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By F. E. Lathe, L. Hodnett

This paper summarizes extensive data supplied by 40 copper converter plants in 18 countries, and includes a partial analysis and comments on the effect of converter slag composition and temperature on the fomzation and elimination of magnetite and the life of basic and neutral refractories. APRELIMINARY draft of this paper, including data from 26 companies which had submitted replies to a questionnaire, was presented at the Annual Meeting of the AIME held in New York in February, 1956. Publication was delayed in the expectation that additional replies would be received, and justification for the subsequent delay may be found in the fact that the present revised paper contains data from 40 converter plants situated in 18 different countries. The suggestion that a questionnaire be sent to the major copper and copper-nickel plants outside the U.S.S.R. and associated countries arose at the Los Angeles Annual Meeting in February, 1953, where several papers dealing with converter construction and operation were presented. In private discussions which followed, a group of metallurgists and refractories engineers raised the question why practices varied so much at different plants. Why did magnesite brick give superior service to chrome-magnesite in some plants but chrome-magnesite prove superior in others? Would metallurgical studies point the way to the development of still better refractories? Could magnetite formation be prevented in converter slags and reverber-atory furnace mattes? If this was feasible, why was a heavy circulating load of magnetite tolerated, when, in all probability, it increased copper losses in the reverberatory slags and, in some cases, made it necessary to shut down the furnaces periodically to clean out the accumulated magnetite? Was the sole purpose of coating brick with magnetite that of

Jan 1, 1959

The International Mining Convention held in Nelson, B; C., May 17 , to 19, was attended by nearly 500 delegates, of whom about 100 were from Spokane, 150 from the Slocan district, and the others from different points in Canada and the United States. Arrangements were in charge of the Nelson, Slocan and Eastern British Columbia Mining Men's Club, under the direction of Secretary Fred A. Starkey, assisted by the City of Nelson, Associated Boards of Trade of Eastern British Columbia and Nelson Board of Trade. The Columbia Section of the American Institute of Mining Engineers; cooperating with the Western Branch of the Canadian Mining Institute, provided the technical program, under the management of Secretary E. Jacobs, of Victoria, and Secretary L. K. Armstrong, of Spokane. Three technical sessions were held, at which the following were read: Difficulties of the Electrolytic Zinc Process, by Thomas French. Sketch of the Geology and Ore Deposits of Nelson and Kootenay Region, by Arthur Lake's. Advantages of Local Organization of National Societies, by W. H. Linney. Review of Kootenay Mining, by Bruce White. Milling of Partially Oxidized Ores, by S. S. Fowler.

Jan 7, 1917

(Members are urged to send in for this column any notes of interest concerning themselves or their fellow-members.) Members and guests who registered at Institute headquarters during the period May 10 to June 10: Rene de Sallier, New York, N. Y. Karl Koelle, San Luis Potosi, Mexico. H. S. Chamberlain, Chattanooga, Tenn. W. A. Wilson, Salt Lake City, Utah. F. R. Pretyman, Oyster Bay, N. Y. P. E. Barbour, Candor, N. C. R. Eustice, South Australia. R. C. Blanchard, London, England. F. C. Darby, South Australia. S. K. Tong, Shanghai, China. Grant H. Tod, Livermore, Cal. W. T. Burns, Great Falls, Mont. J. Murray Clark, Toronto, Canada. F. W. Bacorn, Butte, Mont. J. H. Adams, Birmingham, Ala. H. B. Pulsifer, Chicago, 111. A. Faison Dixon, Encontrador, Venezuela. Dwight E. Woodbridge, Duluth, Minn. C. W. Merrill, San Francisco, Cal. Heinrich Ries, Ithaca, N. Y. Francis Church Lincoln, Boston, Mass. H. L. Slosson, San Francisco, Cal. Frank R. Corwin has severed his connection with the Arizona Copper Co., Clifton, Ariz., and is now shift superintendent at the smelting plant of the Copper Queen Consolidated Mining Co.. Douglas. Ariz.

