Search Documents

By W. C. Merrill, P. G. Nahin, A. Grenall, R. S. Crog

A progress report of an experimental investigation into the role of clay in reservoir performance is presented. The Paper gives some of the reasons for considering clay as a significant component and outlines the objectives of a broad field of stud) which it is intended to pursue. Descriptions of the analytical methods used are given; these include X-ray diffraction. elec tron miscroscopy, thin section petrography, infrared spec-troscopy, and cation exchange analysis. A suite of the more important clay minerals has been assembled and characterized l~y these methods for use as standards in core analysis. From the data obtained it appears that although no one method of analysis is diagnostic for all of the clay minerals the infrared technique shows considerable promise in this direction. For the present, one or more supplementary methods should be used to confirm the clay mineral identifications. The methods of analysis are applied to field cores taken from repesentative and widely differing strata especially as regards their susceptibility to damage by fresh water. well.; completed in the stevens and Gatchell zones in San Joaquin valley are I,articularly clear-cut examples of this behavior with stevens zone wells being more adversely affected by fresh water. cores from these zones have been studied and are discussed. It appears that differences in this behavior can be ascribed to differences in the nature of the contained clays. The value of the infrarecl spectra of the clay fractions in establishing the identity of the predominant clay minerals is given particular emphasis. INTRODUCTION It is a challenge to the technical resources of the petroleum industry that when the economic limit of production is reached, from 40 to 70 per cent of the oil in California reservoirs remains unproduced even by use of the best presently known methods of recovery. The magnitude of this abandoned volume of oil can be appreciated when it is considered that to 1950 in excess of 8 billion bbll has been produced from California reservoirs with estimated economically recoverable reserves in known fields and pools totaling nearly 4 billion bbl.24 If for every barrel of oil produced there is at least another barrel still in place, it is evident that the revenue obtained from the recovery of only a .few per cent of this volume would repay the cost of the required research manyfold. From well completion experience. production behavior, and a growing body of laboratory data it now appears certain that the mineral composition of a producing stratum has an important bearing on the productivity and ultimate yield. In addition to the organic component and water, the cores con,ist of gravel, sand. silt, and clay" in diverse variety of (a, composition and (b) texture. It is the composite effect of these two factors which is probably responsible in large measure for the way in which the oil flows to the well. The role of the clay and fine-size accessory minerals is not clear but there is a growing opinion, based on their physical and chemical properties, that it is a significant one. of particular importance are the prime facts: 1. The silt and clay fractions of the reservoir matrix possess the highest surface area per gram, and 2. The silt and especially the clay fractions are the most chemically reactive of the inorganic constituents present. Only within the last few years has the knowledge of clay mineralogy and the techniques of identifying the clay minerals reached such a stage as to enable reliable inquiry into the composition of argillaceous sediments.2,8,10,11,12,16,26 It is the purpox of this and succeeding papers to add to the fund of information on the role which these materials play in the production of petroleum from California formations by correlating their presence and associated properties with observed reservoir behavior. In the present paper attention is directed to their possible influence on damage by fresh water. OBJECTIVES The attack on this problem divides naturally into two broad phases: 1. Determination of the nature of the clays and their relationships to the other mineral components, and 2. Determination of the physico-chemical relationships between the clays and the interstitial fluids. In the work described in this paper the emphasis has been on phase 1, which stems logically from the necessity of identifying and understanding the materials to be dealt with in Phase 2. Based on the authors' present opinion that not all of the minerals which occur in oil-bearing formation are of equal importance in their effects on the flow and recovery of oil, it was decided to focus attention first upon the clay minerals content and then. later perhaps. work into the field of the normally larger size non-clay minerals and fractions. The

Jan 1, 1951

By S. Shapiro, G. Krauss

We will reply to Dr. Pitsch's discussion by 1) presenting in greater detail the single surface trace analysis which we performed on the reversed austenite plates in a single parent plate of martensite of known orientation, 2) relating the results of our analysis to the conclusions which Dr. Pitsch makes on the basis of our data, and 3) examining the validity of our selection of twenty-nine individual traces from the over 200 austenite plates which were observed in a surface of this single martensite plate. Fig. 7 shows a standard (001) projection of the martensite plate from which the austenite-martensite interface traces were taken. The traces are plotted on the projection as the small solid circles, and the great circles corresponding to the loci of plane normals which could contain each trace or could intersect the surface plane along the measured directions are also plotted. It can be seen that these great circles intersect at a point which corresponds to the normal of the surface plane on which the traces were observed. Also rate which occurred only at particularly low heating rates, see Figs. 1 and 3 in the paper.2 Since in this case the interpretation of Jana and Wayman is plausible and since we have no alternative to this interpretation, we would like to state only that the existence of a diffusion-controlled reversal at low temperatures seems to be not yet proved beyond any doubt. The author wishes to thank Professor G. Krauss for making available his manuscript prior to publication. It is also a pleasure to acknowledge the lively written discussions, which the author has had with Professors G. Krauss and C. M. Wayman prior to this communication. The financial support of the Deutsche For-schungsgemeinschaft for the work on which this communication is based is also gratefully acknowledged. plotted within small dotted circles which represent a i3 deg scatter in each of the twenty-four unit stereo-graphic triangles are our A and B poles7 and the pole P determined by Kessler and itsch.' The data presented in Fig. 7 permit a direct association of the measured traces and the various proposed habit plane poles for the reversed austenite plates in the martensite crystal. If the sample measurements do in fact

