it was considered desirable to investigate the solubility relationships in the copper-rich portion of the copper-nickel-phosphorus system. This paper present&apos;s some of the results obtained in this investigation to date and also gives propertics of typical alloys that appear to be of commercial interest,. Review of literature Copper-nickel System,.—The binary coppcr-nickcl system has long been known to consist of a series of simple solicl solutions, copper and nickel being miscible at all tempcrat&apos;ures and concentrations. This was establisl~cd by Guertler arid Tammannl in 1907 and confirmed by Tafel2 in 1908. Copper-phosphorus System.—The copper phosporus system has been studied by numerous investigators, so that the copper-rich portion is now definitely known. As most recently determined by Lindlief," his system has a cutectic at 8.38 per ccnt P, cuteetic temperature being 714° C. Components of the cutectic are Cu3P and alpha solid solution. Solid solubility of phosphorus in copper, according to Mertz arid Mathewson decreases from a maximum of about 1.75 per cent at 714&apos; C. to about 0.6 per cent at 300&apos; C.

Jan 1, 1940

By D. K. Crampton, H. l. Burghoff, J. T. Stacy

The study of copper alloys of the age-hardening type has received considerable attention, and, among the alloys which the authors have, considered, those containing small amounts of nickel and phosphorus as essential constituents seem especially interesting. Such alloys have attractively great capacity for being hardened and also have relatively high electrical and thermal conductivity in the hardened state. In addition, it has been found that the increase in hardness and strength imparted by aging can be greatly augmented by cold-working, so that excellent combinations of conductivity and strength are obtainnble. In view of the possible importance of the alloys, it was considered desirable to investigate the solubility relationships in the copper-rich portion of the copper-nickel-phosphorus system. This paper present&apos;s some of the results obtained in this investigation to date and also gives propertics of typical alloys that appear to be of commercial interest,. Review of literature Copper-nickel System,.—The binary coppcr-nickcl system has long been known to consist of a series of simple solicl solutions, copper and nickel being miscible at all tempcrat&apos;ures and concentrations. This was establisl~cd by Guertler arid Tammannl in 1907 and confirmed by Tafel2 in 1908. Copper-phosphorus System.—The copper phosporus system has been studied by numerous investigators, so that the copper-rich portion is now definitely known. As most recently determined by Lindlief," his system has a cutectic at 8.38 per ccnt P, cuteetic temperature being 714° C. Components of the cutectic are Cu3P and alpha solid solution. Solid solubility of phosphorus in copper, according to Mertz arid Mathewson decreases from a maximum of about 1.75 per cent at 714&apos; C. to about 0.6 per cent at 300&apos; C.

Jan 1, 1940

By H. W. Gillett

Many of the parts of motor cars, aircraft, etc., that require strong light construction, hence must be made of high-quality steel, are stressed to the maximum limit only in a very small volume. In parts subject to bending stress a line or even a point may take the maximum stress. A series of endurance tests under repeated bending in progress in the U. S. Bureau of Mines laboratories, like similar tests by other investigators, has shown the great difference in life of sister bars of the same stecl, handled in the same way and tested at the same nominal stress. It is known that a surface notch or scratch greatly increases the local stress over the nominal calculated stress; internal notches, such as those formed by inclusions or sonims, probably have a similar effect. From the tetss made by the Bureau of Mines, the cleanliness of the steel at the dangerous section, or point of maximum stress, seems to be one of the most important factors in determining the life of the piece. The more localized the stress, the more does chance, rather than the average properties, dctermine the life of the steel. The usual test, a tension test of a bar taken longitudinally, is not sensitive to the local drop in strength (or tendency to increase the true local stress over the nominal) because of inclusions, which probably have a more injurious effect in hard heat-treated steels, such as must be used when great strength is sought, than in softer steels. Users of steel who make transverse tests find surprisingly low ductility on transverse bars of dirty steel, though the longitudinal tests may be good. Bending tests, reverse bending tests, and notch-bar impact tests,