Jan 7, 1914

By J. C. Swartz

New measurements of graphite and cementite solubilities in ferrite have been obtained to resolve disagreements among previous data. To measure graphite solubility, specimens of iron were equilibrated with rarious carburizing atmospheres at temperatures be-twee~z 480" and 1435°C. The carbon activity of each atmosphere relative to graphite was taken from published data. After quenching from each equilibration treatment the concentration of carbon (typically 10 pprn by wt) was determined from the height of the Snoek peak in the internal friction spectrum. A few inclividual analyses by combustion support the reszdts of Smith on the solubility of graphite near the eutectoid temperature. Combination of these combustion and internal friction analyses determines In a, (at 0.01 wt pct) = 24,000/RT - 12.72, where a, is the activtity relative to graphite in ferrite at fixed cornposition. The same specimens were used to determine the solubility of self-stressed cementite precipitates. The results indicate solubilities of 6.3, 23.2, and 68 pprn carbon by wt at respectively 400°, 500". and 600°C. The once large discrepancy between the cementite solubility determined by internal frictiori and that calculated from flee energy data has been almost completely resolved. A recent study1 (hereafter designated I) on the solubility of cementite in a iron did not fully resolve the disagreement among previous data. The remaining disagreement is illustrated by the phase diagram in Fig. L The data of I are represented by the line labeled "stress-free" cementite. They determine a heat of solution of cementite of (14.8 * 0.2) kcal per mole which contrasts with the (20 * 1) kcal per mole derived from Smith's graphite solubility2 and the formation energy of cementite.3 Toward resolving this disagreement we have obtained new data on the solubilities of graphite and cementite. METHODS As in I the Snoek peak in the internal friction spectrum was used to measure the concentration of carbon dissolved in ferrite. This method relies on the relation C=kQ-1 [1] in which C is the concentration of dissolved carbon, Q-I is the Snoek peak height, and k is a proportionality factor which is a function of the peak temperature, polycrystalline texture, and other parameters characteristic of the ferrite lattice. To determine true heats of solution via Eq. [1], it is necessary to establish that k is independent of the temperature from which the specimen is quenched. Some evidence on this point is contained in a separate report.* Additional evidence is shown by the data points in Fig. 1. These represent the Snoek peaks of two specimens carburized to about 10 ppm C, copper plated, and quenched first from 888º then from 588°C. The copper plate was removed before each Snoek peak measurement. These data show that there is no detectable dependence of k on quenching temperature. The solubility of graphite was determined by repeatedly carburizing various specimens of iron wire with gas mixtures of known carbon activity relative to graphite. To cover a wide temperature range within the a phase boundaries it is desirable to use as low a carbon concentration as is compatible with reasonable precision. With the present internal friction apparatus the best compromise of these desires is a concentration near 10 wt ppm. The dashed line in Fig. 1 was used to approximate the activity of carbon* for

Jan 1, 1970

By T. J. Koppenaal, M. E. Fine

A yield point effect attributed to short-range ordevi?g (SRO) occurs in Cu base Al. At at 296°K varies with heat treatment, decreasing as the annealing ternperature is raised .from 433Oto 598°K. Davies aid Cahn' observed a corresponding decrease in SRO. (523 °K anneal, measured at 77°K) is approximateZy proportional to the variations of A7 with strain rate and testing temperature are also Consistent with the idea that is associated with SRO. A preliminary investigation of the tensile properties of a Cu-Al single crystals showed the presence of a rather strong yield-point effect (drop in flow stress after initial yielding). The object of this research was to investigate its origin and behavior. a Cu-Al alloys are particularly interesting because diffuse X-ray scattering measurements by Davies and Cahn,' Houska and Averbach,' and Borie established the presence of short-range order. The degree of local order may be changed with heat treatment.' cottrel14 suggested that the presence of local order might result in a yield-point effect, and thus the possibility exists here for experimentally ascertaining the importance of short-range order with respect to yield points in these alloys. Since a 12 pct difference exists between the atomic sizes, elastic or Cottrell locking5 must also be considered. Further, Howie and swanne have shown that the stacking fault energy of copper is reduced by aluminum additions. The width of extended dislocations should thereby increase. hus the conditions appear attractive for Suzuki locking.' Finally, the possibility of stress-induced order at dislocations, schoeck locking,' must also be examined, EXPERIMENTAL PROCEDURE Alloys up to 14 at. pct Al were prepared by induction melting high-purity (99.999 pct) Cu and (99.996 pct) Al in a graphite boat under a dynamic vacuum of 5 X 10o mm of Hg. After homogenizing the ingots at 900°C for at least 24 hr under vacuum, they were rolled with intermediate anneals to strips 1.55 mm thick. Single crystals 10 in. long were grown by lowering strips, contained in a split graphite mold sealed in fused quartz at 5 X lo-' mm of Hg, through a single coil induction heater at a constant rate of 1/2 in. per hr. Tensile specimens 1.25 in. long were cut from the single crystal strips and reduced cross sections about 0.7 in. long and 3.0 to 3.5 mm2 in area were introduced by filing and abrading.8 To remove the worked portion about 10 pct of the cross-sectional area was removed by etching. Back-reflection Laue photographs of a filed and etched specimen were taken before and after annealing at 900°c for 24 hr. Small, well defined Laue spots were obtained with no visual difference in the two photographs. Further, specimens with and without the reduced sections began yielding at about the same stress. Hence, for our purposes, filing and abrading did not affect the structure of the specimens. Each single crystal specimen was annealed at 900° c in vacuum for at least 24 hr and furnace cooled; while cooling through the range of 250o to 200°c, the rate was about 55°C per hr. Orientations were determined by the usual back-reflection Laue

Jan 1, 1962

By L. D. Ricketts

AN older man looks back, perhaps wistfully, on a long and rather active experience, and possibly a popular and brief glimpse of some contrast between past and present may hold your attention for a few brief moments and prove useful. In the late nineties an engineer was .called on to de- sign and build two copper ore concentrating mills of 400 tons average daily capacity. There were larger mills than this at Washoe and elsewhere, but a 400 ton' mill was a large one as mills went over thirty years ago, and one might say a large mill of those days could crush a ton of copper ore in 216 seconds. In the mills I refer to steel construction and the conveying belts were introduced into the copper industry and rein- forced concrete came shortly after. Since then we in the West have ever been faced with a constantly de- creasing tenor in the grade of our copper ores and a constantly increasing demand for our product, and we have therefore been obliged to call for far larger castings and finished machines than were formerly used. The mechanical engineer has also enabled us to accomplish notable economies in power generation and distribution. Ore handling and crushing have been simplified and through the introduction of reagents to induce physical or chemical reactions, or both, our older methods have been vastly improved or even supplanted by new and better ones and our recoveries greatly improved.