Jan 1, 1969

(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 February: Paul S. King, Wilmington, Del. William Kelly, Vulcan, Mich. A. Del Mar, South Pasadena, Cal. F. H. Armstrong, Vulcan. Mich. T. D. Babbitt, Nampa, Idaho. Reginald E. More, Toronto, Canada. H. L. Williams, Newtonville, Mass. Tom M. Owen, Broken Hill, Australia. F. W. Bacorn, Pittsburg, Pa. Percy E. Barbour, Candor, N. C. Huntington. Adams, Mexico, D. F. Karl Nibecker, Youngstown, Ohio. Clifton B. Johnson, New. York, N. Y. G. A. Reinhardt, Youngstown, Ohio. W. Spencer Hutchinson, Boston, Mass. Herbert B. Cox, Boston, Mass. F. Louis Grammer, Leesburg, Va. E. C. Pechin, Buchanan, Va. H. C. H. Carpenter, London, England.

Jan 3, 1914

By D. Mizer, J. B. Clark

In a recent investigation of the entire magnesium-yttrium phase diagram, Gibson and Carlsonl report the maximum solid solubility of yttrium in magnesium as 8.0 wt pct Y at 1050°F (565°C). However, independent studies of the precipitation in magnesium-yttrium alloys, 2 conducted prior to the publication of the above phase diagram, indicated a greater solid solubility of yttrium in magnesium. Accordingly, the magnesium-rich region of the diagram was re-investigated to determine more accurately the liqui-dus, solidus, and solvus of the magnesium solid solution in this system. Metallography and thermal analysis were chosen as the best corroboratory methods for accurately determining this region of the diagram. A magnesium-yttrium master alloy was prepared from yttrium of 99.9 pct purity and singly sublimed magnesium of 99.9 pct purity. Subsequently, the twelve magnesium-yttrium alloys shown in Fig. 1 were prepared using standard alloying procedures for magnesium. Metallographic samples of the alloys were heat treated under an SO, atmosphere in an electric furnace capable of control within ±3oF of the desired temperature. Alloy samples for the metallographic determination of the solvus, and for the precipitation studies were solution treated at 1000° F for 16 hr. Subsequent aging times for the solvus determination varied from a minimum of 6 hr for the higher temperatures up to 816 hr for lower temperatures. Periods of 30 min at temperature were used to generate liquation for the metallographic placement of the solidus and eutectic horizontal. The liquidus and the eutectic horizontal were determined by thermal analysis. Simple time-temper- ature heating and cooling curves were obtained from 10-g alloy samples heated and cooled in a well-insulated electric furnace. An Iron-Constantan thermocouple was placed in direct contact with the sample. The thermocouple did not contaminate the alloy sample since metallographic examination showed that the alloy melt did not wet or attack the thermocouple. The heating and cooling rates were approximately 5 to 8OF per min. The standard metallographic procedures for magnesium were used in polishing and etching the magnesium-yttrium alloys studied. Glycol etchant* was etchant was used to reveal precipitate in the solvus determination. The redetermined magnesium-rich region of the magnesium-yttrium diagram is shown in Fig. 1. The

Jan 1, 1962

By L. R. Duncan, O. M. Wicken

Magnesium, the eighth most abundant element in the earth's crust, is found widely distributed in a variety of minerals. Among the more commercially important ones are magnesite (MgCO3), brucite (Mg[OH]2), dolomite (CaMg[C03]2), and the salts magnesium sulfate and chloride often found in natural brines. Among other commercially important magnesium-containing minerals are olivine ([MgFe]2Si04), talc (H2Mg3[Si03]4), and serpentine (H4Mg3Si2O9). These are valuable because of desirable characteristics given them by the magnesium content and its placement in the particular crystal structure. These minerals are the raw materials for a host of products including magnesium metal and several grades of magnesia or magnesia-containing materials for refractories, fluxes, fillers, insulation, cements, decolorants, fertilizers, and chemicals. Considering only those minerals valued for their magnesia or magnesium content, over 85% of the material tonnages are processed to be used as refractories. Dolomite, which is used in enormous tonnages for its physical properties in construction, has an important use as a refractory raw material in its own right and, after calcination, as a precipitant for magnesium hydroxide, which is an intermediate for the production of magnesia or magnesium metal. Magnesia from the reaction of calcined dolomite (or limestone) with seawater or magnesium-containing brines has supplanted much of the production of magnesia from mined magnesite, particularly in the United States. The best known of the minerals directly and widely exploited for magnesia content is magnesite, one of the calcite group of rhombohedral carbonates which includes calcite (CaC03), siderite (FeCO3), and rhodochrosite (MnCO3) among others. The members of this group enter into a wide range of substitutional solid solutions when the positive ions have similar radii. The radii of magnesium and iron ions are within 6% of each other; hence, magnesite and siderite form a complete series of which breunnerite (ferroan magnesite) is a well-known end member. However, the radius of calcium ion is 36% larger than that of magnesium ion, and only limited substitution exists at each end of the MgCO3-CaCO3 series. Dolomite is not a member of the calcite group, but results when calcium and magnesium ions alternate in equal number in an ordered structure among carbonate ions. The result of these relationships is that calcite and dolomite, often found intermixed with magnesite, occur commonly as identifiable crystal entities which can often be separated to a varying degree from the magnesite by various beneficiation techniques. Magnesite, when pure, contains 47.8% MgO and 52.2% CO.. The pure mineral is sometimes, but rarely, found as transparent crystals resembling calcite, but, preponderantly, magnesite contains variable amounts of the carbonates, oxides, and silicates of iron, calcium, manganese, and aluminum. Magnesite may be either crystalline or amorphous (cryptocrystalline). The crystalline form has a hardness of 3.5 to 4.0. The color may range from white to black with shades of yellow, blue, red, or gray. The color is not a fundamentally significant indicator of purity, but in a given deposit, an experienced person can often roughly grade magnesite by assessing color and crystallinity. The crystalline form of magnesite occurs in

