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By A. A. Collins

OF widespread interest to all lead metal¬lurgists is a dross smelting process that will consistently give mattes and speiss of low lead and high copper contents. It is -a problem that has intrigued operators through the years. In the past few years, with increased amounts of copper and overcrowded metallurgical furnaces, it has been almost imperative to evolve some method. Experience at El Paso has shown that high copper-to-lead ratios can be consistently attained by use of the new soda process.* OLDER METHODS Three older methods; i.e., I. Dross plus siliceous ore and limestone, 2. Dross plus one fourth blast-furnace speiss and siliceous ore, 3. Dross plus sulphides and siliceous ore and scrap iron, do not give consistent results and the products are higher in lead and lower in copper than those produced with the soda process. Any radical changes in the blast-furnace drosses will throw any of these older methods into a tailspin. For almost ten years, El Paso used the third method, with varying results. It was noted that as the arsenic and antimony contents of the dross increased, the speiss and matte steadily increased in lead and decreased in copper. A dross containing four parts of copper to one part of arsenic was considered to be ideal. At times this balance of copper to arsenic was almost impossible to obtain, especially when handling copper Cottrell dusts, which vary so greatly in copper and arsenic. Custom smelters like El Paso, handling a great variety of dusts, concentrates and ores, are apt to have anywhere from 1 to 15 pct copper on charge, with a variable in arsenic of from 0.5 to 2 pct. With such conditions, and drosses varying from 12 to 40 pct copper, an operator using the older dross reverberatory practices would find it just about im¬possible to control the reverberatory operations and to produce a good product low in lead and high in copper. These conditions prevailed at El Paso from the year 1940 to the present. In May 1942 it, was decided to experiment with the soda process. THE SODA PROCESS After considerable work the soda method was finally evolved to the present state. It has never failed to produce a good product even under the most adverse conditions. It might be well to remember that many men of thought in the smelting industry have at one time or other suggested the removal of all copper, arsenic and antimony from the lead blast-furnace charge as an aid to better metallurgy.

Jan 1, 1947

By Chester W. Washburne

At present it is impossible to estimate closely the amount of oil obtainable from a given area of land. However, after the completion of a few properly distributed prospect wells, one can calculate the approximate yield of the sands penetrated, with a probable error of say 50 per cent. Even rough predictions of this kind are of value in large operations. Without wells upon it, one can never be absolutely certain that an area will produce any oil whatever, and one can only indulge in wild guesses of the probable productive area, before the geological structure has been carefully contoured and the top of the basal water plotted on a map. This requires wells. At times it is desirable to form an idea of the possible yield of oil in advance of drilling, as in cases where the price asked for undeveloped land seems too high, but where the probability of finding oil is furnished by neighboring development, supported by the geology. In such cases the most one can do is to make an estimate of possible maximum yield, which may of course far exceed results, and which is of use mainly in the prevention of excessive initial investment. The method is very significant in a general way, as in regions like the Bighorn Basin, Wyoming, where the productive sands in the Cretaceous shale are so few and so thin and fine that they cannot develop very great production, although the high quality of the oil probably will counterbalance this defect sufficiently to give local profit in favorable areas. Reservoir Capacity of Sands.—The porosity of a stratum is the measure of its maximum reservoir capacity for liquids and gases. The porosity may be determined experimentally and must be used in connection with the total volume of the sand.

Jan 1, 1915

By O’Brian. Daniel T.