Jan 1, 1929

By Peter K. Strangway

During 1973, a 20,000 net ton (18 100 metric ton) formcoke test was carried out at Inland's 26.5-foot (8.08-meter) hearth diameter on NO. 5 Blast Furnace. The formcoke briquettes were produced from Elko1 coal by FMC at their pilot plant in Kemmerer, Wyoming. The briquettes were shipped to Inland in open railroad cars and most of them were placed in an outside storage field until a sufficient amount was available for the actual blast furnace test. The test consisted of three phases: an initial four-week base period; the actual 33-day formcoke test period; and a final three-week post-test base period. During the formcoke test period, the regular coke skip loads were gradually replaced with skips of formcoke until, after a three-week period, the replacement ratio reached 80%. The furnace operated smoothly and quality hot metal was produced. The burden remained permeable and it was possible to maintain wind rates 9 of over 100,000 scfm (47 Nm3/s) without significant blast pressure increases. Dusting from the formcoke was not a problem either in the stockhouse or in the top gas. The formcoke briquettes maintained their original shape and density as they descended through the furnace. When the 80 percent replacement level had been reached, the inwall temperatures became higher than normal (about 2000 ºF (1090 ºC)) and followed an unusual steady pattern. In addition, the top gas temperature became higher than normal, and the hot metal analyses and temperatures began to fluctuate unacceptably. In general, it is felt that the high inwall temperatures were a result of channeling of the hot furnace gases along the stack walls. This channeling appears to have been promoted by a change in distribution of the burden in the top of the furnace which, undoubtedly, was caused by the increased increments of formcoke. Since it was felt to be unsafe to operate the furnace for an extended period of time with the inwall temperatures at the high level, a decision was made to remove the formcoke from the furnace. When this was done, the inwall temperatures returned to normal. Once the inwall temperatures had returned to normal, the remaining 3,800 net tons (3450 metric tons) of formcoke were used in the furnace at a nominal 40% replacement level for five continuous days. The furnace operated smoothly during this period, and the results were representative of satisfactory furnace operation with partial replacement of regular coke with formcoke. The test was successful in proving that formcoke can replace up to about 50% of the regular coke in a large furnace operating at high wind rates. However, additional work will be required to develop acceptable charging practices for using higher levels of formcoke replacement.

Jan 1, 1977

The following is an incomplete list of members and guests who called at Institute headquarters during the period Nov. 10, 1918 to Dec. 10, 1918. Arthur C. Adair, Camp Meade, Md. L. S. Mitchell, Montreal, Canada. Arthur K. Adams, Camp Humphreys, Va. T. E. Mitchell, San Francisco, Cal. Toner Antisell, Chevy Chase, Md. H. Mortimer-Lamb, Montreal, Canada. V. W. Aubel, New Castle, Pa. Edmund Newton, A. C. Black, El Paso, Tex. Paul T. Norton, Jr., Columbus Ohio. 0. F. Brinton, Baxter Spgs., Kans. Elmer W. Pehrson, San José, Cal. C. S. Corbett, Minneapolis, Minn. Joseph E. Pogue, Washington, D. C. W. M. Corse, Mansfield, Ohio. T. C. Roberts, E. Orange, N. J. G. C. Crossley, Toms River, N. J. D. R. Semmes, Richmond, Va. H. S. Emlaw, Grand Haven, Mich. H. L. Slosson, Jr., San Francisco, Cal. Rudolph Emmel, Boston, Mass. W. H. Staver, S. G. Garrett, U. S. N. R. F. A. L. Sweetser, Boston, Mass. Lt. Francis Geib, Denver, Colo. Lt. H. B. Taylor, Kansas City, Mo. Wm. E. Hubbard, Wichita Falls, Tex. Kirby Thomas, New York. Arthur Iddings, Wichita Falls, Tex. Benj. F. Tibby, Salt Lake City, U. Zay Jeffries, Cleveland, Ohio. J. L. Towne, Whitepine, Colo. S. J. Kidder, Mogollon, N. M. Chas. W. Tubby, St. Paul, Minn. Lt.-Col. W. H. Lanagan (Engrs.). A. G. Waite, Brookline, Mass. Major W. F. Lewis (Engrs.). Timothy D. Walsh, Denver, Colo. 0. M. Lewyn, Thomas Warner, Phoenix, Ariz. A. McClintock, DeKalb June., N. Y. J. P. B. Webster, London, England. Major Donald G. Miller, N. M. E. W. Westervelt, Los Angeles, Cal. C. E. LeN. Arnold, formerly with the Inspiration Cons. Copper Co. at Inspiration, Ariz., has accepted a position with the Consolidated Arizona Smelting Co. at Mayer, Ariz.