Jan 1, 1983

By T. Egleston

The Boston and Colorado Smelting Works are situated in the town of Black Hawk, Gilpin County, Colorado, on the Clear Creek Narrow Gauge Railway, 55 miles from Denver, in the Rocky Mountains, at an altitude of 7800 feet. It was one of the first works erected for the metallurgical treatment of gold ores, and the only one established in Colorado on a large scale which has been uniformly successful. Both gold and silver ores are treated, and gold, silver, and copper produced. The lead is not separated from the ores nor paid for, if it exists, and is entirely lost in the residues. The works were planned and built by Professor Hill, formerly Professor of Chemistry in Brown University, Providence, R. I., and is still managed by him, assisted by Mr. Richard Pearce, formerly professor in the School of Mines at Truro, England. They are very advantageously situated with regard to the ore-producing regions, having Boulder County on the north, which produces, besides ordinary gold ores, a series of tellurium minerals, such as altaite, sylvanite, and hessite, which are very rich in gold and silver. They are associated with copper and iron pyrites, blende, galena, and the carbonate and oxides of iron. Gilpin County itself produces for the most part the pyrites of iron and copper rich in gold, with a small quantity of galena and blende, which is rich in silver. In

By T. PH. D. Egleston

THE Boston and Colorado Smelting Works are situated in the town of Black Hawk, Gilpin County, Colorado, on the Clear Creek Narrow Gauge Railway, 55 miles from Denver, in the Rocky Mountains, at an altitude of 7800 feet. It was one of the first works erected for the metallurgical treatment of gold ores, and the only one established in Colorado on a large scale which has been uniformly successful. Both gold and silver ores are treated, and gold, silver, and copper produced. The lead is not separated from the ores nor paid for, if it exists, and is entirely lost in the residues. The works were planned and built by Professor Hill, formerly Professor of Chemistry in Brown University, Providence, R. I., and is still managed by him, assisted by Mr. Richard Pearce, formerly professor in the School of Mines at Truro, England. They are very advantageously situated with regard to the ore-producing regions, having Boulder County on the north, which produces, besides ordinary gold ores, a series of tellurium minerals, such as altaite, sylvanite, and hessite, which are very rich in gold and silver. They are associated with copper and iron pyrites, blende, galena, and the carbonate and oxides of iron. Gilpin County itself produces for the most part the pyrites of iron and copper rich in gold, with a small quantity of galena and blende, which is rich in silver. In * By consent of the council of the Institute, this paper was first published in London Engineering, from which the engravings are here reproduced.

Jan 1, 1876

By J. M. Lommel

DURING an investigation into the effect of heat-treatment on the creep properties of the magnesium alloy ZW1, (1 pct Zn, 0.6 pct Zr), the previously published methods of final polishing were found to be unsatisfactory. A new diamond-polishing technique has been developed to facilitate the study of fine precipitates in this and other magnesium alloys, and is described in this note. The sectioning and coarse grinding techniques are those of Fox and Hall,' and Hess and Cieorge.' Pre- liminary mechanical polishing is done with 6-µ, and 1-µ( grades of diamond compound on 'Microcloth' using a lubricant of 'Hyprez' oil. When the conventional technique is used with a 1/4- µ diamond wheel for the final polishing of magnesium alloys, scratching is likely to result from the abrasive action of the 'Microcloth' nap on the soft metal surface. This problem has been overcome by the use of a cream on the wheel in order to separate the specimen surface from the polishing cloth. To prepare this cream, a solution of 6-ml tri-ethanolamine in 75-ml water is stirred into 12.5 g stearic acid at a constant temperature of 80o to 90°C. The cream is allowed to cool, and is then 'whipped' to a smooth consistency with 100-ml 'Hyprez' oil. Before polishing, the diamond loaded 'Microcloth' is moistened with a few drops of 'Hyprez' oil, then a small amount of cream is worked into the nap. For the best results a wheel speed of 500 rpm should be used for polishing, and the specimen should be held by hand with a light pressure while being rotated in the opposite direction to the wheel. After polishing it is necessary to swab the specimen thoroughly in methylated spirits to remove residual cream and oil from the surface in order to avoid uneven etching and drying stains. Fig. 1 shows the surface finish obtained on a specimen by polishing on a 1/4- µ diamond wheel using the cream, and Figs. 2 and 3 the precipitate observed in ZW1 after polishing, and etching for two seconds in nitric acid 15 pct in ethylene glycol. This new diamond-polishing technique has made a valuable contribution to the programme of metal-lographic research on ZW1 and has become a routine laboratory practice for other low alloy content magnesium alloys.

