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I TOLD you above that you should save the melted material that you extracted by smelting the ore. In substance this is copper, lead, silver, and perhaps gold, but all are like substances mixed in one body without any distinction. Now if you wish to separate these and to reduce them to their pure qualities, it is necessary to proceed with each one according to its own methods. Now in this method of separating lead in order to extract the silver and gold from the copper, it is necessary to return to the smelting and to follow one of two methods.* The first is to smelt it again with the addition of lead or lead ore, and to make it all run through the channel into the large forehearth that was made in front of the blast furnace, and, as it cools off, proceed to remove layer by layer with the fork, as I told you before and as you did the first time, until the work lead is reached. Then you assay what you have extracted and see whether it contains silver. If you consider that it has enough per hundred to justify the expense, return it again to the smelting. Continue to do this until you have extracted all the unctuousness and the work lead still remains. If it contains little or no silver, you must be satisfied with your work; otherwise return it again to smelt, always accompanying it with lead or galena and do as you did the other times until it

Jan 1, 1942

By Edwin Dudley Martin

DURING the past twelve years the iron and steel industry has made a major advance through the development of the continuous wide strip rolling mill. So far-reaching have been the results that not only has a better product been sold at a lower price but this improvement in quality has permitted manufacturers of products using steel to make important savings in the cost of fabrication. The net result has been a better product at lower cost to the consumer without reduction in either employment or of wages paid within the industry. That is why the iron and steel industry is proud of its attainment. Being a basic industry of strategic importance, such an advance in technology has had its effects on our internal economy, our standard of living, and our industrial power as a nation in both peace and wartime.

Jan 1, 1939

By W. R. Hibbard Jr., T. Michalak

THAT the amount of deformation and annealing time influences the recrystallization temperature of cold-rolled copper has been well established. Evidence that the recrystallization temperature can be affected by the deformation texture has been reported by Brick and Williamson,% ho found that copper straight-cold-rolled to 99 pct reduction to produce one deformation texture and copper cross-cold-rolled to 99 pct reduction to produce a second and different deformation texture correspondingly recrystallized at different temperatures to different textures. The purpose of the present work was to study more thoroughly the effect of the deformation texture on the recrystallization of cold-rolled copper. Experimental Procedure The copper used in this investigation was commercial OFHC copper (nominally 99.985 pct Cu) in the form of 0.500-in. plate. Qualitative spectro-graphic analysis showed only a slight trace of iron and a trace of silver. No analysis was performed to determine the exact content of the iron and silver,

Jan 1, 1958

By L. C. Weiner

For zinc single crystals, xo = 3o, a surface coating raises both the cleavage and yield strengths over a large temperature range. The "brittle temperature," associated with slip after completion of twinning, does not coincide with the point of intersection of the flow and cleavage curves, which is associated with twinning. A surface film has no effect on the brittle temperature, while it lowers the intersection temperature some 20°. For crystals, yn = 83o, a coating decreases the cleavage strength, making it temperature independent, as well as increases the brittle temperature or its equivalent, the intersection temperature, 20°. These observations are described on the basis of a dislocation-pile-up-at-a-barrier model for brittle fracture; in crystals x,, = 3o the number and distribution of twins play a vital role. IN a recent investigation on the effects of solid environments on the brittle fracture of zinc single crystals,' it was demonstrated that the presence of a surface film changes the cleavage strength of these crystals, either increasing or decreasing it, depending on the crystal orientation. An increase in cleavage strength of some 43 per cent was found for coated crystals oriented x, — 3o K = 28",* while a decrease of 48 per cent was observed with crystals X" = y» — 83". Moreover, these effects were found