Ore reserve determinations supporting property appraisals and economic analyses leading to investment decisions typically require many repetitive calculations. Computers have become well-accepted tools for accomplishing these computations, and are partly responsible for the development of new evaluation methods during the last decade. Excellent descriptions of manual ore reserve may be compared with current computer reserve methods1,2 in North America2 and South Africa3. A comparison indicates that computers are used in two cases: a) when a cost savings can be achieved by the simple conversion of a manual method to a computer processed equivalent, and b) when the quantity of data and ore reserve estimation purpose justifies adoption of a complex ore reserve computational method not feasible on a manual basis. Ore reserve computations essentially consist of using sample data and a mathematical method to arrive at an estimated geometry, tonnage, and grade for a mineral deposit. The mineral deposit is then subdivided, if necessary, into ore and waste components. This separation is based on economic factors which may be explicitly introduced in the computation or incorporated in a numerical cutoff grade4. Computer methods for accomplishing these tasks are presented in three papers. "The Use of Contour Surfaces as Predictive Models for Ore Values" discusses the requirements for a satisfactory value prediction model and the importance of considering auto -covariance. A weighted moving average method is described and compared to other mathematical surface development methods. In the second paper, "The Applications and Limitations of Computer Techniques in the Evaluation of Hypothermal Tin Lodes," particular problems encountered in estimating geometrically erratic economic deposits with a low valuable mineral content are documented. Economics and probabilistic concepts are introduced, allowing a comparison of risk and speculative value for a deposit. Economic considerations are integrated with ore estimation techniques in the third paper, "Method of Calculation of the Iron Ore Reserves in the Lorraine Deposit." The prediction model

Jan 1, 1969

By W. T. Nightingale

The three gas-producing "pools" discussed in this paper are in Sweet-water County, southwest Wyoming, and Moffat, County, northwest Colorado. Hiawatha, North Baxter Basin and South Baxter Basin gas fields became economically important in 1929 when a 330-mile gas line connected them with Salt Lake City, Ogden and towns en route. This development immediately focussed attention on the gas-producing fields and the efforts of the producing company to develop them in an orderly, economical manner. Several outstanding interests were acquired and working agreements made with others. Thus the interference of natural drainage areas was avoided, the pernicious practice of drilling direct

Jan 1, 1930

The following is an incomplete list of members and guests who' called at Institute headquarters during the period Mar. 10, 1918 to Apr. 10, 1918. W. Sinclair Brown, Lebong Donok, Sumatra. F. Laroque, Roodepoort, Transvaal. H. B. Catlin, Syracuse, N. Y. A. H. Means, Camp Upton. A. R. Chambers, New Glasgow, Nova Scotia. J. H. Miles, Nome, Alaska. W. M. Corse, Buffalo, N. 1 . Harvey S. Mudd, Washington, D. C. George C. Crossley, Toms River, N. J. Henry Noyes, Melbourne, Aust. F. A. Dalburg, Montoursville, Pa. C. L. Petzel, Camp Upton. Kuno Doerr, El Paso, Tex. J. L. Schueler, Peoria, I11. V. E. Edwards, Worcester, Mass. J. G. Scrugham, Reno, Nev. H. F. E. Gamm, Rutherford, N. J. Frank M. Smith, East Helena, Mont. J. W. Gerhard, St. Louis, Mo. W. G. Swart, Duluth, Minn. Julius H. Gillis, Sudbury, Ont., Canada. A. L. Sweetser, Boston, Mass. S. J. Gormly, Guayacan, Chile. W. N. Thayer, Cincinnati, Ohio. Fletcher Hamilton, San Francisco, Cal. Felix E. Wormser, Cornucopia, Ore. Dorsey A. Lyon, Washington,. D. C. John B. Arnold has opened offices at 606 Lyceum Bldg., Duluth, Minn. E. E. Barker, formerly mine superintendent with the Chile Exploration Company at Chuquicamata, Chile, has resigned his position to become superintendent of mines for the Cerro de Pasco Copper Corporation at Cerro de Pasco, Peru.

Jan 5, 1918

By Hendon R. Johnston

In the Tennessee Valley Authority's program of investigation and treatment of foundations for major structures, many chert, or flint, bodies have been encountered during the diamond-drilling operations. These chert bodies occur most frequently in the Knox dolomite and

Jan 1, 1948

By Hendon R. Johnston

In the Tennessee Valley Authority's program of investigation and treatment of foundations for major structures, many chert, or flint, bodies have been encountered during the diamond-drilling operations. These chert bodies occur most frequently in the Knox dolomite and