Jan 1, 1919

First Session BRASS Wednesday, A.M., Nov. 29 Co-Chairmen: CARTER S. COLE, Staff Engineer, A.S.T.M. E. A. ANDERSON, Chief of Metals Section, Research Div., New Jersey Zinc Co. (of Pa.) Second Session BRASS Wednesday, P.M., Nov. 29 Co-Chairmen: D. K. CRAMPTON, Director of Research, Chase Brass and Copper Co., Inc. A. W. TRACY, Metallurgist, The American Brass Co. Dinner and Technical Session Wednesday Evening, Nov. 29 Toastmaster: N. L. MOCHEL, Manager Metallurgical Engineering, Westinghouse Electric Corp. Talk on "How Do Things Look Today and For the Future" RALPH KELLY, President, Baldwin Locomotive Works Technical Paper on Stress-Corrosion Cracking E. H. Dix, JR., Assistant Director of Research and Chief Metallurgist, Aluminum Company of America Third Session BRASS Thursday, A.M., Nov. 30 Co-Chairmen: W. B. PRICE, Director of Research, Scovill Manufacturing Co. A. L. JAMIESON, Associate Metallurgist, Frankford Arsenal First Session LIGHT METALS Thursday, P.M., Nov. 30 Co-Chairmen: L. L. WYMAN, Metallurgist, General Electric Co. M. A. HUNTER, Professor of Metallurgical Engineering and Head, Dept. of Metallurgical Engineering, Rensselaer Polytechnic Institute Second Session LIGHT METALS Thursday Evening, Nov. 30 Co-Chairmen: R. T. WOOD, Chief Metallurgist, American Magnesium Corp. J. D. HANAWALT, Director, Metallurgical Dept., Dow Chemical Co. First Session STEEL Friday A.M., Dec. I Co-Chairmen: H. S. RAWDON, Chief, Division of Metallurgy, National Bureau of Standards A. L. FEILD, Director of Research, Rustless Iron and Steel Corp. First Session MISCELLANEOUS METALS Friday P.M., Dec. I Co-Chairmen: E. A. ANDERSON, Chief of Metals Section, Research Div., New Jersey Zinc Co. (of Pa.) CARTER S. COLE, Staff Engineer, A.S.T.M.

Jan 1, 1945

By Ashok K. Sinha

During the course of an in~*estigation into the occurrence of ordered AB3 structures, the following new phases have been found —CrRh3 (AuCu3 type), CrCo3 (MgCd3 type), HfCo4 (Ths Mn23 type), and WPt, MoPh type). The composition of the TiPt3-x phase (TiNi, type) is close to Ti23Pl77. The alloy chenzistry of transition rnetal AB3 structures is rezliewed in the light of electron concentration correlations of hex-agonality recently obtained for quasi-binary alloys. The relatizte colurne contraction in the AB3 structures increases with increasing difference in volume of the conzponents. A family of ordered close-packed layered structures is formed by stacking identical layers of composition AB, in various sequences, such that the coordination is twelvefold throughout and there are no A-A contacts. Previous work' on quasi-binary AB3 alloys has led to the conclusion that the stacking sequence of the AB, structures changes with increasing radius ratio RA/RB from a purely cubic, through different mixtures of hexagonal and cubic stacking to a purely hexagonal stacking. However. for binary AB3 alloys, a correlation between the type of the crystal structure and the position of the components in the various volumns of the periodic table has been noted.2-5 It has been noted6 that this correlation appears to hold even though the radius ratio RA/RB may vary over a considerable range with the location of the components in the three long periods. Another study7" of several quasi-binary systems led to the conclusion that an increase in hexagonality of the stacking is associated with increase in the electron concentration e/a. as defined by the average per atom of the total number of electrons outside the inert gas shells. In apparent conflict with this conclusion, it is known that seven binary alloy structures isotypic with TiNi3 which is 50 pct hexagonal occur at a higher electron concentration (e/n = 8.5) than that (e/a = 8.25) for the 100 pct hexagonal MgCd3 type structure present in seven binary AB3 alloys. Table 111. In the present work, an investigation into the occurrence of binary AB3 structures in transition metal alloys was made, and a survey of binary AB3 structures is presented. EXPERIMENTAL The starting materials were pure metals of 99.9 wt pct purity. The alloys were arc-melted under partial pressure of argon and annealed in sealed silica capsules lined with molybdenum foil under argon at- mosphere. The total weight loss upon melting and subsequent annealing was always less than 1 pct and hence the alloys will be referred to by their intended (unanalyzed) compositions. Wherever the constitution permitted. the alloys were given a homogenizing treatment at 1200°C (3 days) prior to annealing. Unless otherwise stated all alloys were annealed at 900°C for 1 week and water-quenched. Sometimes the final annealing treatment was carried out on powders to accelerate the attainment of equilibrium. X-ray powder patterns were taken using a Guinier-de Wolff focusing camera (CuK, radiation) or an asymmetrical focusing camera (Co or CrK, radiation). For lattice parameter determination. internal silicon standards were employed. The intensity calculations were made using a Fortran IV program written by Jeitschko and parthe.9 RESULTS Twenty AB3 and three AB4 alloys were investigated. Table I lists the crystallographic data on some of the intermediate phases encountered in the present work. Table II contains the X-ray data for HfCo, (Th,,Mn,, type). The positional parameter, x. was assumed to be 0.378. the value for Th6Mnn2310 The X-ray pattern of ZrCo, was very similar to that of HfCo, and the previous structure determination of ZrCo, by Kuzma el al." was confirmed. Ordering in the alloy CrCo could be ascertained by the presence of only one weak super lattice line (101). the others being too weak presumably owing to the small difference in the scattering powers of chromium and cobalt. This line was observed in the X-ray pattern of powder from the massive sample annealed at 830°C (7 days) after the powder had been reannealed at 600°C (24 hr). The diffraction pattern of the powder similarly reannealed at 830°C (24 hr) contained only the lines due to a mixture of hcp and fcc Co(Crj solid solutions. Therefore, it appears reasonable to assume that O2 and/or N2 contamination which would be less likely to occur during the 600°C anneal was not responsible for the observed weak reflection. Also. this reflection cannot be identified with any of the strong lines of the neighboring s phase which is present in the Co-Cr system at higher chromium contents. The composition corresponding to the TiNi3 structure observed by Raman et al.12 in the two-phase alloy Ti,zt,, has been established in the present work as being between There was satisfactory agreement for the low-angle lines (up to d = 1.997A) between the observed diffraction pattern of TiCua and that calculated assuming the ZrAu, structure. as recently proposed by Pfeifer-et a1.I3 However. some of the superlattice lines. e.g., at d = 1.937 and 1.919A. predicted by the ZrAu, structure were not actually observed eve? though neighboring lines. at d = 1.947 and 1.986A. of comparable calculated intensity were present. The ZrAu