Jan 1, 1959

By F. M. Lewis, J. F. Myers

The crushing of ore, as defined by Taggart, is "usually a stage process, utilizing . . . machines especially suitable for the reduction of particular sizes. . . . down to a final stage, employed for the reduction of the finest sizes. ... In contradistinction, comminution to 20-mesh or finer is called grinding. There is a twilight zone in which the product is 6, 10, or 14-mesh limiting size which is either crushing or grinding. ..." Since the data in this paper pertain to a rod-mill operation, comminuting a particular ore size of ¾ in. to a final stage, coarser than 20-mesh, the rod mill is designated as a "fine crusher machine" in this paper. The published literature discloses a wealth of data regarding a rod mill as a fine-grinding machine but relatively little as a fine-crushing operation. Typical of the latter operation is: (I) a description by F. J. Tuck2 in which a fine-crushing rod mill replaced crushing rolls and (2) a description by the present authors3 in which a fine-crushing rod mill was installed instead of a collventional fine-crushing machine. The experience of the authors is that a definite distinction must he made between the rod mill functioning as a fine crusher and as a fine-grinding machine. As a fine crushing machine it prepares relatively large amounts of ore for a subsequent fine grinding operation; as a grinding machine, it grinds relatively small amounts of ore to some predetermined finished product. Pulp Movement and Action in Mill In considering the work performed by a fine-crushing rod mill, it seems important to understand just what takes place within the mill. We were inspired to study this matter by a paper by E. W. Davis,4 which indicated that definite water classification of ore particles took place in a ball mill. However, in thinking of the rod-mill action from this point of view, we were confronted with the fact that our rod-mill discharge product showed no evidence of action by water classification. The Tennessee Copper Co. ore is relatively high in sulphides, and the gangue rock and the sulphides are of about the same hardness. In the presence of any action by classification, the coarser sizes are definitely very lean in sulphide minerals.

Jan 1, 1947

By J. F. Myers, F. M. Lewis

The crushing of ore, as defined by Taggart, is "usually a stage process, utilizing . . . machines especially suitable for the reduction of particular sizes. . . . down to a final stage, employed for the reduction of the finest sizes. ... In contradistinction, comminution to 20-mesh or finer is called grinding. There is a twilight zone in which the product is 6, 10, or 14-mesh limiting size which is either crushing or grinding. ..." Since the data in this paper pertain to a rod-mill operation, comminuting a particular ore size of ¾ in. to a final stage, coarser than 20-mesh, the rod mill is designated as a "fine crusher machine" in this paper. The published literature discloses a wealth of data regarding a rod mill as a fine-grinding machine but relatively little as a fine-crushing operation. Typical of the latter operation is: (I) a description by F. J. Tuck2 in which a fine-crushing rod mill replaced crushing rolls and (2) a description by the present authors3 in which a fine-crushing rod mill was installed instead of a collventional fine-crushing machine. The experience of the authors is that a definite distinction must he made between the rod mill functioning as a fine crusher and as a fine-grinding machine. As a fine crushing machine it prepares relatively large amounts of ore for a subsequent fine grinding operation; as a grinding machine, it grinds relatively small amounts of ore to some predetermined finished product. Pulp Movement and Action in Mill In considering the work performed by a fine-crushing rod mill, it seems important to understand just what takes place within the mill. We were inspired to study this matter by a paper by E. W. Davis,4 which indicated that definite water classification of ore particles took place in a ball mill. However, in thinking of the rod-mill action from this point of view, we were confronted with the fact that our rod-mill discharge product showed no evidence of action by water classification. The Tennessee Copper Co. ore is relatively high in sulphides, and the gangue rock and the sulphides are of about the same hardness. In the presence of any action by classification, the coarser sizes are definitely very lean in sulphide minerals.

