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By AIME AIME

LOCAL COMMITTEES. GENERAL RECEPTION COMMITTEE.-Mr. and Mrs. H. S. Chamberlain, Mr. and Mrs. J. T. Lupton, Mr. and Mrs. T. H Lasley, Mr. and Mrs. R. S. Faxon, Mr. and Mrs. H. Clay Evans, Mr. and Mrs. C. E. James, Mr. and Mrs. B. F. Thomas, Air. and Mrs. H. S. Probasco, Mr. and Mrs. W. M. Lasley, Mr. and Mrs. L. W. Llewellyn, Mr. and Airs. T. G. Montague, Mr. and Mrs. E. B. Thomasson, Mr. and Mrs. C. F. Milburn, Mr. and Mrs. C. A. Raht, Mr. and Mrs. C. C. Notting¬ham, Mr. and Airs. Z. C. Patten, Mr. and Mrs. Willard Warner, Mr. and Mrs. S. R. Read, Mr. and Mrs. Carl White, Mr. and Mrs. M. M. Allison, Air. and Mrs. C. E. Buck, Mr. and Airs. H. F. Temple, Air. and Mrs. M. M. Hedges, Mr. and Airs. X. Wheeler, Mr. and Airs. John A. Patten, Air. and Airs. N. T. Montague, Mr. and Mrs. R. H. Williams, Mr. and Mrs. T. R. Preston, Mr. and Airs. Morrow Chamberlain, Mr. and Airs. T. C. Thompson, Mr. and Airs. T. L. Montague, Mr. and Mrs. O. L. Hurlbut, Air. and Mrs. C. A. Lyerly, Mr. and Mrs. Garnett Andrews, Air. and Mrs. M. B. Ochs, Mr. and Airs. Webster James, Mr. and Mrs. D. P. Montague, Mr. and Mrs. Z. C. Patten, Jr., Mr. and Mrs. W. A. Sadd, Mr. and Mrs. J. B. Pound, Air. and Mrs. George D. Lancaster, Air. and Airs. J. F. Johnston, Mr. and Mrs. R. W. Barr, Air. acrd Mrs. W. B. Davis, Mr. and Airs. Douglas Baxter, Air. and Mrs. W. R. Crabtree, Mr. and Mrs. Lewis M. Coleman, Mr. and Mrs. Newell Sanders, Mr. and Mrs. E. Y. Chapin, Mr. and Mrs. W: B. Riddell,. Mr. and Mrs. J. B. Frazier, Mr. and Mrs. John A. Moon, Mr. and Mrs. C. D. Mitchell, Dr. and Airs. J. H. Race, Mr. and Airs. A. W. Chambliss, Mr. and Mrs. J. P. Smartt, Mr. and Mrs. J. F. Tarwater, Mr. and Mrs. L. D. Drewry, Capt. and Mrs. A. B. Putnam, Mrs. Minnie C. Ewing, Mr. G. F. Meehan, Mr. Sam S. Gerstle, Mr. P. A. Brawner, Mr. C. M. Preston, Air. George M. Guild, Mr. L. M. Mansfield, Dr. J. W. Johnson, Dr. J. AI. Hogshead. EXECUTIVE COMMITTEE.-H. S. Chamberlain, Chairman; H. S. Probasco, C. M. Preston, H. Clay Evans, J. T. Lupton, M. B. Ochs, C. C. Nottingham, Al. Al. Alli¬son, R. S. Faxon, C. E. James, C. A. Raht. EXCURSION TO CHICKAMAUGA PARK.-T. C. Thompson, Chairman; B. F. Thomas, G. F. Meehan, Morrow Chamberlain, W. J. Bass, J. K. McGoodwin. EXCURSION TO HALES BAR LOCK AND DAM.-R. H. Williams, Chairman; John A. Patten, Newell Sanders, George M. Guild, Capt. A. B. Putnam. EXCURSION TO ROCK-WOOD.-F. H. Clymer, Chairman; T. L. Brown, T. A. Wright, J. P. Tarwater, T. L. Peterman. INSTITUTE HEADQUARTERS.-The Hotel Patten. THE first session, held Thursday evening, Oct. 1, in the Banquet Hall of the Hotel Patten, was called to order by Capt. H. S. Chamberlain, Chairman of the Local Committee, who, in behalf of the city of Chattanooga, extended a hearty welcome to the members and guests of the Institute.