Jan 1, 1970

By John H. Smith, Michael B. Bever

Pure gold was deformed by wire drawing at room temperature and 78°K. After deformation at room temperature, the stored energy and the resistivity increment reached nearly constant levels at high strains, whereas the yield stress continued to increase with strain. After deformation at 78K, the stored energy, the reszstivity increment, and the yield stress were larger than after deformation at room temperature mzd increased continuously with strain. Annealing at THE stored energy and the changes in properties resulting from cold working of Au-Ag alloys by various processes have been the subject of a series of investigations in this laboratory.'-' The work reported here room temperature after deformation at 78°K did not affect the yield stress appreciably. The stored energy, resistivity increment, and Lncrease in yield stress after deformation at room te-lnperature can be explained primarily in lerrns of dislocations while point defects, as well as dislocations, contribute to the changes in these properties after deformalion at 78°K. extends this research to pure gold. The stored energy, the resistivity increment, and the tensile properties after deformation by wire drawing were measured as functions of the strain at room temperature and at 78°K. The effect of the testing temperature and the effect of intermediate annealing at room temperature before testing at 78°K on the tensile properties of gold deformed at 78°K were also investigated. wire drawing made it possible to use a large range of strains, which was desirable because previous work on the deformation of gold had been carried out mainly at relatively small strains.'-l2 Also, wire specimens

Jan 1, 1969

Professional Divisions I-Institute of Metals Division* GEORGE K ELLIOTT, Chairman GEORGE C STONE, Vice-chairman WILLIAM M CORSE, Secretary-treasurer Executive Committee D K CRAMPTON SAMUEL L HOYT R I, SUHL W K FRANK ZAY JEFFRIES A E WHITE H W GILLETT H C JENNISON R F WOOD STANISLAUS SKOWRONSKI II-Petroleum Division F JULIUS FOHS, Chairman EDWARD L ESTABROOK, Vice-chairman C P WATSON, Secretary-treasurer

Jan 1, 1923

By AUDLEY H. STOW

I. INTRODUCTION. THE general drift of the discussion as to the relative merits of pressure- and exhaust-fans has resulted, if we may judge from the prevailing practice, largely in favor of the latter. The subject has been hitherto treated, however, with special reference to highly gaseous mines, the effect of the form of ventilation upon dust-explosions having been too little considered. Even in mines containing practically no gas, dust-explosions may occur; and if, as I believe, pressure-fans are to be preferred for their effect upon dust, it may be worth while to reopen the debate, and to challenge the advisability of exhaust-ventilation under certain conditions. There are several forms of colliery-ventilation, which may be described as follows: Plain or simple pressure-ventilation, in which the fan acts as a pressure-fan, and the movement of coal is unobstructed at the surface by doors or equivalent devices in drifts or shafts, the traveling and haulage thus being in the return-current. Plain exhaust-ventilation, in which the fan acts as an exhaust-fan, the movement of coal being likewise unobstructed at the surface, and the traveling and haulage being in the intake. Obstructed pressure-ventilation, in which the movement of coal is obstructed at the surface, in order that the traveling and haulage may be in the intake. Obstructed exhaust-ventilation, in which the movement of coal is obstructed at the surface, in order that the traveling and haulage may be in the return. The apparent advantages in running a fan "pressure" during working-hours, and " exhaust" between shifts, seem to justify the recognition of this combination as a standard form of ven-