Jan 1, 1947

By Frederick Jr. Prime

THE first catalogue of Geological Reports of the United States was prepared by Prof. O. C. Marsh, and published in the American Journal of Science and Arts for 1867, vol. xliii, second series. Since then the list has more than doubled, and it was thought that the publication of a new catalogue, brought down to date, would be useful to many of the members of the Institute of Mining Engineers. The compiler will be most thankful to have any omissions or inaccuracies in the list sent to him, to be published as a supplement in the next volume of the Transactions. Especially to have the correct title, number of pages, plates, and maps of any volume on the list to which an * is prefixed, as he has been unable to personally consult such works. A preliminary list was issued last February, which has been almost doubled by the kindness of many friends. The writer desires more especially to express the obligations he is under to the following gentlemen The Chief of Engineers, U. S. A.; Principal Dawson, Mr. G. M. Dawson, Drs. B. J. Harrington and T. Sterry Hunt, of Montreal; Mr. H. Engelmann, of La Salle, Ill.; Dr. F. V. Hayden and Prof. J. W. Powell, U. S. Department of the Interior ; Prof. E. W. Hilgard, University of California; Prof. Henry Y. Hind, Windsor, N. S.; Prof. C. H. Hitchcock, of Dartmouth College; Mr. Henry A. Holmes, State Librarian, Albany; Maj. Jed. Hotchkiss, Staunton, Va. ; Prof. W. C. Kerr, Raleigh, N. C.; Dr. J. S. Newberry, of Columbia College ; Prof. W. H. Pettee, of the University of Michigan ; Dr. Samuel H. Scudder, Prof. N. S. Shaler, and Prof. J. D. Whitney, of Harvard College ; Mr. Sanderson Smith and Prof. J. J. Stevenson, of New York ; Mr. Addison Van Name, of Yale College, and Lieut. Geo. M. Wheeler, U. S. Engineers. PHILADELPHIA, 907 Walnut Street, October 1st, 1879.

Jan 1, 1879

By O. Vartianen, R. T. Hukki

A preliminary investigation of the collecting effects of various fatty acids in tall oil has led to a conclusion that the collecting power of fatty acids used in flotation increases with increasing un- saturation of the hydrocarbon chain. Linoleic acid was found to be an excellent collector for oxide minerals. TALL oil is a mixture of fatty and resin acids extracted as byproducts in the sulphate pulp industry. In the field of flotation a well-known example of this type of product is Reagent No. 708 of the American Cyanamid Co. Its successful use as a flotation collector with many nonsulphide minerals has been described by Falconer and Crawford.' The composition of crude tall oil varies within wide limits.' " By a number of methods the crude oil may be refined to produce a variety of refined products. This investigation presents a preliminary comparative study of collecting properties of the fatty acids in tall oil. In Finnish tall oils these constituents are primarily palmitic, oleic, linoleic, and linolenic acids.:' The first is a saturated fatty acid having 15 carbon atoms in its hydrocarbon chain, plus one in the carboxyl group. The others have 17-carbon-atom chains and are unsaturated. It is of particular interest to note that palmitic, oleic, lino-leic, and linolenic acids represent increasing degrees of unsaturation with 0, 1, 2, and 3 double bonds, respectively. To test the collecting properties of the four fatty acids separately, the vacuum flotation technique described by Schuhmann and Prakash4 was used. By this method the boundary between flotation and non-flotation conditions was approximately delineated, with the use of ilmenite and several other minerals. Collector concentration and pH were the principal variables. On the basis of information obtained, actual flotation tests were run on an ilmenite-bear-ing ore in a laboratory flotation cell. Through the courtesy of P. Kajanne from the Department of Chemistry, Finland Institute of Technology, the following reagents were obtained for this investigation: 1—Palmitic acid, of Judex, had a purity of 95 pct as determined by parallel iodo-metric and spectrophotometric measurements. 2— Oleic acid, product of May and Baker Ltd., indicated purity of 98 pct. By iodometric and spectrophoto-metric determinations the oleic acid content was found to be 83.8 pct. In addition, it contained 6 pct linoleic, 1 pct linolenic, and 9.2 pct saturated fatty acids.' 3—Linoleic acid was prepared from soybean oil by low-temperature crystallization. Its linoleic acid content was 95 pct by the methods indicated above. 4—Linolenic acid was prepared from linseed oil by low temperature crystalIization. Its linolenic

Jan 1, 1954

By G. M. Ritcey, M. J. Slater, B. H. Lucas

The recovery of uranium from acid leach slurries by continuous ion exchange, or solvent extraction using sieve-plate pulse columns, is compared. Differences in processing costs are of prime concern and can be related to differences in the unit operations of the two methods, as well as the chemical and physical properties of the slurry. Parameters are defined for the operation of the solvent-in-pulp process and the design of the continuous ion exchange column. Pilot plant operating experience with both recovery systems is described, and an overall assessment of the relative costs is presented.