Jan 1, 1961

By Guido Bassi

IT is known'" that secondary recrystallization occurs in copper sheet with at least 90 pct reduction after annealing at high temperatures, 700" to 1000°C. Turkalo and Turnbull4 have found recently that secondary recrystallization might occur even after annealing at such low temperatures as 500°C for a high purity, coarse-grained copper sheet. It will be shown in the following that in an electrolytic tough pitch copper wire, with a high degree of deformation, secondary recrystallization might occur at even lower temperatures. A hot-rolled rod of 9.5 mm diam (temperature at which rolling commenced was 850°C) was drawn in continuous drawing machines to 0.4 mm, corresponding to a cross-section reduction of 99.8 pct. The texture in the center of the wire (the sample for X-ray analysis was etched to 0.15 mm diam) is a mixture of the [111] and the [loo] direction, as can be seen from Fig. 1. This is in accordance with the result of Schmid and Wassermann.' After a few minutes annealing of the wire at 200 °C, there is a noticeable recrystallization of the structure with a preferred orientation in the [l00] direction at the expense of the [Ill] deformation texture, as Figs. 2 and 3 show. Farnham and OINeill" reported a similar result. The final recrystallized structure shows mainly the [loo] orientation. There is however a small amount of [111] and random orientations. If the wire is annealed at 400°C, the recrystallized structure first shows a [loo] texture, Fig. 4, but as the annealing time is increased the fine-grained structure transforms into coarse grains, Fig. 5, giving a new preferred orientation, Fig. 6. The calculations show this to correspond to the [I121 direction. Even if the annealing that gives the primary recrystallization is carried out for six weeks at 20O°C, the same secondary recrystallization texture is obtained if the annealing is continued at 400°C. Schmid and Wassermann7 found the [I121 texture, but only after annealing at 1000°C or higher. The appearance of a secondary recrystallized

Jan 1, 1952

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

C. G. McLACHLAN*-I have read this paper with considerable interest and wish to congratulate the authors on the care with which they carried out their experiments and for the detailed sizing data they have presented. 011 the other hand I do not feel that these data establish their contention that "with other factors the same, the work accomplished in a fine crushing rod mill is directly proportional to the rotating speed." My reason for making this statement is that their conclusion is based on the percentage of minus 65 mesh material produced at each of the speeds at which their tests were run. The rod mill is, however, not a fine grinding machine and therefore figures based on minus 65 mesh production are figures outside the range at which it operates to best advantage. Further, if rod mill performance is to be judged on the production of such material it should have been established that a rod mill will produce it as effectively as a ball mill. To check this last point I have gone over some of the rod and ball mill grind-ing figures for our Waite-Atnulet operation and find that the ball mill at that property produces more minus 65 mesh material per horsepower than the rod mill. Moreover, this comparison is even more favorable to the ball mill if it is limited to minus 100 mesh production. It therefore seems to me that the most satisfactory basis on which to try to com-pare the performance of the rod mill in the present case is by taking a weighted average of all the new surface produced per horsepower. W. H. Coghill3 has published data which can be applied to the sizing figures presented by the authors, and if this is done the units of new surface per horsepower produced in the Tennessee tests are as follows: Admittedly the increment of increase in new surface per horsepower shown in the foregoing figures is not great, but its trend is nevertheless definitely in favor of slower speed operation, for the conditions under which these particular tests were run. I also feel that some information regarding liner contour should have been given as I think it will be found that a mill which is equipped with liners which lift the rod load can be run at a slower speed than a mill in which the liners are comparatively smooth. J. F. MYERS and F. M. LEWIS (authors' reply)—The position taken by Mr. McLachlan is to be respected even though we are all aware of the faults of surface considerations. As he points out. the increment of increase is very small. It is so small in fact that for all practical purposes it does not conflict with the conclusions of the paper. The authors appreciate Mr. McLachlan's comprehensive study of the data.

Jan 1, 1950

The following is an incomplete list of members and guests who called at Institute headquarters during the period Sept. 10, 1919, to Oct. 10, 1919. L. D. Anderson, Salt Lake City, Utah. P. S. Matthews, Newark, N. J. Ray J. Barber, New York City. A. Poole Maynard, Atlanta, Georgia. L. A. Barton, Major U. S. Engineers. L. J. Mayreis, Jamshedpur, India. J. A. Battle, Chicago, 111. Benj. L. Miller, Bethlehem, Pa. R. W. Bissell, New York City. Geo. D. Morgan, Bartlesville, Okla. Gilman E. Brown, Shanghai, China. A. C. Munroe, El Paso, Texas. Stanley Brown, Chuquicamata, Chile, Paul I. Norton, Jr., Columbus, Ohio. S. A. Walter G. Perkins, Stanford University, Norman Carmichael, Clifton, Arizona. Cal. Richard H. Catlett, Newark, N. J. Fred S. Porter, Seattle, Wash. Roderic Crandall Charles E. Prior, Cherry Creek, Nevada John J. Croston, Atlanta, Georgia. G. M. Richards I. N. Dally, Seattle, Wash. Gilbert Rigg, Melbourne, Australia. A. Faison Dixon, New York City. Pierre H. Sauvajol, Paris, France. Walter Dobbins, Springfield, Ill. Carl Scholz, Chicago, Ill. Foss E. Douglass, Rancagua, Chile. Ellsworth H. Shriver, Marysville, Ohio. H. S. Emlaw, Grand Haven, Mich. Harvey B. Small, Magangue, Colombia. R. S. Everet, Barre, Mass. Henry B. Smith, New Britain, Coma. H. W. Gipp, Melbourne, Australia. J. T. Smoody, Cornwall, Pa. F. A. Glass, Brainerd, Minn. S.. J. Speak, London, England. C. D. Grier, New York City. D. R. Thomas, New York City. James L. Head, Rancagua, Chile. Kirby Thomas, New York City. Geo. B. Holderer, New York City. R. M. F. Townsend, Washington, D. C. W. Spencer Hutchinson, Boston, Mass. Carl J. Trauerman, Helena, Mont. Henry Jequier, Paris, France. A. C. Veatch, London, Eng. L. W. Kemp, Chuquicamata, Chile. Myron R. Walker, Pittsburg, Pa. Herbert S. Kohlberg, El Paso, Texas. Curtis C. Webb, New York City. H. M. LaFollette, La Follette, Tenn. James Wilding, San Francisco, Cal. Richard Lamb, New York City. S. H. Zimmerman, New York City.