Nov 1, 1908

By A. G. Metcalfe, A. Siede

The hardening of annealed copper during fatigue testing appears to be independent of the applied stress and to occur largely within the first 4000 cycles. Copper hardened by fatigue is more resistant to annealing than copper hardened by static means, and softens by a multistage process. Creep studies at 300°C show that copper hardened by fatigue also has greater resistance to creep than statically hardened copper. Some theoretical explanations are discussed. RECENT interest in the behavior of metals subjected to fatigue stems from observations of phenomena which could not be explained by current theories of the structure of metals. In 1953 Bullen et al.l showed that the hardening caused by fatigue at low stresses did not cause severe bending of the lattice as did hardening by static methods. This was later confirmed by Wood, 'and Broom and Ham.3 Clarebrough et al4 showed that as the stress level used in fatigue hardening was increased, bending of the lattice was introduced, eventually approaching that of metals deformed by conventional cold-working methods. The type of hardening introduced by fatigue has other interesting characteristics. Kemsley5 showed that copper fractured by fatigue at low stresses resisted annealing as compared to copper hardened an equal amount by static means. The work of Clarebrough etal, shows that the manner of energy release during annealing differs for fatigue-hardened and statically hardened metal in both magnitude and temperature range of release. In addition to hardening of the lattice, fatigue has been shown to cause softening in materials previously hardened by static methods,5 and also in age-hardened alloys.7 The superposition of a small fatigue stress on the static loading of high-temperature alloys has been shown to increase their resistance to creep.' The present work was an attempt to determine the relationship between fatigue hardening, resistance to annealing, and the creep properties of pure copper. EXPERIMENTAL PROGRAM The program described here was designed to answer three questions: 1) Can stress-cycle combinations well below the failure values give significant increases in hardness? 2) Does hardening, under different stress-cycle combinations, give increase resistance to annealing? And if so— 3) Does superior resistance to annealing confer superior creep properties over statically hardened material? Three-quarter hard OFHC copper was annealed in vacuo at 550°C for 1 hr to produce a strain-free material having a fine grain size and uniform hardness. (The standard deviation of the mean hardness of the annealed samples was less than + 1.9 Dpn). Annealing was performed after machining the fatigue specimens so as to avoid work-hardened surfaces. Jigs were used to avoid distortion. The fatigue properties of the annealed copper were determined using an accurately aligned Baldwin-Sonntag SF1-U machine operating at 1800 cycles per min. This limited the minimum number of cycles which could be examined to about 4000 stress reversals. Since failure resulted in specimen damage, hardness increase with number of cycles was measured by testing specimens fatigued to different fractions of the failure values. The results are shown in Fig. 1, and are superimposed on the S-N curve of the copper in Fig. 2. The resistance to annealing of fatigue-hardened material was compared to that of material hardened by uniaxial tensile straining. Specimens hardened to equal values by both methods were progressively annealed for 1 hr at temperature in vacuo. After each annealing treatment the hardness was measured using a Leitz Durimet hardness tester with a 500-g load. At least five tests were made for each hardness determination. The standard deviation for individual specimens varied from 0.26 to 1.48 hardness points. The results are shown in Figs. 3 to 5. The discontinuous nature of the annealing process has been brought out by drawing idealized curves through the data points. This can be justified by the consistency of the results as well as by general agreement with results of Kemsley.5 The creep resistance of fatigue-hardened and

Jan 1, 1960

By Tasuku Fuwa, John Chipman

Equilibrium data on the reactions of gases with carbon and oxygen dissolved in liquid iron are reviewed and correlated. A source of error in oxygen analysis of graphitic samples is exposed. New experimental data on the oxygen content of high -carbon iron in equilibrium with carbon monoxide indicate that the activity coefficient of oxygen is decreased by additions of carbon. The carbon-oxygen product decreases slightly with increasing carbon content. In recent years a number of investigations have been reported dealing with the equilibria between carbon and oxygen in liquid iron and gases containing carbon oxides. The laboratory study of these reactions dates back to 1931 with the publication of a paper by Vacher and Hamilton' on "The Carbon-Oxygen Equilibrium in Liquid Iron". The principal object of this study was to obtain data on the reaction shown by Eq. [3] below; their data and others by vacherZ permit evaluation of the other equilibrium constants as well. Subsequent studies have been reported by Matoba, Phragmen and Kalling and by Marshall and Chipman.5 The equilibria may be expressed by the following three equations: C + CO,= 2CO;Kl = Pc° [1] 0-+CO = CO,;K2=-P co, "0.PCO c + O = CO; K3 = In the equilibrium constants, ac and a0 are taken as equal to [% C] and [% 0] respectively in the infinitely dilute solution. At finite concentrations an activity coefficient is introduced such that ac =fc [%C], and so forth. It is to be noted that these equations represent only two independent relations, the third being derivable from any two. Richardson and Dennis have determined the conditions of equilibrium in reaction [I] at temperatures of 1560" to 1760°C. Their results have been confirmed by Rist and chipman7 who have shown how the data may be extended to cover the entire range of liquid compositions at temperatures from the eutectic up to 1760°C. An approximate confirmation has been reported by Fuwa and chipman.' These investigations also established the activity coefficient of carbon which was shown to increase rather rapidly with increasing concentration. For the very dilute solutions the value of Kl is expressed in the equation: log^i = - 7280/T+ 6.65 This equation leads to a value of Kl = 430 at 1540° C in excellent agreement with the average value of Marshall and Chipman.5 It is shown as line 1 in Fig. 1 together with the experimental observations. In the case of reaction [2] the direct experimental results can be supplemented by observations on the corresponding reaction with hydrogen, namely reaction [4]:

Jan 1, 1961

By B. C. H. Steele, C. B. Alcock

In choosing solid oxide electrolytes for use in the measurement of thermodynamic quantities at high temperatures, the two most important criteria are the values of the partial ionic and electronic conduc tizities. Measurements of these conducticities have been made for some Group IVA oxides and solid solutions of these oxides with CaO, Y2O3, and La2O3. The total conductivities as a function of temperature. oxygen partial pressure, and composition were determined, as well as the electromotive forces of cells in which the oxygen partial Pressures of the electrodes were between 10-7 and 10-29 atm at 1000°C. Additional factors that influence the experimental arrangements, such as the operating temperature, the appropviate cell atmosphere, and electrode kinetics, are also discussed. IT has long been recognized that galvanic cells incorporating solid electrolytes can possess many advantages for the measurement of high-temperature thermodynamic data. Unfortunately, the electrical-transport properties have only been established for a few solid electrolytes, although attempts have been made, and are still being made, to use such materials as porcelain' and magnesia.' Kuikkola and Wagner have discussed3 and demonstrated4 various applications of solid electrolytes, and, in particular, their work stimulated the electrochemical measurement of oxygen activities using cells incorporating the solid oxide electrolyte, Zr0.85Ca0.15O1.85 The excellent characteristics of this oxide electrolyte have been confirmed by the investigations of Kingery et al.5 (oxygen ion diffusion), Carter and Rhodes6 (zirconium and calcium ion diffusion), and Weissbart and Ruka7 (electronic transference number). However the observations of Peters and Mobius,8 later confirmed by Schmalzried,9 indicated that the electronic component of zirconia-based electrolytes could become significant at low oxygen chemical potentials. Under these conditions, thoria-based electrolytes have obvious advantages arising from their superior thermodynamic stability. It was known that certain thoria solid solutions possessed defect fluorite structures containing anionic vacancies (cf. Zro.85Cao.l50O1. 85), although data on their electrical properties were conflicting. Kiukkola and wagner4 concluded that thoria-based electrolytes exhibited appreciable electronic conductivity, whereas Peters and Mobius8 mentioned that the electronic conductivity only became important at high oxygen partial pressures, but gave no further details. In addition, both Kiukkola and wagner4 and Peters and Mann'" had determined the oxygen chemical potentials associated with the Fe-FeO, Co-COO, Ni-NiO, and Cu-Cu2O equilibria, and it was not known whether discrepancies in their results could be attributed to the different cell design, or the thoria-based electrolyte used by Peters and Mann. These uncertainties have been resolved during the present investigation into the measurement of low oxygen chemical potentials, and transport properties of the relevant oxide electrolytes are presented and discussed. Other experimental difficulties associated with low oxygen chemical potential measurements are also described, with particular reference to the Nb-O system. 1. THEORETICAL CONSIDERATIONS Oxide systems of potential use as solid electrolytes possess a large energy gap between the valence and conduction bands. Little is known about the defects present in these wide-gap metal oxides as a function of impurity content and deviations from stoichiom-etry, or the mechanisms by which electronic charges move in these solids. For these materials it is convenient to represent the measured conductivity as the the sum of three terms: where a, is the conductivity due to positive hole conduction (p type), and oe is the electronic conductivity due to electron conduction (n type). U there is a large concentration of ionic vacancies fixed by composition then the ionic contribution will not be a function of oxygen pressure. Although the possibility of a pressure-independent electronic component also cannot be ignored, it is likely that such a term would only become significant at very high temperatures, and in general the positive hole conduction will increase with increasing oxygen pressure, and the electron conduction will increase with decreasing oxygen pressure. It follows that the total conductivity is related to oxygen partial pressure as follows:

Jan 1, 1965

By D. R. Walker, M. C. Shaw

Dimitri Kececioglu (Allis-Chalmers Manufacturing Co., Milwaukee)—The idea of applying metal cutting theory to comminution and vice versa is very impressive. Among others, the demarcation of wheel-grinding data into two regions, namely Kick's and Rittinger's, draws attention here. A study of Figs. 6 to 9 shows the following: In Fig. 6, 1 point out of 8; in Fig. 7, 4 points out of 26; in Fig. 8 only 1 point out of 13; and in Fig. 9 practically none out of 13 points fall out of curve No. 2. Also when grinding particles smaller than 5x10." in. it is difficult to measure very accurately the grinding forces, chip geometry, and particle size. In view of the above it would be difficult to make a positive and distinct demarcation of the Wheel-grinding data into two regions, namely, Kick's and Rittinger's. The idea of using machine grinding to determine the comminution properties of materials is indeed unique. The following cautions come to mind, however, regarding applicability of machine grinding data to comminution: 1—Grinding gives uniform particle size, whereas comminution gives a variety of particle sizes in the same process. The fact that grinding gives uniform particle size is not necessarily an advantage because in comminution the overall energy under actual comminution is desired and comminution invariably results in the production of a variety of particle sizes. 2—In grinding, a small particle is ground off a comparatively large surface. In comminution small bodies are broken down to smaller bodies. This makes it difficult to establish a concept of reduction ratio in machine grinding. 3—The mechanics of machine grinding involve direct shearing action under very high strain and comparatively high compression at the shear zone, whereas: comminution involves direct dynamic compression and surface friction with comparatively little strain and shear. Consequently the mechanics of machine grinding appear to be different from those involved in comminution. Hence one might arrive at erroneous con- clusions when comminution characteristics are eval-uated from machine grinding results. It is noticed also that functions other 'than Eq. 16 which do not involve the concept of direct proportionality of useful energy input to new surface area created (Eq. 2 and particularly Eq. 12) may be derived to fit the, data of curve No. 2. One such relationship may be u = ct-", where c is a positive constant and n is a positive constant less than unity. This, of course, is made possible because data of a very small range. of particle size are being fitted by the curves of No. 2 and the hereby suggested relationship. A sound comminution theory should be applicable to a relatively large range of particle size. George B. Clark (Department of Mining Engineering, University of Illinois)—While the experimental work of Walker and Shawin this article is of intrinsic value in revealing certain fundamental aspects of machine grinding, milling, and related processes and in adding to the store of information concerning the comminution of solid materials by this particular process, it appears doubtful that the results of their research can be employed to verify either Kick's or Rittinger's theories. Both these laws were originally developed and proposed on the basis of very simple, idealized hypotheses. The creation of parallel idealized physical laboratory conditions which would be required for either their proof or disproof appear to be well beyond the scope of human ingenuity, at least at present. One great weakness of the imputed verification is that the spread of the points plotted on the graphs is not sufficient to permit accurate 'curve fitting. The range of particle sizes included in the belt and wheel grinding is not extensive enough to show any general trends, particularly for the horizontal portion of the curves, said to represent Kick's laws. That the milling; grinding, and turning data obtained by Walker and Shaw for both metals and minerals happen to comply with. certain interpretations of these two theories under certain specialized conditions