Jan 1, 1973

By Y. C. Liu, R. H. Richman

The effects of gel,manium and tin on the deformation and 9-e-crystallization textures of copper have been explored in detail with in the copper-rich terminal solid solutions. Addition of solute to copper produces a change in deformation texture from the copper type to the 70 :30 brass type. This transition has been measured quantitatively The types mid proportions of recrystal-lization components have been determined as a function of com-position, and correlation of recrystallization components with specific deformation components is discussed. On the basis of information available in the literature, it has been suggested that the effect of solute elements on the recrystallization texture of copper

Jan 1, 1961

By Herbert Dumont

Since 1947 Preussag AG Metal1 has used a process for fuming zinc- and lead-containing dump slags and residues from vertical retorts in a half-shaft furnace at their Hüttenwerk Harz at Oker. Contrary to the classic shaft furnace, only one side of the half-shaft furnace is fitted with tuyeres. The opposite side is a bricked slope. The upper shaft section is piped. There zinc vapor and combustion gases are burned by sucked-in air. Gases and fume enter a boiler located on the rear length of the furnace via a piped fire bridge. The gases are then cooled in an air preheater prior to dedusting in a bag filter. The furnace is charged with briquettes of metal-bearing materials, coal and pitch. The leaded zinc oxide fume is comparatively rich in both lead and zinc. The copper in the feed is recovered in low-copper matte. The slag can be discarded. The Oker plant comprises 13 furnaces of 2.9 to 4.9 m length in the tuyere area. Two other plants in Italy and Spain are processing zinc leach residues by this technique. Fuming of zinc-lead-oxide ores as well as partially roasted sulfide- zinc-lead-copper bulk concentrates will be possible.

Jan 1, 1970

By R. L. Smith, J. L. Rutherford

ALTHOUGH considerable effort has been devoted toward the determination of the mechanical properties of pure metals, it is extremely difficult to compare the results of such work. This is because of differences in method and type of test, grain size, heat treatment, and purity of material. There is very little information on the properties of most of the high melting point reactive metals with purities greater than 99.9 pct. Previous evidence concerning the tensile properties of unalloyed metals show that: body-centered-cubic metals are brittle at low temperatures; face-centered-cubic metals remain ductile; some hexagonal metals remain ductile, others become brittle. It may be that traces of impurities decrease the low temperature ductility of the body-centered-cubic lattice. This would suppose that a body-centered-cubic lattice free from impurities would exhibit nearly the same ductility as a face-centered-cubic structure. The present investigation has been an evaluation of the tensile properties of zone refined iron in order to determine whether higher purity material than that previously evaluated behaves differently. Experimental Procedure In this investigation, high purity iron was zone purified using the floating zone method.' The starting stock was obtained from two sources. The first,