Jan 11, 1919

By A. W. Schlechten, R. F. Doelling

Parkes' process crusts were vacuum distilled using a shortened Pidgeon retort. Zinc was effectively removed below 800°C and recovered as a zinc sheet easily stripped from the furnace liner. Lead dasdistillationazinc required about 950°C and the resulting lead condensate tillationtended to stick to the thin metal liner. Final purity of residue is limited only by nonvolatile metals such as copper. THE successful commercial application of vacuum distillation for the removal of zinc from lead, as described by W. T. Isbell,' raises the question of whether or not a similar method can be used for other metal separations. Preliminary laboratory experiments on the vacuum distillation of Parkes' crusts by one of the authors' gave such encouraging results that it was decided to make a series of tests with large scale equipment to determine the results that might be expected in plant operation. The pilot-plant test results are reported in this paper. The great advantages of vacuum dezincing are its simplicity, the relatively low temperature of operation, and the fact that the zinc is recovered in the metallic state ready for use again in the desilveriza-tion of lead bullion. These same advantages and others would be realized from the vacuum distillation of the zinc-lead-silver crusts made in the Parkes' process. Zinc readily will distill over at temperatures of 800" to 900 °C as contrasted with the 1200°C or more used in the Faber du Faur furnace. Furthermore, the recovery of zinc as metal is practically perfect since there is no loss by oxidation or fuming. If the vacuum distillation is continued and hastened by raising the temperature to around 1000°C, the lead will distill over at an appreciable rate and deposit in a warmer zone of the condenser. This lead will contain a small amount of silver, but it can be returned to the desilverizing kettles and there is not the chance of loss that there is in disposing of the rich litharge from cupelling. The lower temperatures required will mean a saving of fuel and less wear on the equipment. One further point is that the vacuum distillation could be run on a small scale practically continuously, so as to avoid the accumulation of large amounts of silver-rich material and the need of assembling a large crew for special cupellation runs. It should be pointed out here that the final purity of the silver residue will depend on the copper or iron content of the crusts, as these and other metals with low vapor pressure will not be eliminated. The idea of treating the silver-zinc-lead crusts from the desilverization of lead bullion by vacuum distillation is not a new one, but such experiments have not been reported, as far as can be determined. In 1912, T. Turner presented a paper3 before the Institute of Metals on the vacuum distillation of brass, and a member of the audience suggested that he try his method on Parkes' crusts. In 1935, W. J. Kroll, noted for his discovery of debismuthiz-ing lead by calcium additions, published a paper' on vacuum distillation of metals and pointed out possible applications in the lead industry. Principles of Separation The successful separation of two or more metals by distillation depends upon an appreciable difference in the effective vapor pressures of the metals in the alloy to be treated. The vapor pressures of the common metals have been determined with considerable accuracy; for example, at 800°C the vapor pressures of the individual metals which are of particular interest in this paper are about .as follows: Zn, 241 mm; Pb, 0.0553 mm; and Ag, 0.0000276 mm. Unfortunately,, data are not available on the activities of the components in the ternary system Zn-Pb-Ag, but it can be estimated that on the basis of the vapor pressures of the individual metals a good separation can be made by distillation. The preliminary laboratory tests previously mentioned' supported this assumption. The pilot-plant size vacuum distilling furnace is shown in Fig. 1. It consisted of an abbreviated Pidgeon retort, 5 ft long with an ID of 8 in., heated by six silicon carbide elements placed symmetrically

Jan 1, 1952

By B. H. Kear

Clustering of slip bands in different systems has been observed in both ordered and disordered Cu3Au crystals compressed in the <110> orientation. Certain features of the slip band patterns are explained in terms of reactions between dislocations with Burgers vectors at 120 deg; in a few rare cases, the slip band evidence suggests that the Products of such reactions form diffuse tilt boundaries between the differently slipped regions of the crystal, similar to the known behavior of ionic crystals, but not nearly so well defined. WHEN crystals with orientations favorable for multiple slip undergo plastic deformation, slip may occur in different systems in localized regions, so that clusters of slip bands are developed. This phenomenon has been observed in fee1-4 metals and also in ionic crystals having the sodium chloride structure.5-8 In the ionic crystals, the boundaries formed between the differently slipped regions of the crystal assume characteristic orientations and are associated with macroscopic tilts that are plainly visible on the sides of the crystal. Recently, this interesting feature was explained in terms of the formation of diffuse low-angle boundaries as a result of interactions between families of glide dislocations in the different systems meeting in the boundaries.9 This paper describes an attempt to obtain similar evidence for boundary formation in an fee crystal. The alloy Cu3Au was chosen for the present study simply because this material is currently being used in a general study of differences in deformation behavior of the ordered and disordered phases of this alloy, which will be described elsewhere. EXPERIMENTAL PROCEDURE The two specially oriented compression specimens used in the present study were prepared from a melt-grown single crystal by careful cutting, grinding and polishing. The finished specimens were about 6 mm by 2 mm in cross section by 6 mm tall, with their ends parallel to (101) and sides parallel to (111) and (121); the broad faces of the specimens were made parallel to (711). Both specimens were annealed in an evacuated quartz tube at 850oC for several hours, slowly cooled to 500°c, and then quenched into water in order to obtain the disordered state for the alloy. One of the specimens was partially ordered (with S- 0.8) by reannealing at 350oC for 100 hr. After these annealing treatments, both of the specimens were electropolished. 10 Finally, the specimens were compressed in the [loll orientation and their stress-strain curves were recorded. The deformation was carried out in increments of a few percent strain. At each stage in the deformation the specimens were unloaded, removed from the compression jig, and examined optically for slip bands. Before reloading, the specimens were repolished, so that the observed slip band patterns were characteristic of a particular stage in the deformation. EXPERIMENTAL RESULTS Fig. 1 show!; the stress-strain curves for the ordered and disordered specimens and also indicates the stages 1, 2, and 3 where the deformation was interrupted for examination of slip bands. The curves show marked differences in flow stress and in work hardening rate in the two specimens, as observed by previous workers.11,12 Also, it was found, in agreemement with the observations of Taoka and Sakata,&apos;3 that the plastically deformed disordered alloy showed the characteristic coarse slip bands of alloys, whereas the ordered alloy exhibited a fine slip band structure similar to that of pure metals. Slip Band Observations. In what follows, the description of the slip band patterns, with accom-