Jan 1, 1955

By H. H. Johnson, Eric W. Johnson

A newly developed ac technique was used to measure the electrical-resistivity changes associated with both cyclic stressing and subsequent annealing of high-purity and OFHC copper. The early stage of push-pull fatigue was explored at 293° and 4.2°K, with stresses chosen for an expected fatigue life of 2 to 8 X 105 cycles. For high-purity copper, fatigue at 293°K was accompanied by an initial increase in resistivity. After about 5000 stress cycles, no further increase was observed. Annealing studies showed that the resisticity increment could be accounted for solely in terms of an increased dislocation density, to about 2 x 1010 disl pev sq cm. Fov 42°K fatigue, however, the resistivity increased continually, with no evidence of saturation, as approximately (No. of stress cycles)1/4. This is intevpreted to result from both dislocation multiplication and vacancy production; estimated vacancy concentrations are 10-4 to 10-9. The continuous resistivity increase was inhibited by interspersed annealing treatments at 293°K, which also raised the level of the stress-strain curve. These effects are attributed to annealing of vacancies into dislocation loops. In contrast, OFHC copper fatigued at 4.2°K showed saturation of electrical vesistivity after only a few hundred cycles, and it appeared that vacancies annealed out completely between 77° and 293°K. MaNY observations suggest that both dislocation multiplication and point-defect production are important aspects of fatigue deformation. An increase in dislocation density with number of stress cycles has been demonstrated or implied by several experimental techniques, including optical metallography with lithium fluoride,' electron microscopy with copper,2 thermal conductivity of Cu-Zn alloys,3 and peak-stress measurements during cycling at constant plastic strain amplitude.4,5 At low amplitudes and/or stresses saturation of fatigue hardening and dislocation density occurs early in the expected fatigue life,4-6 frequently by a few hundred cycles. The evidence for point-defect production is somewhat less extensive, but it is nonetheless persuasive. Rosenberg7 reported briefly that, for equal stresses, copper fatigued at liquid-hydrogen temperature displays an increase in electrical resistance some ten times that which accompanies unidirectional stressing. Further, the extra resistance saturates after a few hundred stress cycles, and does not anneal significantly until a temperature of about 170°K is attained.' Point-defect production during fatigue is also suggested by 1) the softening during cyclic stressing of initially strain-hardened polycrystal-line copper9, 2) the strong temperature dependence of the yield strength of fatigue-hardened mono- and polycrystalline copper,579"0 and 3) the influence of intermediate annealing upon slip-band formation in copper fatigued at 90°K.8 It is evident that characterization of the fatigued state requires a knowledge of both point-defect and dislocation densities. For this purpose electrical-resistivity measurements are useful, but they are difficult to perform because of geometric limitations. Push-pull fatigue is necessary to obtain a macroscopic ally uniform deformation over the specimen cross section; however, the specimen must then have a low slenderness ratio to avoid plastic buckling, while the standard dc resistivity technique requires a very slender specimen for

Jan 1, 1965

By G. R. Love, M. L. Picklesirner

THE use of color adds a new beauty, power, and versatility to metallography. This has been amply demonstrated in a number of public exhibits and on the walls of corporate, government, and university metallographic laboratories around the world. Indeed, in a number of cases, the color not only is of esthetic value but is scientifically essential to the competent examination of particular samples and systems. Optical strain analysis,' determination of true grain size in U-A1 alloys: phase identification in Nb-base alloys,3 analysis of transformation rates in heat-treated Nb-Zr alloys,4 measurement of solidification segregation in cast Nb-Zr alloys,' study of the intermediate phases in Nb/Sn diffusion couples,6 investigation of the oxidation kinetics at various surface orientations in single crystals,7'8 and a number of other research efforts9'10 would have been vastly more difficult without the extra clarity and distinction introduced by color—either the colors resulting from particular polarized light techniques or the interference colors obtained by oxidation. It is unfortunate that the beauty of colored micro-structures cannot be shared more widely, but the economics of publishing a technical magazine apparently prohibits color plates except under extraordinary circumstances. It is doubly unfortunate that no convenient, general method exists for communicating the information available in colored microstructures to the scientific community. True, in some instances the color changes observed are dramatic enough that direct black and white photography is adequate. In photoelastic stress analysis, several orders of interference fringes may be produced and it is frequently desirable to suppress the color effects (use monochromatic light) to simplify interpretation. On the other hand, relatively minute color variations may be readily detectable by eye, be of considerable assistance in interpreting a structure, and yet be enormously difficult to reduce to an unambiguous black and white print. In order to illustrate a possible compromise or solution to the above problems, we wish to show three black and white photographs of the same region of an Nb/Sn diffusion couple whose interpretation depends heavily upon use of color techniques. These micro-structures were obtained from a section through a rod consisting of commercial-purity niobium tubing filled with 99.995 pct Sn (melt-filled in 10"6 Torr vacuum). The composite rod, measuring 500 mm long, was bent into a hairpin shape and inserted into water-cooled copper grips in a vacuum high-temperature furnace. The rod was outgassed for 2 hr at a furnace temperature of 800°C and was further heated by self-resistance using a 2.2-kva ac power supply. The rod was raised to 1910°C over a 4+-hr period, held for 15 min, slow-cooled to 1500°C over a -hr period, and free-cooled to room temperature (all temperatures were measured with W5Re/W26Re thermocouple). Throughout the heat treatment the ambient pressure was kept below 8 x lo-' Torr. Metallographic preparation of the sample was completely conventional except that it was necessary to extend the grinding steps to remove damage in the brittle NbsSn phase introduced by sectioning. No satisfactory chemical or electrochemical etch has been found for these diffusion couples; of those which have been tried, any that attack the niobium-rich phases at all attack the tin-rich phases disastrously. However, the final polishing steps did produce a slight relief effect and this, coupled with anodizing, yielded excellent clarity in the microstructures for direct observation. The anodizing voltage was chosen to give maximum change in color per unit change in composition. In this case, indeed normally, this maximum sensitivity occurred in the blue-to-red color range. The pure niobium tube wall anodized to a relatively bright blue