Jan 1, 1958

By William L. Boyd, Eugene L. McCarthy, Laurance S. Reid

Proper control of the moisture content of natural gas is essential to reliable operation of gas transmission and distribution facilities serving northern markets. The moisture content of natural gas is usually determined by dew point measurement at the existing pressure. For any gas of constant moistrire content. the dew Point varies with the pressure. A correlation of the data of several investigators is prezented in graphical form by the authors. These data were correlated by the authors and F. M. Townsend, C. C. Tsao. M. I). Rogers. Jr.. and J. A. Porter. graduate students in chemi(.a1 engineering at the University of Oklahoma. Of articular interest are the hitherto unpublished low temperature data observed by Wickliffe Skinner. Jr., which are included in this correlation. PRESENTATION OF DATA The problem of interpreting water dew points, or saturation temperatures. of natural gas in terms of specific moisture con-tent has increased in importance during the past decade bec.arl.;e of extensive development.; in the transmission and petro-chemical phases of the natural gas industry. Virtually all gas transported to northern and eastern markets must be dehydrated to a low water vapor content to prevent hydrate formation in transmission and distribution lines and resultant interruption.; in gas deliveries. Complete dehydration is required in certain phases of tile petro-chemical industry involving low-temperature operations. It is a well-known fact that the water vapor content of pure hydrocarbon vapors and their mixtures at superatmospheric pressures cannot be predicted with accuracy by assuming validity of the ideal gas laws." Earlier interest in the general problem was concentrated on the water vapor content of pure hydrocarhons and hydrocarbon mixtures in the pressure and temperature ranges common to gas and oil producing reservoirs in order to obtain fundamental data for the improvement of production techniques and the furtherance of reservoir studies. Excellent data are published for pressures ranging from atmospheric to 10,000 psig and for temperatures ranging from 100° to 460° F4,9,10,11 and are found to be in close agreement. However, experimental data at high pressures and temperatures below 100°F are comparatively limited in scope. Experimental data in the lower temperature range have been reported by Laulhere and Briscoe.8 Deaton, et al,2,3 Hammerscllmidt,5,6 and wade," In general, the pressures employed in these investigations ranged from atmospheric to 1.000 psig while temperatures ranged from 32° to 120°F; i.e., the usual conditions encountered in gas transmission line operations, Additional data were reported by Russell, et al,12 at pressures as high as 2.000 psig and covering a rather narrow atmospheric temperature range. In 1947, Hammerschmidt published a correlation of all available data,' in which the water vapor content of gases at saturation. under high pressure and low temperature. was predicted by extrapolation. In 1948, Wickliffe Skinner. Jr.. presented data on the moisture content of a low nitrogen content gas at low temperature and at pressures ranging upward to 1.500 psia.1-3 Comparison of Skinner's experimental data with the extrapolated data of Hammerscllmidt revealed an appreciable variation in the lower temperature range. emphasizing the need for a new correlation which would rely on Skinner's data at lower temperatures. Careful scrutiny of available data suggested that presence of an appreciable quantity of nitrogen in a gas mixture may affect its saturated moisture content so that data obtained from gases with more than three per cent nitrogen were not used in this correlation. CORRELATION OF DATA Data employed in this correlation are presented in Table I. The data of Dodson and Standing.4 McKetta and Katz,9 and Olds, Sage and Lacey10 were compared and found to be in close agreement so that the data of Olds. et al, re-plotted in a more convenient form by the Humble Oil and Refining Co.,' were used for temperatures of 100°F and above. Skinner's data were used for temperatures below 40°F. Between these intermediate temperature limits, the data of Hammerschmidt.7 Wade" and extrapolated data of Olds. et al.1 were tabulated