Jan 1, 1962

By Charles Stein

The effects of several different prior treatments an the creep behavior of 99.9995 pct aluminum at 260°C and 1000 psi canstant stress are compared with annealed specimens. Quenching from 538oC, irradiation with 2 mev electrons, and tension-compression room temperature fatigue damage were used to change the substructure of the specimens prior to their creep testing. The quenched and the irradiated specimens showed a larger primary and transient stage contribution to the creep curve than those specimens which were only annealed prim to creep testing. The specimen receiving prior fatigue damage at room temperature showed no first stage or transient creep when tested under identical conditions as the above specimens and had an average creep rate seven orders of magnitude lower than that of either the annealed, the quenched or the irradiated creep specimens. In a previous electron transmission microscopy investigationl of the substructure developed during the creep of pure aluminum at 0.57 Tm, it was noted that a large concentration of vacancy loops and dislocation loops were present in and near the subboundaries while the interior of the subgrains contained few of these defects and had a low dislocation density, see Fig. 1. Yim and Grant2 and Hazlett3 have shown that the presence in nickel of a substructure developed by prior cold work effectively reduces the primary and transient contributions to the creep curve. Hultgren,4 McLean,5 Gervais, Norton, and Grant,6 Chang and Grant,7 and others have shown the same effect with the higher stacking fault energy material, aluminum. However, the specific defect responsible for the change in the creep behavior developed by the prior cold work was not established. Specifically, what effectively interfered with dislocation motion in these materials at elevated temperatures? Was it jogs on dislocations produced by their interaction with other dislocations or with vacancy or dipole loops, see Fig. 1, or did the subgrain walls determine the mean free path for glissile dislocations? This would be a realistic possibility only if subgrain boundaries are effective barriers to dislocation motion. The ability of a subgrain boundary to act effectively against glissile dislocations depends on the number and the arrangement of dislocations in the subboundary,8 which in turn is a function of the creep strain.&apos; This paper compares the creep rate of specimens possessing a large vacancy concentration to that of annealed specimens and with specimens having a stable subboundary wall containing Lomer locks produced by prior fatigue damage. EXPERIMENTAL PROCEDURE Vacancy Loops. Aluminum creep specimens, 99.9995 pct pure, were machined from zone refined rod to a 2-in. gage length and a cross-sectional area of 0.025 in. These specimens were annealed at 538oC, 1000°F, for 10 min and quenched into ice water. They were then reheated to the creep test temperature of 260°C, 500°F, and held at this temperature for 18 min to al-low for vacancy condensation and loop formation. The specimens were subsequently creep tested at 1000 psi constant stress at 260°C. The temperature along the gage length was monitored by three Pt-Pt, 13 pct Rh thermocouples, two embedded in the upper and lower shoulders of the specimen and one attached to the mid-point of the gage length- The temperature gradient was held to ± l°C or less throughout the Creep test. Elongations were measured by two LVDT&apos;s &apos;connected in an averaging &apos;On-figuration, with quartz extension arms placed against the specimen at the extremes of the 2-in. gage length. i K 3J?--&apos; * *H - >^> - &apos; ^L r 77 . *y J OJL, J Fig. 1—Transmission electron micrograph of pure aluminum strained 8.2 pct at 260°C and 1000 psi constant stress. Note the presence of numerous loops near the light dislocation tangle