Jan 1, 1923

By H. W. Gillett

Many of the parts of motor cars, aircraft, etc., that require strong light construction, hence must be made of high-quality steel, are stressed to the maximum limit only in a very small volume. In parts subject to bending stress a line or even a point may take the maximum stress. A series of endurance tests under repeated bending in progress in the U. S. Bureau of Mines laboratories, like similar tests by other investigators, has shown the great difference in life of sister bars of the same stecl, handled in the same way and tested at the same nominal stress. It is known that a surface notch or scratch greatly increases the local stress over the nominal calculated stress; internal notches, such as those formed by inclusions or sonims, probably have a similar effect. From the tetss made by the Bureau of Mines, the cleanliness of the steel at the dangerous section, or point of maximum stress, seems to be one of the most important factors in determining the life of the piece. The more localized the stress, the more does chance, rather than the average properties, dctermine the life of the steel. The usual test, a tension test of a bar taken longitudinally, is not sensitive to the local drop in strength (or tendency to increase the true local stress over the nominal) because of inclusions, which probably have a more injurious effect in hard heat-treated steels, such as must be used when great strength is sought, than in softer steels. Users of steel who make transverse tests find surprisingly low ductility on transverse bars of dirty steel, though the longitudinal tests may be good. Bending tests, reverse bending tests, and notch-bar impact tests,

Jan 1, 1923

By Rossiter W. Raymond

In the case of The Eureka Consolidated Mining Company v. The Richmond Mining Company of Nevada, recently tried at San Francisco, California, the real defendant was the Richmond Consolidated Mining Company, of London; but this being a foreign corporation, holds its mining property in Nevada through the Nevada corporation of similar name, in which the London Company owns all the stock, except the few shares necessary to " qualify" the American directors. The trial would naturally have taken place in the Circuit Court at Carson City, Nevada, and before a jury. But by stipulation of the parties, the case was tried in San Francisco, before Hon. Stephen J. Field, Justice of the Supreme Court of the United States, Hon. Lorenzo Sawyer, United States Circuit Judge of the Ninth Circuit, and Hon. E. W. Hillyer, United States District Judge, for the District of Nevada. The hearing began July 23d, 1877. The witnesses occupied two weeks, and the argument of counsel three days. Very eminent lawyers were engaged on both sides; for the plaintiff, Messrs. Solomon Heydenfeldt, R. S. Mesick, John Garber, and H. J. Thornton; for the defendant, Messrs. S. M. Wilson, Thomas Wren, and J. J. Williams. The court held the case under advisement until August 22d, when Mr. Justice Field delivered its unanimous opinion in favor of the plaintiff. The action was a complaint in ejectment, and an appeal was taken to the United States Supreme Court. The questions at issue between the Eureka and the Richmond Company in this suit, comprised several points in the construction of the mining law of the United States, and its relation to the customs and regulations of the mining districts, which possess an importance and an applicability far beyond the limits of the case in which they arose. It is my purpose to state these points, the arguments

Jan 1, 1879

By Helmut Thielsch

METALLOGRAPHIC specimens whose surfaces are to be investigated are too thick to allow either light or electrons to pass through them for microexamination by transmission. This difficulty is overcome with optical microscopes by illuminating the surface through the objective lens. For electron microscopes best results are obtained by preparing thin replicas of the surface of the specimen, placing them in the microscope and passing the electron beam through them. Since electron microscopes represent a rather recent invention, they have found little application as compared with optical microscopes. This is true because, aside from the cost of new equipment and development of new techniques, some of the older replica methods necessitated the destruction of the surface from which a thin transparent replica was obtained. In other processes in which the surface is preserved, either too tedious a procedure is required, unsuited to "mass-production " requirements of industrial laboratories, or replicas of insufficient contrast and sharpness are produced. In general, investigations with the electron microscope involve five steps: (I) polishing the surface of the metal specimen, (2) proper etching of the surface, (3) preparing the suitable replica from the surface, (4) examination and photography in electron microscope and (5) interpretation. PREPARATION OF METAL SURFACES Usual metallographic polishing is generally satisfactory. It is important though that the final polish be applied very care- fully, since otherwise evidence of a small amount of deformation might show up even on relatively deeply etched surfaces. A high-power microscope should be used to determine the suitability of the polish and etch. This, of course, is not different from optical examinations, but in these, if a deep etch is used, the problem is less serious. It is frequently difficult to detect with optical microscopes poor polishing aside from superficial scratches before etching. Figs. I and 2 show micrographs of "well" and "poorly" polished nickel etched by immersing the same for 20 min. in a solution containing 8 grams cupricsulphate in 40 C.C. of concentrated HCl and 40 C.C. of H20 (Marble&apos;s reagent). The sample shown in Fig. I was polished in its final stages for 5 min. on a carborundum wheel followed by 10 min. on a rouge wheel, whereas the sample shown in Fig. 2 was polished only I min. on the rouge wheel. Generally, this procedure does not guarantee that the surface of the specimen will be either undistorted or deformed. It was applied here merely to show the effects of good and poor polishing. To the experienced investigator, plastic deformation is