Jan 1, 1967

By Stephen G. Wright

Jan 1, 1985

By L. H. Schwartz, S. K. Lahiri, M. E. Fine, D. Chandra

WHILE the yield stress of solution treated Fe-Cu alloys increases rapidly with aging, a precipitate has only been directly observed in overaged samples.'-" This precipitate is essentially pure fcc copper, the E phase. Hornbogen2 suggested that the initial hardening is due to clustering of copper atoms in a bcc iron matrix. Hornbogen was not able to obtain direct confirmation for such bcc clusters by either X-ray diffraction or electron microscopy; however, he did observe analogous clustering in Fe-Au alloys7 where the scattering factor difference between iron and gold is more favorable than that for iron and copper. Fujii, Nemoto, Suto, and Monma4 recently observed diffuse electron diffraction scattering in a 2.5 pct Cu alloy aged at 500°C: for 30 hr. They suggested that part of the diffuse SCattering was due to a modulated structure of 26 to 42 wavelength parallel to the (110) matrix plane. This disappeared with further aging. However, 30 hr at 500°C is well beyond the peak strengthening in this alloy which occurred at less than I hr at 500oc.4 By transmission electron microscopy they could not distinguish between quenched samples and samples aged to maximum strength. The purpose of the present investigation was to try to obtain further confirming evidence for a precipitation stage preceding the formation of the fcc E phase. Change in Young's modulus was selected for study be- EXPERIMENTAL PROCEDURE The Fe-1.67 at. pct Cu alloy was supplied by the U.S. Steel Corporation in the form of a hot forged rectangular bar. The carbon and nitrogen contents of this alloy were 70 ppm and less than 10 ppm, respectively. The samples for Young's modulus measurements were made by cold swaging to & in. diam and cutting to 2 in. lengths. Tensile test samples 1 in. long were prepared by cold rolling to a thickness of 0.012 in. and then machining to gage dimensions of 0.5 by 0.012 in. For Mijssbauer studies, foils 1 mil thick were prepared by cold rolling. During fabrication the alloy was given intermediate anneals at 845OC followed by quenching. The specimens after preparation were solution treated at 1000°C (y field) or 845°C (a field) for 1 to 2 and 5 to 6 hr, respectively, in a dynamic vacuum of about 2 x lom6 torr. The tensile and modulus specimens were drop-quenched into iced brine through an aluminum foil which vacuum-sealed the bottom of the furnace tube. The MOssbauer foils were drop-quenched into helium gas cooled by passing through N2 (liq) in a copper coil. The grain diameter of the modulus and tensile specimens was between 0.025 and 0.035 mm. The samples were aged from 400" to 500°C in a dynamic vacuum of 2 x 10-6 torr and cooled by pulling into a water-cooled portion of the vacuum system. The dynamic Young's modulus was measured at room temperature using electrostatic excitation and detection of longitudinal vibrations.' Neglecting any length change during the aging, (this is expected to be comparatively small), the fractional change of Young's modulus (?Et)/Eav, is equal to twice the fractional change of the resonant frequency (?ft)/fav . ?ft =ft —fo where fo and ft are the resonant frequencies of a specimen before aging and after aging to time t. The measured f's, approximately 51,000 cps, were corrected to 25°C for any variation in the ambient temperature. The tensile tests reported were carried out at room temperature in an Instron with a 1000 lb full scale load cell. The flow stress reported herein corresponds to a strain of 0.002. The Massbauer spectra were taken in a constant acceleration model AM-1 NSEC spectrometer. The

Jan 1, 1970

By Nicholas J. Grant, David S. Bloom

An investigation of the Cr-Ni system has revealed that there exists a eutectoid transformation at about 1180°C. 'The transformation in chromium implied by the eutectoid reaction was detected at about 100°C below its melting point. Associated with the eutectoid transformation, a metastable transition structure has been found. THE Cr-Ni phase diagram is shown in current literature to be a simple eutectic system in which the high chromium end of the diagram is incompletely determined, Fig. 1. The last investigation of this system was undertaken in 1936.' Because of limitations in metal purity, especially of chromium, and temperature measuring techniques, the diagram should be accepted with some reservations, as was indicated by Hansen.V or examwle.-, the wresence of the compound Cr²Ni, with a tetragonal structure," remains unverified and incompatible with the simple eutectic diagram. The work reported here began because of discrepancies that appeared in experimental studies in the binary alloys Cr-Ni and in the ternary system Cr-Mo-Ni. The existing binary Cr-Ni diagram failed to provide a complete explanation of observations made by microscope, X-ray, and thermal analyses. Experimental Methods The materials employed were of a higher degree of purity than were available to previous investigators. The Mond nickel used had a nominal purity of 99.87 pct, while the electrolytic chromium analyzed 99.03 pct with the major impurity being 0.5 to 0.7 pct oxygen with some iron. All alloys were melted in a vacuum furnace to remove dissolved gases, sufficient carbon was added to the charge to combine with all the oxygen as CO. Final analysis determined the carbon as about 0.02 pct and the oxygen around 0.06 pct or slightly more. Stabilized zirconia crucibles and thermocouple protection tips were used throughout and contributed no detectable impurity to the melts, as long as the oxygen in the chromium was kept low. Heats averaged about 250 g, which permitted about 2 in. of the thermocouple protection tips to be submerged. The temperature drop across the thermocouple protection tip was determined to be about 3°C, a minor source of error. The alloys, after removal from the vacuum furnace, were placed in a furnace operating in a purified argon atmosphere for the thermal analyses. An- nealed wolfram-molybdenum thermocouples provided the primary means of temperature determination, though a Pt-Pt-10 pct Rh couple was employed for a check when possible. A sensitive, high-speed Leeds and Northrup Speedomax recording potentiometer indicated the thermocouple output. X-ray diffraction patterns were obtained primarily on a Norelco unit, which permitted diffraction angles only up to 45" (28 = 90"). In general, either rotated or stationary solid samples were used, because it later evolved that many samples were susceptible to transformation resulting from the cold working involved in pulverizing. It was also noted that rotating a sample sometimes suppressed weak lines, so, usually, samples were not rotated. Later a high temperature camera was adapted for use at temperatures up to 1400 °C on the Norelco unit utilizing both solid and powdered samples. Unless otherwise noted, all X-ray patterns were made with a chromium tube and a vanadium filter. Further-