Jan 1, 1970

By Lawrence H. Van Vlack, Otta K. Riegger

Periclase-type oxides were examined microscopically after being exposed to siliceous liquids. The rate of grain growth was found to be inversely proportional to the grain diameter. Grain growth proceeds more rapidly at higher temperatures, but is retarded by increasing liquid contents. aMag-nesiowiistites with higher MgO contents grow less rapidly than those with higher FeO contents. The growth rate is reduced by the presence of a second solid phase. The silica-containing liquid penetrates as a film between the individual magnesiowus tite grains. This is independent of time, temperature, amount of liquid, or the MgO/ Fe0 ratio. When present, olivine and spinel-type phases can provide a solid-to-solid &apos;&apos;bridge" between magnesioustite grains. THIS paper presents the results of a study of the microstructures of periclase type oxides in the presence of a silicate liquid. The purpose was to learn more about the effect of service factors such as 1) time, 2) temperature, and 3) liquid content upon A) grain growth, and B) liquid location among the solid grains. This study was prompted by the fact that periclase refractories are known to have very little solid-to-solid contact when the phases which are present are limited to periclase and liquid. Such a micro-structure gains industrial significance because it permits fracture during service when stresses are applied at high temperatures. The details of ceramic microstructures have not received extensive attention. This is in contrast to the extensive attention given to a) the phase relationships pertaining to refractory compositions, and b) the details of the microstructures of comparable metallic materials. A brief review will be made of the pertinent phase relationships and microstructural considerations in general, as well as of refractory compositions. a) Phase Relationships. This investigation was limited to those compositions in which (Mg, Fe)O was the solid phase. MgO and FeO form a complete series of solid solutions. Pure MgO has the name of periclase. The related FeO structure is called wustite. Both have the NaC1-type structure: however, wustite possesses a cation deficiency so that the true composition is Fe<10 even in the presence of metallic iron. The phase relationships involving solid (Mg, Fe)O and a silicate liquid are shown in Fig. 1. In this case. the liquid is saturated with (Mg, Fe)o. There-fore its SiOz content is below that encountered in orthosilicate liquids. As a consequence the liquid phase specie:; are primarily the following ions: and 0-&apos; plus occasional Fe+ ions. Two features are of importance: a) the liquid contains relatively small species and b) the liquid contains large quantities of the same species as the solid. viz., Fig. 2 shows the system, FeO-SiOz, which will be used in some of the discussions that follow. This diagram is the right side, vertical section of Fig. 1. Here, as pre\iously, the composition at the FeO end of the diagram is nonstoichiometric, varying from Feo.950 when the liquid oxide is in contact with the solid iron, to about Fe 0, when the solid oxide is in equilibrium with an atmosphere of equal proportions of CO and C02 at the solidus temperature. The Fe/O ratio will be maintained in wustite in the presence of SiO,. However, the FeM/Fe++ ratio in the liquid will be lower because of the effect OIF the SiO, on the activity of the FeO. With the addition of MgO to wustite, the over-all composition (IvZg, Fe)@, has a value of x lying between 0.9 and 1.0 when the COz/CO ratio is 1.0&apos;. b) Microstructures. In general, published attention to refractory microstructures has been directed toward the phase analyses that accompany compositional variations. This is illustrated by Harvey6 in his work on silica brick and by wells7 in his work on periclase brick. In each case, a series of altered zones is encountered which provides a sequence of phase associations. If due consideration is given to reaction kinetics, such an examination reveals phases that are compatible with equilibrium studies. Admittedly, however, it is often necessary to determine more complicated polycomponent systems to account for all the phases present.8 Relatively little attention has been given to microstructural geometry in ceramic materials. Certainly less attention has been given to this aspect of ceramic microstructures than to the size, shape, and distribution of the constituent phases in metals. Burke has pointed out that the grain size of oxides follows the same growth rules as for metals, viz.,

Jan 1, 1962

By M. R. Pickus

THE study of the plastic deformation and recrystallization of metals has been the subject of many investigations. In regard to the simple deformational processes, such as tension and compression, the early knowledge gained from studies of polycrystalline material has been supplemented by many significant researches on the behavior of single crystals. Unfortunately, this has not been true for more complicated deformational processes. As far back as 1927, G. I. Taylor1 wrote: It is impossible in the present state of knowledge to do more than give a possible reason why (face-centered cubic) crystals set themselves with a (110) direction in the plane of rolling, and at right angles to the direction of rolling. The explanation of why the orientation of the crystal axes round the transverse direction is what it is, must be left till the distortion of metals, and particularly single crystals of metals in the process of rolling, has been studied in greater detail. That this gap in the systematic study of deformation and recrystalliza-tion has not yet been filled was indicated by C. H. Samans,2 who wrote in 1934 that "only four investigations upon cold-rolled single crystals of any of the face-centered cubic metals have been reported in the literature." Of these four studies, only those of S. Tanaka3 and T. Sakao,4 both of whom worked with aluminum crystals, had quantitative significance. The other two, carried out by F. Wever5 and W. G. Burgers,6 were of a. qualitative nature. It is our hope that the present investigation may contribute some-thing to the knowledge necessary for a rationalization of the origin of rolling textures in terms of the known behavior of single crystals, and may add pertinent information concerning the recrystallization characteristics of deformed single crystals.

Jan 1, 1938

By Jay N. Fairbanks, Richard G. Robinson

This paper discusses a computer program and related formulas for fire fighting responses by coal mine personnel. The computer will interpret the mine air analysis, print reports, and provide relevant graphs allowing quick and accurate responses to coal mine fires.

Jan 1, 1983

THE Nominating Committee appointed at the Division meeting in October and consisting of Frank A. Herald, A. W. Peake, C. R. McCollom, Joseph Jensen, H. W. Camp, C. P. Watson, F. Julius Fohs, George Otis Smith, J. B. Umpleby, J. M. Lovejoy and A. W. Ambrose, have presented the following ticket for the year 1929: Chairman, Joseph B. Umpleby; associate chairman, A. C. Rubel; secretary-treasurer, R. Van A. Mills; vice-chairman for Economics, Warren A.. Sinshein~er; vice-chairman for Engineering Education, H. C. George; vice-chairman for Engineering Research, Harry H. Hill; vice-chairman for Production, C. P. Watson;vice-chairman for Refinery Engineering, A. D. David. For Production Engineering Charles V. Millikan. is named vicechairman, with ,Charles E. Beecher, Glenn D. Robertson and W. W. Scott as associate vice-chairmen. The Executive Committee named is to consist of Joseph B. Umpleby, chairman with A. W. Ambrose, Charles E. Beecher, A. D. David, Glenn D. Robertson, H. C. George, Harry H. Hill, John M. Lovejoy, Charles V. Millikan, R. Van A. Mills, Earl Oliver, A. W. Peake, A. C. Rubel, W. W. Scott, Warren A. Sinsheimer and .C. P. Watson, members. Ballots will be mailed to members of the Division.