Jan 1, 1946

By Theodore H. Orem

In 1928 Elam,1 discussing the subject of twinning in metals, disclosed that she had observed this phenomenon in aluminum, a metal little susceptible to twinning. The twinning described was one in which the boundary between the twinned portions was not a geometric plane but appeared, in one section, more like a normal grain boundary. Under these circumstances twinning might remain unrecognized by an observer of microscopic sections. She therefore suggested that twinning in aluminum might be much more prevalent than expected. Whereas the parallel composition lines shown in sections of polysynthetic twins were characteristic of the phenomenon of twinning, Elam pointed out that from the absence of

Jan 1, 1963

By R. W. Ells

That portion of Quebec to which the few remarks I propose to make are more particularly intended to apply, viz., the Eastern Townships, has long been known for its mineral wealth, and has enjoyed a reputation for mining enterprises, second probably to no other part of Canada. Capital has been invested in large amounts at various points, some of which has yielded a handsome return to the investors, while in other cases the inevitable results of rash and foolish speculation have followed, much good money has been sent after bad, and the principal result has been a dearly bought expe- .

Jan 1, 1890

By P. A. Freeman, T. W. Healy, D. R. Dixon, L. O. Kolarik, D. N. Furlong

The effect of water, acid and alkali washing on the surface properties of natural magnetite were investigated by microelectro-phoresis. The general control on the isoelectric point ([i]ep) of the natural magnetite that is effected by colloidal and adsorbed silicate species can be reversed by various acid/alkali washing procedures. Added aqueous silicate and aluminium ions lower and raise the [i]ep to values consistent with hydrous silica and alumina coatings respectively.

Jan 1, 1980

By John Birkinbine

The press, trade publications, and special circulars, some elaborately illustrated, have been liberally employed within recent years in this country, to set forth the advantages of various locations as industrial centers, having as a basis the possibility of profitably producing pig-iron at these proposed centers: and special stress has been placed upon opportunities believed to exist at certain points for making iron of a quality suitable for the manufacture of Bessemer steel. The remarkable statements and prophecies made in some of these publications, have suggested the present paper, treating of the influence which location exerts upon the special industries named.

Jan 1, 1893

By Frank Firmstone

In a paper read at the meeting in Cleveland, Ohio, in 1875,* I showed that as a result of changing from open-topped to close-topped furnaces at the Glendon Iron Works, there had been a decided falling off in regularity of working, which we attributed to the very different distribution of the materials in the new method of filling. Subsequent experience has, on the whole, confirmed the opinions then expressed, and in 1881 we decided to try the modification of the Langen charger, shown on the accompanying drawings, thinking by its use to approximate to the distribution obtained by dumping the barrows at six equidistant points in the circumference of the open-topped furnaces. The top of the furnace is closed by a ring-shaped " bell," as we still call it, the outside of which is cylindrical and rests by the turned lower edge on the bored seat of a " loose ring," supported by the lower part of the hopper. The inside of the bell is an inverted frustrum of a cone, the central opening in which is closed by a cylindrical plug, which is prolonged into a pipe to carry off the gas.? This center-plug is connected by rods and chains to sectors on the ends of a forked lever, to the other end of which is attached, by a wire rope, the piston-rod of the blast-cylinder used in opening the top. The rods connected to the center-plug pass loosely through the apexes of triangular frames, to the other angles of which the bell is attached; it thus being suspended by four points when the top is open. When the materials are dumped out of the barrows into the hopper, a part is thrown over the crest of the bell into the space between it