Jan 1, 1950

By C. J. Rosa, W. C. Hagel

An attempt is made to determine the diffusion coefficients of oxygen ions in hypostoichiometric zirconium oxide. A phenomenological theory is developed for three-phase, unidirectional volume diffusion of a gaseous species from a planar source. Knowledge about oxygen diffusion in a and ß zirconium and experimentally measured rates of movements of interfaces permit the evaluation of oxygen ion diffusivi-ties in ZrO2-x. The results conform to the relationship: sq cm per sec, for the temperature range of 875" to 1050° C. DIFFUSION coefficients of oxygen ions in stoichio-metric oxides have been studied by many investigators. The obtained results not only supplement the knowledge about the lattice-defect structures of oxides and conduction mechanisms but also provide information of technological importance. Rate processes such as oxide sintering, high-temperature creep deformation, and oxidation of metals and their alloys are directly dependent on diffusion phenomena. Unfortunately, diffusion coefficients obtained from studies on stoichio-metric oxides cannot be treated without restraints when applied to oxidation kinetics, if precise evaluations of oxidation rates are desired. Oxides formed on metals are usually nonstoichiometric and exhibit nonuniform distribution of either cation or anion vacancies across their thicknesses. Debuigne and Lehr1 extended Danckwerts'2 mathematical analyses and furnished a semitheoretical treatment for evaluating oxygen diffusion coefficients in zirconium oxide in terms of weight gain measurements during oxidation of zirconium in the temperature range 400° to 850°C. Their calculations are based on theoretical partitioning3 of the total amount of oxygen between a zirconium and its oxide phase. An inherent discrepancy appears to continue throughout their calculations. The amount of oxygen confined to the oxide phase should be corrected by multiplying the calculated oxide thickness by the inverse of Pilling-Bedworth ratio, if expansion of zirconium dioxide is taken into account. The purpose of the present investigation is to provide a new semitheoretical treatment for evaluating diffusion coefficients of moving species in hypostoichiometric oxide. The analyses are relevant to unidirectional volume diffusion. Although the presented method is quite general, its applicability will be discussed in terms of kinetic measurements from oxidation of zirconium at temperatures above the a/ß transition, for reasons stated in the later part of this paper. EXPERIMENTAL Pure, 99.93 wt pct, zirconium samples of approximately 2 by 1 by 0.35 cm were exposed to oxygen for various times at four temperature levels: 875°, 950°, 1000°, and 1050°C. High-purity, better than 99.9 vol pct oxygen was passed through a cold trap and columns containing anhydrous CaSO4 to remove residual water vapor. Before exposing to oxygen at a pressure of 500 Torr, specimens were subjected to wet abrasion on 200- through 600-grit Sic papers and polished with 1—p diamond dust. Prior to oxidizing, all zirconium samples were vacuum-annealed at 10-6 mm Hg for about 15 min at the test temperature. The temperature variation across the uniform heat zone was ±2°C from the preset value. Final polishing, for phase thicknesses measurements, was performed by using 8- and 1-p diamond dust and followed by vibrator polishing with 0.05-µ ? Al2O3 solution. Measurements of phase thicknesses were made by projection on a metallographic viewing screen. Conventional powder X-ray analyses for the oxide were employed. RESULTS Fig. 1 is an example of the cross section of oxidized zirconium. Designations of phases given below this figure are the same as those used in the three-phase diffusion system represented by Fig. 5 in the following section. Zirconium oxidized for longer exposure times showed two types of oxides: white oxide at the surface and an underlaying layer of gray oxide. X-ray powder patterns of these oxides at room tern-

Jan 1, 1969

By J. R. Mihalisin

THE application of electron-microscopic techniques to the study of high-temperature alloys has met with considerable success.' This is due, in part, to the submicroscopic nature of the phases present in this type of alloy making high resolution methods necessary. Among the newer electron-microscopic techniques, the extraction replica technique' has proven to be of great value. This method allows phases to be examined in situ in the microstructure and permits their identification by means of electron diffracticn. This technique eliminates the main disadvantage in using electrolytic extraction of residues as a means of phase identification; that is, the uncertainty of relating constituents identified in the residue to what is observed microscopically. In the course of work relating microstructure to physical properties in high-temperature alloys, it was found that the formation of grain-boundary carbide phases and intragranular precipitation of an age-hardening phase greatly influence strength and ductility at high temperature. In particular, it was found that the formation of a unique type of precipitate in Nimonic "80" (a nickel-chromium-aluminum-titanium type superalloy), termed cellular or discontinuous precipitate, at grain boundaries generally results in poor ductility at high temperature. However, this mode of precipitation can be avoided by proper heat-treatment. It was assumed that this precipitate was either a carbide or age-hardening type of phase. Using various etching procedures with the extraction-replica technique, it was found to be possible to extract the carbide and age-hardening phases preferentially in this type of alloy. Previous work has shown that the age-hardening phase can be extracted from superalloys merely by

Jan 1, 1959

By John F. Allan

This paper does not pretend to advance any facts or improvements not known to many members of the Institute, but is intended merely to give a few practical hints on preliminary tests, and to call attention to a possible enlarged field for the cyanide process in the treatment of some silver-ores, which merits investigation. Broadly considered, the choice of a process for the treatment of silver-ores in Mexico is confined to the following alternatives: (1) Concentration for treatment by smelting; (2) milling and pan-amalgamation; (3) the patio and Ortega process; [4) chloridizing roast and lixiviation; (5) chloridizing roast and cyaniding; and (6) cyaniding of the crude ore. These methods of treatment may also be combined, and cyaniding or concentration, or both, may be introduced, at what-ever stage it is found to be most advantageous. The characteristics of the ore (especially its gold-content) and local conditions, such as distance from railway, cost of fuel, amount of water available, vary so much that it is impossible to make general comparisons between the different processes, either as to extraction or cost. Concentration and subsequent smelting may be made very expensive by long-distance transportation of concentrates; pan-amalgamation is undoubtedly expensive; and the patio process is barred when the ore contains appreciable amounts of gold, by reason of its poor extraction of that metal; yet there are many ores for which each of these processes is especially adapted, and the expense of treatment is compensated by the results obtained.