Jan 1, 1948

By D. Harker, W. E. Seymour

CERTAIN alloys of iron and nickel, when rolled and annealed, possess a preferred crystal orientation: (001) in the rolling plane and [loo] in the rolling direction, when recrystallized at 850" to 1050°C after approximately 98 pct cold reduction. Since the preferred orientation makes a direction of easiest magnetization coincide with the rolling direction, these alloys, especially a 50 pct iron in nickel alloy, have found wide application in the electrical industry' for choke coils and special types of transformers. The rate of the recrystallization reaction was studied at temperatures ranging from 500° to 600°C. The heat of activation for the reaction was calculated from the observed rates, and crystal orientation determinations were made before and after re-crystallization. A vacuum melted iron-nickel alloy* analyzing 49.6 pct nickel, 0.018 pct carbon, and 0.30 pct manganese was used for the experiments. The alloy was cold-rolled 98 pct into strips 1/2 in. wide by 0.002 in. thick. Specimens 1 in. long were sealed under a vacuum (approximately 10-8 mm Hg) in 1/2 in. ID pyrex glass tubes. For heat treatment these tubes were fastened to Nicrohm wires and submerged in a molten salt bath controlled to ±2°C. (The maximum measurement error was within 3°C.) The time at temperature was varied logarithmically from one sample to another, and runs were made at 500°, 525", 550" and 575°C. A molten lead bath was used for a run at 600°C which was controlled to the same accuracy. To determine the extent of recrystallization after a particular time at a given temperature, a method was used suggested by the work of Decker, Asp, and Harker.3,4 This method employs an X-ray spectrometer whereby X rays are diffracted from crystallites whose diffracting atom planes are parallel to the rolling plane of the specimen. The intensities of the diffracted rays are measured by a Geiger counter. The counter can be rotated through a range of angle, and can be motor driven through this range at a speed of 2" per min. The measured intensities are plotted vs. angle by a potentiometer recorder. In a 50 pct iron-nickel alloy it was found that only (200) reflections were obtained from the rolling plane with recrystallized material, and that only (220) reflections were obtained from the rolling plane with unrecrystallized material. No other reflections were obtained under these conditions over a range of Bragg angle of 0 to 45" using either type of specimen. As a consequence, the intensity of the (200) reflections from the rolling plane was taken to indicate the amount of recrystallized ma-terial present in a specimen, and the corresponding intensity of the (220) reflections was taken to indicate the amount of unrecrystallized material present. To insure flatness and proper alignment of the reflecting specimen in the spectrometer, the sample was laid in a slot 1/2 in. wide x 0.001 in. deep which was machined in a 3/4x2x1/2 in. steel carrier. The specimen then was taped down with cellophane tape. This steel cradle was mounted vertically in the specimen holder of the spectrometer so that the bottom edge of the carrier rested against a horizontal shoulder. Intensity data used in plotting the percent of recrystallized material vs. time at temperature were obtained by directly counting the diffracted beam of nickel filtered copper Ka radiation used throughout the work. The X-ray spectrometer was employed also in obtaining pole figure data to be used for orientation determinations. At the beginning of this investigation a transmission pole figure holder was used." As a thickness of 0.002 in. of this alloy was found to be opaque to the copper Ka radiation, it was necessary to reduce the thickness of the pole figure specimen. A cold-worked sample was etched in a 50 pct HCl solution for 5 min and was found to transmit a

Jan 1, 1951

By Persifor Frazer

COMPARATIVE columns expressing the series of rocks of the lower half of the Mesozoic age in this country and in Europe are not yet definitely established. The following represents a co-ordination of the beds in England and Germany,* with a list of materials to be worked in from this country. † * Cotta, " Geologic der Gegenwart." † Section from York to Dillsburg. Report C, 1875; Second Geological Survey of Pennsylvania.

Jan 1, 1877

Jan 1, 1920

By AIME AIME

PAST President R. C. Allen, then State Geologist of Michigan, gave George Corless his first job-tracing ?magnetic? with the dip compass in northern Wisconsin. His second job was also with a man now Past President of the Institute-"Chief" Buehler, for whom he worked at Joplin three years. Then came seven years as geologist and later as assistant manager of the Chanute Spelter Co., a subsidiary of The American Metal Co., Ltd. His entrance into the oil business was not planned. During a lull in the zinc industry in July, 1926, he stopped at Houston, after a trip to the Rio Grande Valley, and was so impressed with the city that he decided to migrate. His first job there was with the Texas Company, whose impressive building across from the Post Office caught his eye after he had mailed a letter saying that he was settling in Houston and would not be home until Christmas. Some months later, A.I.M.E. Past President Philip N. Moore learned that he was in. Houston and wrote an unsolicited recommendation that resulted in his present employment with the Humble Oil & Refining Co. Today he is superintendent of the Gulf Coast Division of its production department. The Division extends from Jackson County, Texas, to New Orleans, and includes such pools as Sugarland, Conroe, Toni Ball, Thompsons, Anahuac, and Friendswood. -