Jan 1, 1885

By C. M. Wayman, M. A. Gedwill, C. J. Altstetter

Cobalt Whiskers were grown by the hydrogen reduction of CoBr,. The fcc = hcp martensitic trans-formation in these whiskers was studied using X-ray and metallographic techniques. Present theories of the fee + hcp martensitic transformation were ex-amined in the light of the present findings Experimental evidence for slip as a part of the transformation mechanism is presented. In the bulk form cobalt is known to undergo a martensitic transformation1 from an hcp to an fcc structure upon heating above about 430°C. Upon cooling, the reverse transformation starts at about 400°C, but does not go to completion except in single crystalline or coarse-grained samples, or upon plastic deformation. The transformation may be thought of as the shearing of close-packed atomic planes in such a way as to change the stacking sequence from ABCABC to ABABAB with a contraction normal to the shearing planes and an expansion in the planes,2 producing a c/a ratio slightly less than ideal. This restacking to give {0001) and (112) 11 (1010) can be accomplished by the passage of a shockfey partial dislocation over every other (111)f plane resulting in a theoretical shear of 19.47 deg. To date there has been no completely satisfactory explanation of how the partial dislocations are produced on the close-packed planes or propagated from plane to plane to give the correct stacking sequence. The object of the present research was to study some of the characteristics of the fcc to hcp transformation in geometrically simple single crystals. It was felt that whiskers of cobalt grown by halide reduction would be ideal specimens with which to study the transformation, because whiskers have the following desirable features: 1) are easily grown as fcc single crystals; 2) exhibit relatively simple geometries; 3) have comparatively low dislocation densities;

Jan 1, 1964

By E. W. Mehal, R. H. Cox

A planar Gunn oscillator was developed for use in a monolithic microwave integrated circuit. The device was designed to operate in the frequency range of 20 to 30 GHz with a continuous wave output. Selective epitaxial deposition was used to form the n+n-n+ device structure in (111)-B semi-insuluting GaAs. The active n- region was about 5 µ thick and was doped to about 2 x 1015 electrons per cu cm by the reactor background. The mobility was -5000 sq cm v-1 sec-1. The n+ epitaxial deposits were doped to 1 x 10" electrons per cu cm using S2Cl2. Planarity of the three DURING the past few years, new microwave devices in discrete form have been developed utilizing GaAs. The next logical step is to combine these devices in a successive deposits was quite good; total overgrowth was less than 1 µ. Metal ohmic contacts were applied to the n+ or n- regions using a Ag-In-Ge alloy. The n+n-n+ devices had symmetric IV characteristics and could be operated C. W. for both directions of device bias. Metal ohmic contacts made directly to the n-region always Produced asymmetric devices. C. W. operation was obtained over the 22 to 28 GHz frequency range. The best performance obtained was 1.5 mw C. LV. output at 28 GHz. microwave integrated circuit. A potential application would be a radar receiver operating in the millimeter wavelength region. The key component in such an integrated circuit is a microwave oscillator, recently described by Gunn.1, 2 Under the influence of a large electric field, high-resistivity GaAs exhibits a bulk negative resistance, and high-frequency current oscillations result. Since relatively high voltage and

Jan 1, 1969

By D. C. Hilty, W. Crafts

The solubility of oxygen in iron containing aluminum has been determined at 1550°, 1600°, and 1650°C and found to be much higher than predicted from theoretical considerations, possibly due to equilibria with an iron-aluminum spinel phase rather than pure AI,O.. The presence of manganese greatly increased the deoxidizing power of aluminum. DEOXIDATION and inclusion formation in steel have proved to be elusive phenomena that are difficult to control in spite of much effort to understand and evaluate the reactions. Study of the problem indicated that more accurate data on the solubility of oxygen in iron containing deoxidizers were essential to further progress, and an empirical determination of oxygen solubilities has been initiated at the Union Carbide and Carbon Research Laboratories, Inc. The investigation has included the effects of aluminum, silicon, manganese, and combinations of these elements at 1550°, 1600°, and 1650°C. The equipment and experimental procedure as well as the results of a study of the effects of aluminum are described below. In general, it was found that the solubility of oxygen in iron containing aluminum is much higher than predicted, possibly because of the formation of complex nonmetallic phases, and that manganese greatly increases the deoxidizing power of aluminum. The generally accepted deoxidation curves for 1600°C are summarized in fig. 1, from "Basic Open Hearth Steelmaking"&apos;. These curves are assumed to represent the solubility of oxygen in the presence of deoxidizers and should indicate the limits of mis-cibility gaps in the phase diagrams of the systems that control the formation and character of non-metallic inclusions as described by Benedicks and Lofquist&apos;. They were derived mainly by application of the methods of thermodynamics to the available experimental observations, and by calculations based on the thermal constants of the pure substances when experimental data were lacking. Among the more notable researches contributing to the development of knowledge of oxygen solubilities are those of Korber and Oelsen8, 4, C. H. Herty, Jr. and associates5,6, Krings and Schackmann7, Went-rup and Hieber8 Schenck and Briiggeman9, Vacher and Hamilton&apos;" and Chipman and co-authors 1,11,12,13 Practically, the deoxidation curves are of limited value in predicting oxygen content and rationalizing deoxidation practices. The reasons for this inadequacy appear to be error from inaccurate data, oversimplifying assumptions, interacting effects of combined deoxidizers, and possibly unknown extra-equilibrium and side reactions. Although inclusion formation is a very complex reaction it must be re-