Jan 1, 1905

By H. R. Ogden, E. S. Bartlett, A. G. Imgram

Notched and unnotched tensile specimens of wrought and recrystallized, oxygmted and hydro-genated tantalum and columbium were tested over a range of temperatures selected to encompass the ductile-to-brittle transition. Increasing the oxygen content of tantalum and columbium increased their strength, and raised their ductility transition temperature, but did not cause a marked deterioration of notch properties below that of commercially pure material. The adverse effects of oxygen were more pronounced for recrystallized structures than for wrought material. The effects of hydrogen are complicated by strain aging or slow strain rate hydrogen embrittlement at -105°F. However, in general, hydrogen had only a minor effect an strength, but markedly increased the effective transition tem-terature and caused a deterioration of notch properties . BCC metals including the refractory metals in Groups Va and VIa (V, Cb, Ta and Cr, Mo, W) can be expected to undergo a ductile-to-brittle transition and exhibit brittle fractures at low temperatures.' Notch embrittlement is associated with this phenomenon, and can be a serious design problem. Table I compares the tensile transition behavior and notch sensitivity of commercially pure Group Va and VIa refractory metals. The Group VIa refractory metals have considerably higher transition temperatures, and become notch sensitive at higher temperatures, than do the Group Va refractory metals. In addition, the Group VIa refractory metals are sensitive to metallurgical structure. Recrystallized structures generally have higher transition temperatures than wrought material of the same composition. The relatively poor transition behavior of the recrystallized structures of these metals is generally attributed to the segregation of interstitial impurity atoms at grain boundaries. Pronounced sensitivity to structure is not evident with commercially pure Group Va refractory metals, however. Since these metals have higher solubilities for interstitial elements than do the Group VIa metals ,4 it can be expected that higher total interstitial concentrations are necessary to develop a comparable degree of grain boundary segregation and to produce a similar sensitivity of transition temperature to structure. Increasing only the concentration of interstitial atoms in solution would tend to increase the flow stress of a metal in relation to its cleavage fracture stress and thereby raise its transition temperature, but would not be expected to cause a marked sensitivity of transition temperature to structure. A research program has been conducted at the Battelle Memorial Institute to evaluate the effects of interstitial oxygen and hydrogen on the transition behavior and notch sensitivity of tantalum and columbium, and to evaluate the effects of structure on "contaminated" material. EXPERIMENTAL PROCEDURES Notched and unnotched tensile specimens of oxygenated and hydrogenated tantalum and columbium with both wrought and recrystallized structures were tested over a range of temperatures selected to encompass the ductile-to-brittle transition Oxygen levels selected for study in both tantalum and columbium were nominally 500 and 1000 ppm, whereas nominal hydrogen contents were 150 and 500 ppm in tantalum and 150 and 300 ppm in columbium. Oxygen and hydrogen additions were made directly to 6-in. lengths of 1/2-in.-diam electron beam melted wrought bar stock, in a Sieverts Apparatus. Subsequent high-temperature annealing was required for homogenization of the oxygenated material, but was not necessary in the case of hydrogenated stock. The oxygenated and hydrogenated bars were then swaged to 1/4-in.-diam rods. Tensile specimen blanks were cut from the 1/4-in.-diam rods and annealed to achieve stress-re-