Jan 1, 1938

By F. G. McCutcheon

UNTIL about 1930, the universal practice of horizontal-retort zinc smelters in the United States, as far as the writers are aware, was to operate the retort furnaces on a 24-hr cycle; that is, the retorts were charged in the early morning of one day, and in the early morning of the following day the residues were cleaned out, the retorts recharged, and a new cycle started. During the business depression of the early thirties, zinc production fell off to the extent that zinc smelters had idle retort capacity. Rather than continue to run some of the retort furnaces on a 24-hr cycle and shut down the remainder, a few companies decided to try out a longer cycle. Although the output of zinc per retort per day is lower, the longer cycle permits a larger charge per retort and improved zinc recovery. Advantages of the longer cycle were soon evident, and the practice spread rapidly. Various lengths of cycle were used, typical examples being 28-hr, 32-hr, 36-hr, and 48-hr. The 48-hr cycle fits in best with the standard routine of smelter practice that was built up on the basis of the 24-hr cycle; that is, the retort furnace "maneuver" always comes at the same time of day, and can be performed in the cool hours of the early morning. Under some conditions, particularly in some of the older plants, where the retorts are smaller than in newer plants, a 48-hr cycle is longer than necessary, and some intermediate length of cycle may theoretically be most economical. Use of an intermediate cycle, however, means that the maneuver comes at different times on consecutive days, and that sometimes it comes during the hottest part of the day. The work on the retort furnaces is extremely hot and arduous at best, and it is much worse, of course, if it is done during the heat of a summer day. When labor was plentiful and tractable, many plants were able to operate on cycles of intermediate length, but the workmen did not like the working hours. Under present labor conditions, it is hardly practicable to operate with a cycle of intermediate length, so the choice has narrowed down to the alternatives of 24-hr or 48-hr cycles. In any discussion of economics, too comprehensive generalization is not warranted, because local conditions affecting economics vary greatly. The best economic practice at one plant at any given time may be uneconomical at another plant, or even at the same plant at another time. To determine the length of cycle that is the better practice at a given plant at a given time requires a weighing of the advantages and disadvantages of each cycle, taking into consideration all the local conditions. Some of the factors that must be considered in making the comparison are discussed briefly in the following paragraphs.