Jan 1, 1951

By Y. C. Kim, S. L. Barua

M. Armstrong&apos;s paper is very interesting and can be regarded as a pioneering work of applying geostatistics on washed coal. The density levels used in her study are uniformly spaced, which facilitated curve fitting through a proper experimental design. Most of the existing coal washing plants in the US, however, gather washability data at non-uniform intervals which, in turn, affects the goodness of curve fitting. We would like to emphasize the importance of having a proper experimental design, if a similar geostatistical application is to be conducted on washed coal. We, at the University of Arizona, tried the variogram on recovery (Kim, Barua, and Baafi, 1982, SME preprint 82-143) which showed a similar pattern as Fig. 4 of Armstrong&apos;s paper. In both cases, the first experimental variogram value is invariably and inexplicably higher than the second variogram value. Although Armstrong ignores the first point because of "small number of sample points," we did not do so because there were 17 sample pairs. As a consequence, we concluded that the obtained experimental variogram was unsatisfactory and that further research is warranted. In other words, this disagreement in variogram interpretation between M. Armstrong and the University of Arizona begs the question whether the experimental variogram of Fig. 4 truly reflects the spatial correlation in washed coal, assuming there is such a correlation. Finally, we wish that Armstrong could have done a similar study on clean sulfur, which is a vital interest to the coal mines in the US. Her implied remark on sulfur in the concluding section of the paper may turn out to be incorrect because our experimental variograms on clean sulfur at different density levels were even less satisfactory than those on recovery. ?

Jan 1, 1986

By K. R. Grube, D. N. Williams

It is often desirable to perform fatigue studies at relatively high strains and at low strain rates. A low-cost fatigue machine has been constructed for this purpose which has proven quite versatile. This machine is based on the principle of repeated bending of a strip sample over a shaped mandrel. A photograph of a group of fatigue tests in progress is shown in Fig. 1. The test sample is held in place between two shaped mandrels having a flat at their base to grip the sample firmly. A cam-driven loading frame is used to bend the sample alternately over each mandrel. The sample slides freely in this frame and is held in place by a light spring to accommodate increases in sample length. The pivot point for the loading frame is selected so as to minimize movement at the loading point during operation. The number of cycles to failure is recorded by a rachet counter which is kept in operation by a series electrical connection through the sample and is operated by the drive cam. The maximum strain imposed at the sample surface on bending from one mandrel to the other is readily calculated from the relationship, where t is the sample thickness and r is the radius of curvature of the mandrels. The rate of straining can be controlled by control of the cam speed. The device as shown in Fig. 1 is set up to run six samples at ambient temperature. A much larger number of samples can be run at one time without difficulty. ALSO-, by slight realignment of the components the mandrel unit can be enclosed in a separate chamber permitting control of test temperature and environment. This permits a variety of fatigue and corrosion fatigue problems to be studied.