Jan 1, 1952

By Willard L. Cumings, Benjamin L. Miller

(Glen Summit Meeting, June, 1911.) I. THE CAMAGUEY DEPOSITS. 1. Location. THE Camaguey brown iron-ore deposit covers the top of San Felipe hill, the nearest point of which lies 14 miles NW. of the city of Camaguey. While there are several low flat-topped hills in the vicinity covered with a more or less continuous mantle of brown iron-ore, the deposit of San Felipe hill is the only one of any size and importance, and the name "San Felipe district " is proposed for the region. The deposit extends in a NW-SE. direction for a distance of about 10 miles, with an average width of 5 miles. The location is shown in Fig. 1, a sketch-map of the eastern part of Cuba. Fig. 2 is a map of the San Felipe district. 2. Description. The district is mentioned by Spencer,1 who says: "The Cubitas iron-ore fields are situated from 12 to 15 miles north of Camaguey City, in the province of Camaguey Within an area measuring roughly 10 miles east and west and 4 miles north and south, there are several flat-topped mesas rising 300 to 400 ft. above the level of an almost featureless plain which extends for many miles in all directions except toward the north." With the exception of the discrepancy in his statements as to the distance from Camaguey and the area of the hill, which is over 50 sq. miles, his description is a very good one. Kemp 2 has the following to say of ores in Carnaguey Province * Geologist, Bethlehem Steel Co. + Professor of Geology, Lehigh University. 1 Bulletin No. 540, U. S. Geological Survey, p. 324 (1908). 2 The Iron Ore Resources of the World, printed by the Eleventh International Geological Congress, vol. ii., p. 795 (1910).

Mar 1, 1911

By William T. Folwell

The Lucky Friday mine east of Mullan, Idaho, is an outstanding example of a property in the Coeur dlAlene district where a small and insignificant-appearing silver-lead-zinc vein at the surface has changed at depth into a large vein of great importance. The Lucky Friday vein has little if any surface expression and above the 1200 level the ore shoots are small and discontinuous. Between the 1200 level and 2450 level, the lowest developed level, the main ore shoot has shown remarkable improvement on each succeeding lower level, and today the mine is one of the major lead-silver producers in the Coeur d'Alene district. History: The Lucky Friday property is on the north side of the South Fork of the Coeur d'Alene River in sections 25, 26 and 35, T. 48 N., R. 5 E., Hunter mining district, Shoshone County, Idaho. This is about one mile east of the town of Mullan, which serves the eastern portion of the Coeur d'Alene district. The southern part of the property is crossed by a branch line of the Northern Pacific Ry. and by U. S. Highway 10. This highway is the principal road crossing the panhandle of Idaho and connects the district with Spokane, Wash., on the west and Missoula, Mont., on the east. The main portal and surface plant of the Lucky Friday mine is at an elevation of 3365 ft, only a short distance above the valley floor and a few hundred feet from U. S. Highway 10. so the mine is readily accessible for year-round operation. The property is comprised of six claims, known as the Lucky Friday group, owned outright by the Lucky Friday Silver-Lead Mines Co. There are four patented claims, Good Friday, Lucky Friday, Northern Light, and Lucky Friday Fraction No. 2 (Mineral Survey No. 3028), and two unpatented claims, Hunter and Creek. In addition, Lucky Friday owns an undivided one-half interest in the Hunter Creek property. which adjoins the Lucky Friday group on the north: a 90 pct interest in the mineral rights in the Jutila Ranch (160A), which adjoins the Lucky Friday group on the east; and a 60 pct interest in the Lucky Friday Extension claim group, which adjoins the Lucky Friday group on the west. The company also has a long-term mining lease on the Hunter Ranch, which adjoins the Lucky Friday group on the west. The claims of the Lucky Friday group were located between 1899 and 1906. The Lucky Friday Mines Co. was organized in 1906 and did considerable exploration work by surface trenching and shallow underground workings, only to see the property sold by the Shoshone county sheriff to satisfy labor claims totaling $2000 in 1912. Another firm, Lucky Friday Mining Co., bought the claims in 1914 and spent 12 years driving what is now known as the tunnel level crosscut. This tunnel intersected a vein previously exposed in a higher tunnel, but it was only a few inches wide. The vein was followed a short distance westerly but was so unpromising that the work was discontinued in favor of extending the main crosscut tunnel several hundred feet north. No ore was found and all work was discontinued. The property was held in such low esteem by the firm that it let taxes amounting to less than $15 a year go delinquent for nine years. Then the property lay idle for two more years until in 1938 John Sekulic, a Mullan service station operator, took a lease, with a $15,000 purchase option, on the advice of an old miner who had worked in the mine. Sekulic re-opened the tunnel level crosscut and explored the vein with an easterly drift for about 200 ft. The vein was too narrow to be of commercial value but was believed interesting enough to warrant further exploration at depth. Lacking funds to explore the vein at depth, Sekulic tried to get the district's larger operating companies to take over his lease and option. They were not interested because of the lean tunnel level showing and the fact that the property lay between the White Ledge fault on the north and Osburn fault on the south, an area which geologists always considered unworthy of exploration. Sekulic then organized the present company and assigned his lease and option to it for stock. This was in 1939. Enough stock was sold locally to finance sinking of a shaft 100 ft from the tunnel level east drift. The vein at this additional depth still was not commercial but showed some improvement. Treasury stock was offered at 5 to 10C a share