Jan 1, 1947

By R. F. Shurtz

R. Duval (Mining Engineer, Ancien eleve de PEcole Polytechnique, Paris, France) I do not agree with the Eq. 3, reading: m =1/100- [(0.214x30.4) + (0.7B6 x0.00)] =6.5pct CaO If 0.214 and0.786 were proportions by weight, the equation would represent the well known mixtures law of the conventional arithmetics and 6. 5 pct CaO would be the correct average content. But it is not the case as the author states: "In samples consisting of single grains of mineral, those grains must, as already mentioned, be either of dolomite or magnesite. Since 78.6 pct of the deposit consists of magnesite and 21.4 pct of dolomite (excluding for present purpose the presence of other minerals), for any single grains picked at random the probability will be 0.214 that is it dolomite and0.786 that is it magnesite. In 1000 such samples the expected numbers of dolomite and mapesite grains will be 214 and 786 respectively." 0.214 and 0.786 would be proportions by weigbt under the necessary condition that all grains of dole mite and magnesite should have an identical weight. Obviously it is not the case, as the specific gravities are not the same for mapesite and dolomite and the volumes of the grains are different. Furthermore, because of these differences the conditions for a random sampling are not fulfilled and we are not authorized to state that the probabilities are, respectively, 0.214 and 0.786. The author however makes a simple application of Eq. 1: M = 1/n— ? fi x i . n Should we deduce that this relation is wrohg? Not at all, but when applying Eq. 1 you must not overlook what it actually. means. Eq. 1 gives a definition of the arithmetic mean of a total of n observed values Xi and nothing else. But the average conteht of a deposit has not the same significance. It is the ratio between the weight of concerned mineral in the deposit and the total weight of the deposit. As from 1000 particles the 214 of dolomite and the 786 of magnesite have not the same weight, the two definitions do not concur, and when applying Eq. 1 the result is an arithmetic mean of figures which has no connection with what is named average contentof a deposit. The situation is similar to the calculation of an average velocity. If a car travels a first mile over at 30 miles per hr and a second mile over at 60 miles per hr, when applying formula 1 you find as average velocity for the 2 miles: 30+60 ------- - 45 miles per hour. Many people calculate in this way and they do not realize that a mistake is involved. In fact the definition of he average velocity for the 2 miles is the quotient of the distance of 2 miles by the time (in hours) necessary for 2 miles travel, i.e.: 2 ---------- = 40 miles per hr. 1 + 1 30 60 In other words, the average volocity wanted is not the arithmetic but the harmonic average of the two velocities. The above mentioned bias in the calculation of the average contents of deposits is frequent, even in the assessments made by experienced engineers and is independant of what is named the sampling error. In order to supress the bias and to be able to use Eq. 1, you must apply a correction. An example on the subject can be found in an article by Duval et al. in the January 1955 issue of the ''Annales des Mines" (French), page 19. R. F. Schurtz (Author's Reply) Mr. Duval's position is quite correct. The proportions shown for dolomite and magnesite., respectively, of 0.214 and 0.786 are, in fact, proportions by weight uncorrected for specific gravity. In our day to day operation of producing magnesite from these mines at a very substantial rate, we do not normally make corrections for the difference between the specific gravity of dolomite and that of magnesite. If these corrections are made in Eq. 3 as shown in my article, then the numbers of grains turn out to be in proportions of 0.226 dolomite and 0.774 mapesite instead of the values actually shown in the equation. For the purposes of our work, and in view of the inherently low accuracy of the data, this correction was not deemed worthwhile making.

Jan 1, 1961

By Rossiter W. Raymond

I desire to call the attention of the Institute to an interesting experiment, which may turn out to be an indication of a valuable improvement in the manufacture of steel. As the members are aware, the addition of ordinary spiegeleisen, in the open hearth or Bessemer converter, to a bath of decarbonized iron, has a twofold object,—the recarbonization of the bath to a desired degree, and the remedy of the red shortness otherwise found to be inevitable in the final product. This red shortness is ascribed to the presence of oxide of iron in the molten metal; and it is supposed that the manganese of the spiegeleisen, uniting with the oxygen of such oxide, carries it into the slag. At the same time there is a small percentage of the manganese usually left in the cast steel, probably to the improvement of its quality. Whatever be the true explanation the effect of the manganese is acknowledged to be not only beneficial, but necessary. But the use of spiegeleisen containing high percentages of carbon limits the quantity that can be introduced, because the carbon must be limited if soft steel is desired. This inconvenience becomes so serious as to prevent the use of ordinary spiegeleisen in the manufacture of steel containing more than, say two-tenths per cent. of phosphorus; since the quality of the steel can be made tolerable only by reducing its contents of carbon in proportion as the