Feb 1, 1909

By E. P. Sadowski, R. J. Raudebaugh

A study of micro structural characteristics of a 30 pct Cr, 42 pct Ni, 26 pct Fe alloy has been correlated with its behavior in creep and rupture tests at 1400°, 1600°, and 1800°F. Nitrogen pickup observed at 1600" and 1800°F was associated withfissur-ing of specimens prior to fracture. IN studying the high-temperature characteristics of a nominally 30 pct Cr, 42 pct Ni, 26 pct Fe alloy certain anomalies were observed, namely: The alloy had greater stress rupture and creep strength at 1800" than at 1600° F for time periods beyond 550 hr. As placed in test, this alloy was nonmagnetic. After test, some specimens were found to be fairly magnetic. The gain observed in magnetic response was not solely a function of time and temperature of testing. This is a report of the observations and a recounting of the results of studies made in an attempt to explain the behavior of the material under investigation. MATERIAL AND PROCEDURE All test material was taken from a production size heat of an experimental alloy melted and processed using commercial practice and having the following percentage composition: C Fe Cr Ni Ti 0.05 25.83 30.13 41.59 0.41 Al Mn Si S Cu 0.42 0.75 0.45 0.011 0.34 The material was tested in two conditions, namely mill-annealed and grain-coarsened. Mill annealing, which consisted of heating to about 1900° F in a continuous furnace for about 30 min and air cooling, gave a grain size of ASTM 8 and finer. To produce the grain-coarsened condition, mill-annealed material was soaked for 2 hr at 2050°F in a laboratory furnace and air cooled. This resulted in an ASTM grain size of 4 to 5. Rupture tests were carried out at 1400, 1600, and 1800° F in accordance with ASTM procedures. In tests where only rupture life and elongation at fracture were determined, specimens of 0.252 in. diam and 1 in. gage length were used. In tests where creep curves were obtained, specimens were of 0.375 in. diam and 4 in. gage length. Several of the tests under relatively low stress were discontinued short of rupture. Three low-stress tests are still in progress at this writing. Structural changes which occurred during testing were determined from examination of the tested specimens by light microscopy and X-ray diffraction. Diffraction pattern recordings were made with a diffractometer using copper radiation on samples heavily etched in a picric-hydrochloric

Jan 1, 1960

By P. Wynblatt, J. E. Dorn

The effect of strain rate, temperature, and interstitial impurity concentration on the flow stress was investigated in a poly crystalline Fe-2 pct Mn alloy. The temperature dependence of the flow stress was found to be independent of the interstitial impurity concentration, removal of interstitials merely decreasing the atherma1 stress level. Below 160%, the large temperature dependence of the flow stress was interpreted in terms of the Dorn-Rajnak theory of the Peierls mechanism of plastic deformation. Above 160"K, some other thermally activated intrinsic meckanisln seems to be operating. The strong temperature dependence of the flow stress of bcc iron at low temperatures has been studied by numerous investigators and interpreted in terms of several different thermally activated dislocation mechanisms. The following mechanisms have been proposed: a) interaction of dislocations with interstitial impurity atoms1 or with solute atoms in general; b) interaction of dislocations with clusters of impurity atoms;3 c) resistance to the motion of dislocations due to jogs on screw dislocations;* d) resistance to the motion of dislocations due to the Snoeck effect;' and e) interaction of dislocations with the intrinsic resistance of the bcc lattice or Peierls "hills". In previous work: it was found that the plastic behavior of polycrystalline iron containing 2 wt pct Mn (and 100 ppm C + N) is in good agreement with predictions based on the Peierls mechanismlo from 77" to 160°K whereas from 160" to about 370°K another as yet unidentified thermally activated mechanism is operative. The purpose of the present investigation was to determine the effect of interstitial impurities on the temperature dependence of the flow stress, by purifying the previously investigated alloy with respect to interstitial impurities. The investigation revealed that removal of the interstitial impurities to a level that eliminated Cottrell locking and the Portevin-LeChatelier effect (i.e., serrations in the stress-strain curve due to dynamic strain aging) affects neither the strong temperature dependence of the flow stress at low temperatures nor the general characteristics of the higher-temperature behavior. Such purification, however, lowered the athermal yield stress. I) EXPERIMENTAL PROCEDURE AND RESULTS The material used in this investigation consisted of an Fe-2 wt pct Mn alloy having the following additional elements present: 0.004 pct C, 0.006 pct N, 0.05 pct 0, 0.004 pct S, 0.003 pct P, and 0.001 pct Si. This was the same material as that studied in the previous investigation and will henceforth be referred to as the "impure material". The as received -jr by 2 in. hot-rolled bars were cold-rolled to 0.08-in. thickness, recrys-tallized under argon for 30 min at 80O0C, and further cold-rolled to 0.053-in. thickness. Flat tensile specimens 3 in. wide having a 1.625-in.-long gage section were machined from the sheet and then purified. The first stage of purification consisted of holding the specimens at 850°C for 24 hr in a stream of hydrogen saturated with water vapor at room temperature. Material prepared in this fashion will subsequently be referred to as "wet hydrogen purified material". It has been estimated that this type of treatment reduces the carbon content of iron to less than 5 ppm.' The second stage of purification consisted of holding the specimens in a closed system through which hydrogen was circulated past the heated specimens as well as a zirconium hydride getter. The specimens were held at 850°C and the getter at 800°C. The process was continued for 212 hr. The starting material for this process was wet hydrogen purified material. Material prepared in this manner will be referred to as "ZrHz purified material". The technique used was substantially the same as that described by Stein et al.' who have shown that the carbon level at the end of the process is reduced to about 5 parts per billion. The mean grain size of the three materials was found to be -60 C( for the impure material and -160p for the wet hydrogen and ZrHz purified materials. All tensile testing was carried out on an Instron Testing Machine either in controlled-temperature baths or at fixed-point baths such as boiling liquid nitrogen, and so forth. When fixed points were used the temperature was kept constant to better than *1°C whereas in all other tests the temperature variation was less than *2°C. Test of Purity. It was not possible to determine the purity achieved at each stage of the purification because the resulting level of interstitial impurities was near or below the limit of sensitivity of standard analytical techniques. It was possible, however, to obtain a qualitative measure of the extent of purification from the appearance of the stress-strain curves for the three materials. Fig. 1 shows the stress-strain curves for the three different materials tested at 300°K. It can be seen that the effect of wet hydrogen