Jan 1, 1928

By J. R. FINLA

THE three great war periods of recent times involving the-chief industrial, commercial, and military nations of the world have been the following: 1. Wars centering around the French Republic and Napoleon Bonaparte, .1791-1815;. involving every nation in Europe, parts of Asia Minor and *North Africa., and the United States of America. 2. Wars in Europe, Asia, and North -America beginning with the Crimean War, 1854-56, the British Empire, France, Sardinia, and Turkey against Russia; the Sepoy rebellion in India, -1857; -war of France . and Sardinia against ..Austria in Italy, .185.9; :the Taiping rebellion in China, 1861; Civil War in , America, 1861-65; French. occupation .of .M Mexico, .1863; Prussian war against :Denmark, :1864; (Prussia and Italy against Austria sand various -south German : states, 1866; :the Franco-German War, 1870.7,1.

Jan 1, 1931

By R. G. Davies

The activation energy for steady state creep above -500°C is observed to be independent of the applied stress although it varies from -67 kcal per mole at 2 at. pct Si to -100 kcal per mole at 11 at. pct Si due to changes in crystallographic order. The magnitude of the activation energy, by comparison with Fe-A1 alloys, indicates FeSi type of order in certain alloys. X-ray results confirmed the presence of FeSi type of order. It is proposed that dislocation climb is the rate controlling mechanism for all the alloys. It has been demonstrated that when a diffusion mechanism is the rate controlling process, the formation of a superlattice in brass,1 Fe3A1,2 Ni3Fe,3-5 and Feco6 1) increases the creep resistance, and 2) increases the activation energy for steady state creep. Furthermore, a study of creep in Fe-15 to 20 at. pct A1 alloys7 has revealed that as the alloy composition approaches the long-range order field, there is an increase in the activation energy for steady state creep which is thought to be due to an increase in short range order. Fe-A1 and Fe-Si alloys are similar in that they both form the DO3 superlattice in which aluminum or silicon atoms have only iron atoms as first and second nearest neighbors. There are, however, two important differences between the alloy systems: 1) The superlattice formation at -350°C commences at -10 at. pct si8 as compared to -20 at. pct Al,9 and 2) Fe-A1 alloys form a FeAl (B2 type) super-lattice where aluminum atoms have all iron first nearest neighbors even at 22 at. pct Al, but so far no similar FeSi superlattice has been observed. With the similarity between Fe-A1 and Fe-Si alloys in mind, alloys of iron with 2 to 11 at. pct Si were examined for variations with composition of the activation energy for steady state creep and of creep strength. The temperature range of greatest interest was above 1/2 TM (TM is the absolute melting temperature) where it is usually observed that diffusion is the rate controlling process. A subsidiary X-ray investigation of the Fe-Si system was undertaken in an attempt to define the position of the order-disorder boundary as a function of cooling rate. EXPERIMENTAL DETAILS a) Creep. Specimens whose gage length was 1.5 in. and with a cross-section 0.04 by 0.08 in. were strained in tension by a lever-arm arrangement, and the load was adjusted between each creep test to maintain constant stress. The apparatus and mode of operation have been fully described in a previous publication.7 As each test produced a creep strain of 0.25 pct, the variation in stress during the test was negligible. Creep strain was measured at the end of one of the alloy steel grips by a displacement transducer with the out-of-balance potential being recorded on a variable speed recorder. The full-scale deflection of the recorder could be varied in steps to give limits of sensitivity of between 0.1 and 0.001 pct creep strain. The alloys, Table I, were made available by the Metallurgical Department, National Physical Laboratory (N.P.L.), england,10 and by the Research Department, General Electric Co. (G.E.), Schenectady, N.Y. They were hot worked at -850°C, warm worked at 550° to 650°C, and recrystallized in vacuum at -750°C to give a grain diameter of -0.1 mm. All the alloys had a very low impurity content; those from the N.P.L., for which a complete analysis is available,&apos;&apos; show carbon less than 0.026 pct, manganese less than 0.006 pct, and oxygen plus nitrogen less than 0.0024 pct. b) X-ray Procedure. A General Electric XRD-5 X-ray set with a focussing lithium fluoride mono-chromator in the diffracted beam, and a pulse height analyzer to eliminate harmonic wavelengths of the cobalt radiation, was used to investigate the structure of several very fine grained (grain diameter <.01 mm) Fe-Si alloys after the following heat treatments: 1) Quenched from 700°C, 2) slow cooled from 650°C (-40°C per hr), and 3) very slowly cooled from 400° to 100°C (10°C per hr with a 24 hr anneal every 100°C). The method of obtaining the diffraction pattern over the range of 20 from 15 to 45 deg was to count for at least 100 sec every l/3 deg with a slit subtending 1 deg in 20 at the focus; the probable counting error was less than 2 pct.

Jan 1, 1963