By J. F. Breedis

The morphology and crystallography of marten -site formed during quenclzing were examined by transmission electron microscopy in alloys whose compositions lie between Fe-19 wt pct Cr-11 wt pet Ni and Fe-33 wt pet Ni. Depending upon composition, four types of transformation products were observed in this portion of the Fe-Cr-Ni system. Three of these products are denoted as lath, plate, and surface martensite. The hcp structure found in association with martensite it? certain higlz-clzromium stairzless steels does not influence the transformation crystallogyaphy and cannot he Considered to act as a transitional structure in the transformation from austenite to martensite. DISTINCT changes in the characteristics of mar-tensitic transformations are produced by the partial replacement of nickel by chromium in austenitic iron alloys. Large, discrete martensite plates form in Fe-30 pct Ni, while aggregates of small crystals form in sheets parallel with (111)A austenite planes in stainless steels containing in the vicinity of 18 pct Cr and 8 pct Ni. These transformation structures are termed plate and lath martensite, respectively. In addition, an hcp structure (E) has been observed in certain high-chromium stainless steels in association with martensite. It has been suggested that the E structure acts as an intermediate step in the nucleation of martensitel-' and influences the morphology and crystallography of the final transformation product. However, this structure may be the consequence of the deformation of austenite arising from the shape distortion accompanying the transformation to bcc martensite.' An hcp stacking of atoms is produced in an fcc lattice by the introduction of an intrinsic stacking fault on alternate (111)A planes. At present, the arguments behind each explanation for the E structure are based on circumstantial evidence. This investigation seeks to determine the importance of the hcp structure to the martensitic transformation, and to examine the crystallography and morphology of the structures produced in bulk samples by quenching in alloys whose compositions lie between Fe-19 wt pct Cr-11 wt pct Ni and Fe-33 wt pct Ni. These aspects of the martensitic transformations occurring in these alloys have been studied by electron metallography and selected-area diffraction of foils examined in transmission in the electron microscope. EXPERIMENTAL METHODS The alloys have been prepared from thoroughly mixed powders of pure iron (99.6+ pct, 0.06 max pct C, 0.15 max pct N), chromium (99.9+ pct), and nickel (99.9+ pct). After sintering in an Ar-H2 atmosphere, the mixtures were melted by induction heating in recrystallized alumina boats under purified argon. The ingots were cold-rolled to 0.4-mm sheets (100 pct reduction in thickness) after the removal of at least 1.5 mm from their surfaces by grinding. Three-millimeter discs were punched from the cold-rolled sheet and annealed at 1150°C for approximately 24 hr in evacuated quartz capsules. The average grain size was 40 µ Thin foils for examination in transmission in the electron microscope were prepared from discs quenched to liquid-nitrogen temperature. A depression was first jet-machined into the center of a disc and a thin area (less than approximately 3000A in thickness) was produced at the base of the depression by electropolishing. Electron-microscope studies utilized the RCA EMU-3 and the Philips EM-100B microscopes operating at 100 kv. X-ray examination of the polycrystalline alloys was performed either in a diffractometer or in a

Jan 1, 1964

By H. C. Fiedler

SILICON-IRON strip with a cube-on-edge secondary recrystallization texture is made commercially as thin as 10 mils. With inclusions present to inhibit normal grain growth, a few grains, and these have the (110)[001] orientation, grow very large at the expense of the matrix grains. In the absence of inclusions, only normal grain growth occurs and the texture is not as strong as when it is developed by secondary recrystallization.1 Strip for use at frequencies of 400 cps and higher is made in thicknesses of 1, 2, and 4 mils by a process developed by Littmann.2 Attempts to develop a strong texture in these thin gages by the same methods as were used for the 10 mil and thicker strip were unsuccessful,2 and Littmann's solution to this problem was to cold roll the grain