Jan 1, 1959

By J. W. Freeman, J. P. Rowe, R. F. Decker

HEAT-to-heat variations in properties of an alloy of constant nominal chemical composition have been a perplexing problem to the metallurgist. These heat-to-heat differences have been especially baffling in high-temperature metallurgy. In order to establish fundamental reasons for these heat-to-heat variations, the National Advisory Committee for Aeronautics has sponsored and financially assisted an extended research program on heat-resistant alloys at the University of Michigan. As part of the program to find the contribution of processing variables, Frey, Freeman, and white' studied effects of heat treating on nickel-base alloys and Ewing and reeman' investigated effects of hot-working practice on N155 alloy. To extend the program to the study of effects of melting practice on high-temperature properties, a 55 Ni-20 Cr-15 Co-4 Mo-3 Ti-3 pct A1 composition was selected for experimentation. The objective of this program was to establish the melting-practice variables which influenced the hot-working characteristics and creep-rupture properties and, at the same time, establish the metallurgical mechanisms for the effects. During the course of the investigation of practices using vacuum melting, it became increasingly evident through chemical analyses supplied by industrial concerns that a major variable was melt reaction with the crucible. This paper is devoted to the results of this phase of the melting-practice study. EXPERIMENTAL PROCEDURES Experimental 10-lb heats were induction melted in the University of Michigan vacuum-melting unit with the melting practices outlined in Table I. Aim analysis for the basic alloy, in wt pct, for all heats was as follows: Cr Co Mo Ti Al 20.0 15.0 4.0 3.1 3.1 Mn Si C Ni 0.12 0.12 0.08-0.15 Bal. Small amounts of boron and zirconium were added to certain heats as listed in Table I. These additions

Jan 1, 1959

By C. C. Wright, R. J. Day

Although data on the exact tonnage of recoverable coal silt are not known, the quantity produced in 1943 was estimated to be over five million tons for the anthracite region of Pennsylvania alone. Since that time the recovery of the No. 5 buckwheat size previously included in silt estimates has increased greatly thus reducing the total silt tonnage. As a compensating factor, however, the methods of recovering silt previously escaping into the rivers and streams have been markedly improved so that the net figure may not have changed materially. Comparable estimates for bituminous coal are lacking, but undoubtedly the silt represents a significant tonnage. With the trend toward increased wet cleaning of the smaller sizes of bituminous coal, it is to be expected that even greater quantities of silt will be available in the future. The raw silt from anthracite collieries usually contains a high mineral matter content, but technological developments in fine coal cleaning have been making rapid advances and it appears probable that more extensive use of these methods will be employed in the near future. Bituminous coal silt in many instances contains a similar high mineral matter content. As with anthracite silt, however, the cleaning of this material, where necessary, appears both technologically and economically feasible. With a view to upgrading the size and value of silt, considerable laboratory and pilot plant work has been conducted by a number of organizations on what is commonly known as pelletization. Actually the process is one of extrusion in which the moist silt is extruded from a die in the form of rods, which usually break into relatively short lengths—a few inches long—as they fall from the die. Fig I is a photograph of some extruded 3/8-in. diam pellets and of the anthracite silt from which they were produced This technique of producing larger sized material from fines is by no means new, having been used extensively by the industrial carbon and clay industries for years.' The application of the process to coal silt appears, however, to be relatively new. The first major program of investigation dates back only to July 1945, when a group of engineers representing the Anthracite Institute, The Pennsylvania State College and the J. F. Pritchard and Co. conducted preliminary tests on the extrusion of anthracite silt at the Floridin Co. plant at Warren, Pa. Since that time these three organiza-tions—individually, together, and in cooperation with other interested groups— have actively pursued work on various phases of the problem. Much of the early history and details of the laboratory and pilot plant work by the Anthracite Institute, has been reported by Mulcey and Eckerd.2 It is the purpose of this paper to report additional information on the process, especially with respect to the factors influencing the quality and use properties of the product, and the current develop-

Jan 1, 1949

By G. K. Manning, P. C. Rosenthal

USE of copper as an intentionally added alloy in steel and cast iron has rapidly expanded with-in the last fifteen years. It is estimated that in 1931 not more than 2000 tons of copper were so used; by 1941, however, this figure had grown to 13,000 tons. Tonnage figures during the war years have been restricted just as copper itself has been restricted, but copper-bearing cast irons and steels have played a part in the production of ordnance equipment. They are used in gun carriages, airplane landing-gear assemblies, scout cars, bulldozing equipment, army trucks, armor plate and many other instruments of war. These wartime applications have their counterpart in many peacetime applications; derricks, dredges, mine equipment, railway equipment, trucks, farm implements, automobiles, and tractors, all usually contain some parts made of copper-bearing steel or iron. An example of this is the Ford tractor which in 1940 contained over 300 lb. of copper-bearing steel castings. To this list should be added corrugated building sheet for exterior use most of which, at the present time, contains upward of 0.15 per cent copper. With the return to peacetime economy and the removal of wartime restrictions, it appears certain that copper cast irons and steels will find increasing application in civilian goods.