Jan 1, 1967

By W. A. Backofen, R. L. Fleischer

Single crystal, bicrystal, and polycrystal tensile tests of aluminum at 4.2°K, 77°K, and 300°K have been used to examine the role of grain boundaries in the deformation process. Results indicate that a grain boundary may affect the extent and slope of easy glide. The stage II hardening rate, on the other hand, is independent of the presence or absence of grain boundaries. This conclusion allows the size of the region of multiple slip caused by an incompatible grain boundary to be determined. For the size of bicyystal sample used in this study, multiple slip occurs in about half of the cross section. PREVIOUS studies of the stress-strain characteristics of bicrystals of face-centered-cubic metals have been limited to aluminuml-5 at room temperature. Recent results, however, indicate that the stress-strain curves of single crystals of such metals may be separated into at least three stages6 in which different deformation processes are occurring7 provided testing is done at sufficiently low temperatures.' Since for aluminum a well-defined stage II develops only below room temperature, previous studies have not been able to relate effects of grain boundaries to all of the three stages of deformation. It is therefore to be expected that low-temperature deformation of aluminum single crystals and bicrystals should clarify the effects of grain boundaries on the different processes of deformation. EXPERIMENTAL PROCEDURE Single crystals and bicrystals were grown from the melt by the standard techniqueg with aluminum reported by Alcoa to be 99.993 pct pure. Ridges in the boat were used to guide the grain boundary during growth, assuring that the boundary would bisect the sample.10 The rate of furnace motion during growth was 1.0 cm per hr. During growth zone purification resulted, as evidenced by the ability of the first material to freeze to recrystallize at room temperature following severe deformation. Samples were approximately 4.4 X 6.6 mm in cross section and 103.5 mm in length between grips. Samples were annealed at 635" i 5°C for 40 hr and furnace cooled over a 7-hr period. They were then electropolished in a solution of 5 parts methanol to 1 part perchloric acid at a current density of 15 amp per sq dm for about 30 min at temperatures below 0°C. Tensile testing was performed at 295" (room temperature), 77" (sample in liquid nitrogen), and 4.2"K (sample in liquid helium) on the hard-type machine indicated schematically in Fig. 1. The machine con- sists basically of a tube surrounding a rod; one end of the sample is attached to each member, and the rod is pulled up the tube to extend the sample. The rod is rigidly mounted and is moved vertically by a system described by asinski." The pulling force is measured continuously by an electrical strain gage load cell, and the relative displacement of the tube and rod is also recorded continuously by a soft cantilever beam with electrical strain gages. Maximum stress and strain sensitivities were ±2g per sq mm and * 3-10-5. In all tests the strain rate was approximately 5.10-5 per sec. The thin wires in the tensile apparatus introduce softness, which may be corrected for, however, by measuring load vs displacement with the sample replaced by an elastic member. For loads greater than 15 kg the spring constant is 1.875.106 g per cm. The flexible wires also served to reduce substantially the large shearing forces which may arise in the case of grips having horizontal rigidity.'' As in any gripping system, however, bending moments will arise in the course of deformation by single slip. Engineering stress, s = (load)/(original cross-sectional area), and strain, E = (increase in length)/ (original length), are used for stress-strain curves unless otherwise indicated. Tables list resolved shear stress, T=mo and shear strain ? = dm, where m is the usual Schmid resolved shear stress factor for the primary slip system at the start of deformation. The first group of samples to be described forms an isoaxial set, all of the crystals making up the single crystals or bicrystals having the same tensile axis, the orientation of which is indicated by the cross in Fig. 2. For this orientation the primary slip plane and slip direction make angles of 45 deg with the tensile axis and the Schmid factor m has its maximum possible value of 0.5. Rotations about the tensile axis are indexed by means of an angle 0 between the small-area surface of the samples and the projection of the primary slip direction onto the cross section, as defined in Fig. 3. In single crystals, values of 0 were 0 and 90 deg, while in bicrystals 0 values were (0 deg, 180 deg), (90 deg, 270 deg), and (0 deg, 90 deg) as indicated in Fig. 4.

Jan 1, 1961

By Kidd, Robert L.

INASMUCH as galena and sphalerite flotation concentrates are being produced that contain over 95 per cent galena or sphalerite, it is not unreasonable to believe that a flotation concentrate assaying at least 80 per cent of native gold can he secured provided the gold is free. As yet, little if any fundamental information has been published concerning the flotation of free gold either alone or in the presence of sulfides. So far, we are unable to make as complete a separation of gold from sulfide minerals by flotation as is possible in, the separation of one sulfide from another by this method. An introductory study of the flotation of several free gold ores has been made in our Utah laboratories. For this study three general types of gold ores were chosen, namely: (1) Quartzite containing 0.26 oz. gold per ton in which no base metals are present; (2) sulfide ore (2.04 oz. Au; 1.31 oz. AO containing pyrite as the only sulfide present and the gold free; and (3) oxidized ore (1.10 oz. Au; 0.70 oz. Ag) from an oxidized zone of the vein from which sulfide ore (No. 2) was taken; little sulfide iron was present.