Jan 1, 1963

By J. C. Scully, G. Sanderson

The electrolytic formation of y hydride in thin foils of Ti-5Al-Z.5Sn alloy and four Ti-A1 binary alloys has been studied by electron microscopy and electron diffraction. Two orientation relationships have been found: THE adsorption of hydrogen by titanium alloys from aqueous solutions has been widely reported. This can occur, for example, in both alkaline' and acidic2 pickling baths, in chemical polishing374 and electro-polishing Solutions,3,4 during cathodic polarization5" and under certain corrosion conditions,7,8 Etching reagents may also produce visible precipitates, sometimes after an aging period.9 During an investigation into the stress corrosion susceptibility of a titanium alloys by thin foil electron microscopy many observations have been made of hydride precipitation which has been deliberately promoted by techniques that are described below. The characteristics of hydride precipitation are reported and the observed crystallographic orientation relationships are discussed with reference to distortion in the titanium lattice created by the presence of the hydride. EXPERIMENTAL TECHNIQUE One grade of commercial titanium and five alloys were examined. Their composition and hardness values are shown in Table I. All the materials were in the form of thin sheet, 0.05 to 0.065 cm thick, which had been annealed after cold rolling. Foils suitable for transmission electron microscopy were made in two ways: a) by chemical polishing; and b) by elec-tropolishing. The solution used for chemical polishing was a mixture of 44 pct HF and 73 pct HNO3 in the volumetric ratio 2:3. During this polishing specimens were manually moved up and down in the solution. The reaction was veFy rapid, specimens thinning to foil thickness (2000A) in 5 min. Since chemical polishing solutions tend not to cause hydride contamination if they are kept cool3 no attempt was made to prevent the solution from becoming hot during the thinning operation. Electropolishing was performed at -30° C with a mixture3 composed of 295 cu cm methyl alcohol, 175 cu cm n-butyl alcohol, and 30 cu cm perchloric acid with an applied voltage of 40 v after chemically thinning specimens to approximately 0.017 cm thickness in a cool solution of 44 pct HF, 40 vol H2O2, and water in the volumetric ratio 1:6:3. EXPERIMENTAL RESULTS 1) Ti-5A1-2.5Sn Alloy. The Ti-5A1-2.5Sn alloy was severely contaminated by hydrogen during the chemical polishing. Foils obtained in this way contained large amounts of the y hydride phase. A typical micrograph is shown in Fig. l. The laths were identified as the hydride phase by selected-area diffraction of a large number of foils examined in a tilting stage that could be turned through 40 deg. Using the lattice spac-ings of the alloy obtained by X-ray diffraction as a standard the a value of the hydride was determined fromo the electron diffraction patterns to be 4.38 to 4.40A. The accuracy of this figure is only about ±2 pct. Further evidence of the identification was obtained by vacuum annealing chemically polished foils of the alloy at 500°C. This resulted in the dissociation of the hydride with the production of dislocations and possibly vacancy loops as shown in Fig. 2. The hydride

Jan 1, 1968

By P. Dayal, L. S. Darken

THE migration of carbon in austenite under the influence of an electric current has been observed qualitatively several times.14 Lebedev and Guterman5 recently have reported quantitative measurements; their method consisted of welding a low-carbon to a high-carbon wire, passing current, and later estimating the carbon distribution metal-lographically. We believe the method reported in this paper is superior in principle since electrolytic migration and ordinary diffusion are not necessarily coupled as in the weld method; also for the first time the extent of migration is determined by combustion analysis for carbon. A uniform tubular specimen (S.A.E. 1045 or 1095) was mounted as illustrated in the figures. the whole assembly being in an atmosphere of purified nitrogen. Direct current (129 to 226 amp at 0.65 to 1.0 v) served as source both of heat and of potential gradient for carbon migration. The duration of experiment was 7.5 to 12 hr, during which time the temperature was controlled (±10°C) manually. The experimental conditions are indicated in the first five columns of table I. With this experimental arrangement, the temperature initially has a maximum value at the central plane. Also, in this vicinity (by virtue of the symmetry), the carbon entering any volume element is equal in quantity to that leaving; the loss or accumulation of carbon occurs near the electrodes since the carbon moves uniformly near the center and is "frozen" at the cold ends. Hence, providing the time of experiment is not sufficiently long to seriously influence the conditions at the central plane, carbon crosses this plane only under the influence of the electrical potential gradient and not under the influence of temperature or concentration gradient. The amount of carbon which has crossed this plane was determined by combustion analysis of the two halves of the specimen. The results of these analyses are shown in the sixth and seventh columns of table I. It will be noted that substantial amounts of carbon migrated from the anode portion to the cathode portion (except at 920°C, which temperature was too low to exhibit the effect in the allotted time). In spite of precau-tions taken, considerable decarburization occurred as may be seen by comparing cols. 8 and 5. In three cases (indicated by asterisks in table I) the specimen was ground on one side, polished, and examined metallographically before analysis. One specimen was normalized and re-examined. Micrographs of selected areas in specimens 4 and 6 are shown in figs. 1 and 2, respectively. Evidence of carbon migration from the anode toward the cathode is quite apparent. Fig. 2 shows abundant graphite as well as cementite in a region near the cathode. The temperature of this zone is estimated at about 800°C. In fig. 1, particularly in the micrograph on the extreme right (the right side of which is of unaltered carbon content), there is evidence of slight depletion of carbon in the immediate vicinity of the cathode as contrasted to the general increase in carbon of the cathode half of the specimen. Although this may be attributed in part to decarbur-ization, it is believed that it is occasioned also by thermal diffusion—migration (of carbon) from a cool to a hot zone4—a phenomenon superimposed upon the electrical migration. Evidence of carbon migration was visible particu-larly during the course of the high-temperature,