Jan 1, 1945

By William H. Waggaman

CURTAILMENT of the mineral industry as a whole undoubtedly will follow world peace, but the output of certain minerals should pursue a course well above the average on any curve of probable output projected beyond the trends exhibited through 1939. Without speculating on industrial conditions in the pending recomversion period, demand for fluorspar should be greater than before the war because of these factors, introduced by or resulting directly from military necessity: (1) Discovery and development of new deposits. (2) Improved technology in benefication. (3) New and expanded uses for fluorspar and its derivatives. The steel industry has been and continues to be the greatest consumer of fluorspar, and it wag largely to meet the wartime needs for steel that the domestic fluorspar industry has been expanded so greatly. Not only were the search for and development of new deposits of this mineral considered esstinal but the marginal nature of some of the,c- domestic deposits made it necessary to improve mineral dressinc and processing techniques to utilize them

Jan 1, 1945

By Wallace E. Pratt

TO SERVE their primary function of balancing supply with demand. crude-oil prices must not only return full cost plus a reasonable earning to the efficient producer but they must also offer an additional reward to stimulate exploration sufficiently to maintain adequate reserves. High prices increase the volume and efficiency of exploration; low prig e- -Idle exploration. Over the last decade average prices for crude oil have been much lower than for the proceeding ten years, and lower even than the average over the life of industry. Under these circumstances no one should be surprised to learn that over this same recent period of discovery of new oil fields has also lagged and fallen below its average level for the previous decade. Crude oil prices have been too ion to support the required activity in wildcatting.

Jan 1, 1941

By J. G. Thompson

PROJECT 8411 of the U. S. Bureau of Standards, sponsored by the Iron and Steel Division of the A.I.M.E., is an attempt to define more concisely than has been possible heretofore the accuracy and the Limits ' of usefulness of the ' various methods now in use for the determination of oxygen as it exists in ferrous materials. It originated in correspondence between John Johnston and other metallurgists, and was brought to the attention of the Iron and Steel Division of the Institute at the Annual Meeting in February, 1933. As reported in MINING AND MET,ALLURGY, Vol. 14, page 152, March, 1933, "Dr. Johnston introduced, and those present adopted, a resolution that the Iron and Steel Division of the A.I.M.E., believing that a careful comparison of the several methods now in use for the analysis of steel for nonmetallic elements such as oxygen is highly desirable, heartily endorses the proposal that the U. S. Bureau of Standards act as a clearing house " in this matter, undertaking the final preparation and allocation of identical samples to those laboratories willing to collaborate in this important question, and collate the results re- ported back to the Bureau.'"

Jan 1, 1934

By Werner Ostertag

A series of rare earth cobalt compounds of the composition RCoa (r = Ce, Pr, Nd, Sm, Gd, Tb, Dy, Ho, Ev, Tm, Lu) has been prepared. The compounds crystallize in space gvoup R3m and are isomorphous with PuNi3. Except for CeCo3 and PrCo, the series shows decreasing- values of a. and co. The relalively small parameters of CeCo, and PrCo, are explained by valencies of cerium or praseodymium which exceed the usual rare earth valency of three. The structure of the compounds is discussed as in-fillings of kagome nets in direct and staggered superposition. In the course of a systematic investigation of rare earth cobalt compounds"2 and their magnetic properties,, a series of alloys corresponding to the formula Rco3 has been prepared. The investigation of the Rco3 series was stimulated by our investigation of the yttrium cobalt system2 as well as by reports in the literature: Smith and Hansen4 reported the structure of YcO3 and Van vucht5 that of GdCo3; ceco3,6 Gdco3,7 and DyCo3 7 have been found to be single-phase during phase diagram studies. It was the purpose of this work to report crystallographic data on the entire Rco3 series and to interpret the structure of these compounds on the basis of general principles as discussed by Frank and Kasper.8 At the time this work was terminated, it was learned that a similar investigation has been carried out independently by Bertaut, Lemaire, and schweizer.9 Except for CeCo3 (ao = 4.952, co = 24.73') and NdCo3 (a0 = 5.067, co = 24.76') data of this work are in satisfactory agreement with their investigation. EXPERIMENTAL TECHNIQUES A series of samples having the composition Rc03 was prepared from stoichiometric amounts of the rare

Jan 1, 1968

By J. Gordon Parr, A. J. Goldak

OgdEN et al.1 and Bumps et al.2 suggested that the solubility of aluminum in a titanium extended to 30 pct.* Sagcl,3 Clark and Terry,4 Anderko et al.,5 Ence and Margolin6 and Saulnier and croutzelles,7 subsequently proposed the existence of an intermetallic compound in the region of 25 pct Al. Although Anderko et al.5 suggested that the structure of this phase, Ti3Al, was of the DO,, (Ni3Sn) type, their conclusion was based only upon the results of a powder photograph that included reflections from ? = 0 to ?= 27° (CuK),some of which were reported to be indistinct. Ence and Margolin,6 referring to a 25 pct alloy (but without indicating whether the figure referred to weight or atomic pct) stated: "The structure of Ti2Al is isomorphous with Ti3Sn DO19, as pointed out by Pietrokowsky". But the point was not proven, because Ence and Margolin did not report values of calculated intensities of Ti2Al with the DO,, structure. In fact, the observed intensities they reported are in poor agreement with the values we calculate for DO19 (see Table I). Saulnier and croutzelle7 concluded, on the basis of electron micrography and microdiffraction studies, that the structure of the 25 pct A1 alloy was ordered hexagonal. Our purpose has been to unequivocally determine the Ti3Al structure. Alloys containing 25 pct Al were prepared from iodide titanium and spectrographic standard aluminum by levitation melting. The levitation chamber was evacuated to 10-6 mm Hg before filling with 99.999 + pct A. After casting, the alloy was chilled to liquid air temperature and crushed to -200 mesh in a percussion mortar. The powder, wrapped in molybdenum foil, was annealed (by induction heating) at 1000 "C for 2 hr in the argon atmosphere of the levitation chamber. No sublimate was seen on the foil or elsewhere, and therefore the assumption is

Jan 1, 1962