Jan 1, 1963

By R. L. McCarron, G. R. Belton

The diffusivities of oxygen and sulfur in liquid iron have heen determined hy a capillary technique in which the surface concentrations of the solutes were established by means of appropriate H2/H2 and H2S/H, gas mixtures. Total diffusate and concentration profile results are shown to be in good accord, yielding for- 1560 and Supporting results at 1660°C are also presented. The conditions necessary to avoid gas transport control in this type of experiment are discussed. IN spite of their importance in understanding the kinetics and mechanisms of refining reactions, the dif-fusivities of oxygen and sulfur in liquid iron are not well established. Accordingly, as a first step in studies of rates of solute absorption from the gas phase into liquid iron, new measurements of these diffusivities have been made and are presented in this paper. The only published results for the diffusion of sulfur in pure liquid iron are those of Kawai.&apos; He used a diffusion couple technique in which two cylindrical specimens, one containing sulfur and the other with negligible sulfur concentration, were joined together and held in a refractory capillary. After an experiment, the sample was quenched and the concentration distribution of the solute determined. Kawai recognized that significant changes in solute distribution occurred during melting and freezing and he attempted to correct the concentration profiles for these effects to give a sulfur diffusivity of 4.6 x 10-6 sq cm per sec at 1560°C. The method of correction, however, was not rigorous and the uncertainty in this result cannot be easily assessed. Koslov et a1.2 have reported the diffusivity of oxygen in iron as 7.8 x 10"3 sq cm per sec at 1660°C. This value appears to be unreasonably high but, unfortunately, details of their experiments are not available. Shurygin and Kryuk have used the rotating disc method for a study of oxygen diffusion in liquid iron. In their experiments a silica disc was rotated in liquid iron containing oxygen, and the rate of formation of liquid iron silicate was determined by measuring the decrease in weight of the disc. On the assumption that the rate of dissolution was controlled by the diffusion of oxygen in the iron, the diffusion coefficient was computed to be 5.2 x sq cm per sec at 1550°C. However, the Levich equation, which was used to interpret the rate data, was originally de- rived for the case of mass transfer between a solid disc and a single-phase liquid. The hydrodynamic and diffusion boundary layers in the iron stirred by a disc, via coupling of the silicate melt, may be appreciably different from those predicted by Levich&apos;s equations. Recently, Novokhatskiy and Ershov, using an identical experimental method to that of Shurygin and Kryuk, obtained a diffusivity for oxygen in liquid iron of 1.22 x 104 sq cm per sec at 1550°C: no reasons were offered for the disagreement. Schwerdtfeger5 has also recently studied the diffusivity of oxygen in liquid iron. He reacted shallow melts of liquid iron, 0.5 to 1.0 cm deep and contained in high-purity alumina crucibles, with appropriate H20-HZ-He mixtures. The total sample was analyzed, without sectioning, to obtain the average concentration of diffusate. A value at 1610°C of D = 12(3) x 10-5 sq cm per sec was obtained from the results of twenty experiments.= Oxygen profile measurements, which were carried out in three additional experiments using long capillaries and the semiinfinite boundary conditions, indicated a diffusivity about half that computed from the shallow bath experiments. Possible sources of error in Schwerdtfeger&apos;s study will be discussed later in this paper. EXPERIMENTAL TECHNIQUE The essential arrangement of the diffusion cell is shown in Fig. 1. The liquid iron was contained in an alumina capillary, 3 to 4 mm diam and 3 to 9 cm long, which was supported by a hollow alumina pedestal and this whole assembly was held within a movable alumina reaction tube. This tube, which was about 7 mm in bore

Jan 1, 1970

By Helmut Thielsch

MeTallographic specimens whose surfaces are to be investigated are too thick to allow either light or electrons to pass through them for microexamination by transmission. This difficulty is overcome with optical microscopes by illuminating the surface through the objective lens. For electron microscopes best results are obtained by preparing thin replicas of the surface of the specimen, placing them in the microscope and passing the electron beam through them. Since electron microscopes represent a rather recent invention, they have found little application as compared with optical microscopes. This is true because, aside from the cost of new equipment and development of new techniques, some of the older replica methods necessitated the destruction of the surface from which a thin transparent replica was obtained. In other processes in which the surface is preserved, either too tedious a procedure is required, unsuited to "mass-production" requirements of industrial laboratories, or replicas of insufficient contrast and sharpness are produced. In general, investigations with the electron microscope involve five steps: (I) polishing the surface of the metal specimen, (2) proper etching of the surface, (3) preparing the suitable replica from the surface, (4) examination and phorography in electron microscope and (5) interpretation. Preparation of Metal Surfaces Usual metallographic polishing is generclly satisfactory. It is important though that the final polish be applied very carefully, since otherwise evidence of a small amount of deformation might show up even on relatively deeply etched surfaces. A high-power microscope should be used to determine the suitability of the polish and etch. This, of course, is not different from optical examinations, but in these, if a deep etch is used, the problem is less serious. It is frequently difficult to detect with optical microscopes poor polishing aside fiom superficial scratches before etching. Figs. I and 2 show micrographs of "well" and "poorly" polished nickel etched by immersing the sample for 20 min. in a solution containing 8 grams cupric sulphate in 40 C.C. of concentrated HCl and 40 C.C. of Hz0 (Marble&apos;s reagent). The sample shown in Fig. I was polished in its final stages for 5 min. on a carborundum wheel followed by ro min. on a rouge wheel, whereas the sample shown in Fig. 2 was polished only I min. on the rouge wheel. Generally, this procedure does not guarantee that the surface of the specimen will be either undistorted or deformed. It was applied here merely to show the effects Of good and poor polishing. To the experienced investigator, plastic deformation is

Jan 1, 1946