Jan 1, 1963

By W. F. Carew, F. A. Crossley

IT has been reported that the Ti-8 pct A1 alloy is ductile as water quenched from 800°C but brittle as annealed at 650 °C." The present, somewhat limited, investigation was undertaken to discover the cause of the embrittlement. In order to evaluate to some extent the continuity of the embrittling phenomenon, alloys of 6, 8, and 10 pct A1 were studied. Subsequent to the completion of most of this work, Ence and Margolin reported that a Ti,A1 phase exists and that two or more unidentified compounds may exist in the Ti-A1 system.' Materials, Equipment, and Techniques The alloys were prepared using Kroll process sponge of 124 Bhn hardness. In addition, some 8 pct A1 material was made with iodide titanium. The sponge-base alloys were prepared as melts of 4 lb or more by double arc melting. The iodide Ti-8 pct A1 alloy was prepared as 200-g buttons. The alloys were forged at temperatures of 980" to 1150°C. Results of chemical analyses are given in Table I. A Baldwin-Southwark 60,000-lb capacity tensile machine, equipped with an autographic stress-strain recorder, was used for the tensile tests. Standard tensile test specimens, 0.252 in. diam, were used. Standard Charwy V-notch impact specimens were tested using a -kiehle machine. specimens were sealed in evacuated Vycor bulbs for heat treatment. Powder samples for Debye-Sherrer anal- ysis were prepared by filing and screening through 325 mesh. The —325 mesh fraction was taken in an effort to concentrate a microstructural constituent assumed to be less ductile than the a phase. The powder samples were stress relieve2 by annealing

Jan 1, 1958

By Howard A. Smith

Of late considerable experimental and theoretical interest has been shown in the rates of transformation from a single phase, usually a supercooled solid solution, into one or more phases. Such reactions may involve both diffusion and transformation of the major constituent, as in iron alloys, or it may simply involve diffusion, as in superstructure formation and in age-hardening systems. Most of the work has been confined to ferrous alloy1-9† although two investigations have been made on copper alloys10*". That such work may be of considerable practical importance has been demonstrated by Bain12, by the workers at the Kaiser Wilhelm Institut fur Eisen-for~chung'13, 14, and by the everyday use of precipitation and age-hardening principles15. Experiments in this country have generally followed Davenport and Bain's technique of rapid supercooling followed by isothermal treatment. In Germany16, 17 the work has been extended to the study of the influence of accurately controlled and measured rates of cooling. The work on steel indicates that there are two subcritical temperature ranges where reaction starts sooner after quenching and proceeds at a more rapid rate than at other temperatures. At suberitical temperatures above Ar" (temperature of martensite formation) where reaction is dependent upon atomic migration there is a period of time of which the length depends upon the alloy content and the temperature, before which no reaction has been detected. Davenport and Bain' find that different sorts of atoms in solid solution in gamma iron affect the length of this " prereaction" period differently, manganese probably being the most effective in lengthening it. It is very difficult to believe that nothing occurs within these "prereaction" regions, for if this were so there is no reason why any reaction at all should be observed. In the light of experimental facts and theoretical considerations it is certainly

Jan 1, 1935

By Howard A. Smith

Of late considerable experimental and theoretical interest has been shown in the rates of transformation from a single phase, usually a supercooled solid solution, into one or more phases. Such reactions may involve both diffusion and transformation of the major constituent, as in iron alloys, or it may simply involve diffusion, as in superstructure formation and in age-hardening systems. Most of the work has been confined to ferrous alloy1-9† although two investigations have been made on copper alloys10*". That such work may be of considerable practical importance has been demonstrated by Bain12, by the workers at the Kaiser Wilhelm Institut fur Eisen-for~chung'13, 14, and by the everyday use of precipitation and age-hardening principles15. Experiments in this country have generally followed Davenport and Bain's technique of rapid supercooling followed by isothermal treatment. In Germany16, 17 the work has been extended to the study of the influence of accurately controlled and measured rates of cooling. The work on steel indicates that there are two subcritical temperature ranges where reaction starts sooner after quenching and proceeds at a more rapid rate than at other temperatures. At suberitical temperatures above Ar" (temperature of martensite formation) where reaction is dependent upon atomic migration there is a period of time of which the length depends upon the alloy content and the temperature, before which no reaction has been detected. Davenport and Bain' find that different sorts of atoms in solid solution in gamma iron affect the length of this " prereaction" period differently, manganese probably being the most effective in lengthening it. It is very difficult to believe that nothing occurs within these "prereaction" regions, for if this were so there is no reason why any reaction at all should be observed. In the light of experimental facts and theoretical considerations it is certainly

Jan 1, 1935