Jan 1, 1932

By Francis Foley

IN examining steel under the microscope, one is constantly confronted with structures that are difficult to interpret. Recently, in a collection of samples for exhibition purposes, the writer found apiece of open-hearth runner metal, 2 in. (50 mm.) in diameter, that had been fractured for use as a sample of cast-steel structure. On polishing and etching a section for the purpose of photographing a field to typify the microstructure of steel in the "as cast" condition, a variety of structures was found (Fig. 1) so arranged as to arouse interest at once. For a distance of about 0.065 in. (1.6 mm.) from the skin of the runner, normal ingot structure was found (Fig. 2); this was followed by a zone, about 0.215 in. (5.5 mm.) wide, of considerably lower carbon content in which occurred a most pronounced Widmannstättian structure (Fig. 3); from this point on to the center of the runner, the metal was again of normal ingot structure (Fig. 4). Representative samples taken from the metal in the three zones showed the following analysis: C Ni Cr Metal from skin 0.34 1.26 0.63 Widmannstättian zone 0.21 1.18 0.63 Metal from center 0.34 1.32 0.67

Jan 7, 1919

By J. Greenspan

The anisotropy of fracture and slip, that is, the brittleness and ductility of the beryllium single crystal, is characteristic also of po1ycrystalline beryllium in which the grains are oriented in a preferred manner. Beryllium with grain orientations resulting from hot working either unidirectionally or bidirectionally is ductile or brittle in directions given by the anisotropy and orientation of the grains. Textures developed from various hot-working sequences are given, and tensile results are correlated with textures. Not only texture, but fine grain size is necessary for obtaining high tensile elongation. Ultimate tensile strength and elongation are both correlated with grain diameter. Of particular interest is the case in which unusually high tensile elongations of 30 to 40 pct are obtained when basal planes are oriented to carry THE beryllium crystal (of nominal purity) is probably unique among metals with respect to its unusually acute anisotropy of slip and fracture. While extensive slip can occur on the system (1010) [ll20] starting at about 19,000 psi, the (0001) plane is particularly vulnerable to fracture at 4500 psi or less. Fracture occurs also on the (11zo) plane at about 26,000 psi.1"3 Further, there seems to be no other slip System which contributes significantly to

Jan 1, 1960

By Charles Luner

ALTHOUGH the kinetics of the atmospheric oxidation of tin have been studied,1-3 the kinetics in pure oxygen have not been reported. This note presents some results of the kinetics of the oxidation of tin foil in pure oxygen. The tin foil used in this investigation was 99.78 pct pure, the two major impurities being Pb (0.17 pct) and Sb (0.024 pct). The foil was degreased and air-dried prior to oxidation. The air-formed film was estimated by coulometric reduction4 of the surface oxides to be about 25A. The samples, which were in strip form and had a total geometric surface area of about 300 sq cm, were first evacuated at room temperature in an oxidation bulb to 1 X 10 -5 mm Hg and subsequently degassed for 1 hr at the temperature of the experiment. Spectroscopically pure oxygen was then introduced into the bulb. The rates of oxidation were measured by following the rate of pressure change due to oxygen consumption in a closed system, the volume of which was sufficiently large so that the pressure change during an experiment was 10 to 15 per cent of the total pressure. An oil-mercury manometer,5 with a sensitivity of 3 X x mm Hg (which corresponds approximately to 5 X 10 -7 gm of oxygen) was used to measure the pressure change. The oxidation bulb was heated by an oil-bath and controlled to within -10.3 C. The reproducibility of the rates was good, as determined by the coincidence of rates at 190oC for duplicate experiments. Fig. 1 shows the oxidation curves in the temperature range 168 to 211.5oC at 8 mm Hg pressure. The effect of pressure on the rate of oxidation at 190°C is also shown. The rate of oxidation was not markedly affected by changes in pressure in the range 4 to 9 mm Hg, except perhaps at the lowest pressure, 4 mm Hg, where after about 70 min there appeared to be a decline in the rate, as compared with the rate at the higher pressures. At the lower tem- perature, 168oC, and for short reaction times, it is difficult to distinguish between a linear relationship and a slight curvature in the oxidation rate. However, for longer times, there was a somewhat larger indication of curvature. The samples after oxidation were gold-colored in appearance. The oxide that was formed at 170°C was identified as a-SnO by reflection electron diffraction. This is in agreement with results obtained by other workers.6, 7 The rate data best fitted the logarithmic-oxidation rate law, w = K1n ln(1 + -t/to) [1] where w is the weight of oxygen consumed, t is the time, and K In, and to are constants. First estimates to were obtained according to the method of Taylor Thon8 and were then employed to obtain the best simuItaneous estimates of to and K In, that would fit the logarithmic expression. These estimates were found numerically, so that the residual variance could be minimized. The calculations were performed on an

Jan 1, 1961