Jan 1, 1951

By T. F. Bower, M. C. Flemings, H. D. Brody

A series of experiments are reported which show thai reasonable assumptions for analysis of solute redistribution in solidification of castings and ingols illclr(de: negligible undercooling before nuclcation of solid phases, negligible increase of solute in advance of the tips of growing dendrites, complete diffusion within the Liquid oer distances the order, of dentrite arm spacings, platelike dentrite t/o?$holog?.. Qzmli/ali,e and periment is obtained JOY Al-Cu alloys front measurements of amount of nonequilibrium second phase, minimum solute content at the centers dentrites arms (after solidification), and 3) change in minimum solute content in dentrite arms during solidification. In a previous paper' analyses were given describing solute redistribution in dendritic solidification. The analyses were undertaken primarily to permit prediction of "severity of microsegregation" in a casting or ingot after solidification and cooling to room temperature, but can also be used to predict "local fraction solid' as a function of temperature in the solidifying alloy. Numerical results were given for Al-Cu alloys. The aims of this paper are to examine the validity of some of the assumptions of that analysis, and to compare predictions of the theory with experiments. All experiments reported are on Al-Cu alloys, the bulk on Al-4.5 pct Cu alloy. EXPERIMENTS Experiments conducted were on small ingots, 41/2 in. in diam by about 10 in. high. solidified in a controlled thermal environment (i.e., in a resistance-heated, re-circulating air furnace, whose temperature could be controlled to 1°C). In one series of experiments, the ingots were solidified very slowly (solidification time was varied from 8 to 1000 hr) and at constant rate of heat extraction. In a second series of experiments the ingots were solidified ( 'unidirectionally". Fig. 1 is a sketch of the method of making the two different types of ingots. The unidirectionally solidified ingots were fully columnar, and the slowly solidified ingots had equiaxed structures, Fig. 2. In making the slowly solidified ingots, the mold employed was carbon steel, coated with inert refractory. Typically the mold and its environment were heated to 700°C. The molten alloy was then poured into the mold and the temperature of the system equilibrated above the liquidus. The environment of the mold was next cooled with a controller responding to a differential thermocouple that measured the difference between the temperature of the melt and the temperature of the mold environment. The differential thermocouple consisted of one chromel-alumel junction in the melt connected in opposition with a second junction in the furnace. The potential across the differential thermocouple was input to the controller which acted to keep this potential at a set. constant value; hence the temperature difference between the two junctions was maintained nearly constant. Major resistance to heat flow in the above apparatus was between the metal surface and the furnace atmosphere, not in the metal itself. By maintaining a constant temperature difference between the metal and the furnace atmosphere, the controller maintained an essentially constant rate of heat extraction during solidification, regardless of amount of heat released by the metal per unit temperature change. When the metal temperature dropped just below the eutectic temperature. the ingot was removed from the furnace and water-quenched. The unidirectionally solidified ingots were cast in a similar mold to the foregoing except that provision was made to extract heat through the bottom face of the mold by passing air or water through the mold base, Fig. 1. For these experiments, metal and mold temperature were again equilibrated above the liquidus. Temperature of the mold environment was then held

Jan 1, 1967

By C. H. Li, J. Washburn, E. R. Parker

Yield stress in single crystals of zinc was shown to be dependent on prior annealing temperature and rate of cooling after annealing. Rate of strain hardening beyond the yield was not sensitive to annealing procedure. A tentative mechanism for the effect was discussed. COMPARATIVE mechanical tests of metal single crystals generally show a large scatter of results. Many factors may contribute to this variation. The present investigation was undertaken to evaluate the influence of two factors not ordinarily considered of major importance—annealing temperature and cooling rate after annealing. Since plastic properties of crystals are thought to depend on the presence of lattice imperfections, it follows that a variation in properties should result from differences in the distribution and density of these imperfections. Furthermore, in the light of current theories of interaction between edge dislocations and lattice vacancies,' it seems possible that annealing temperature and subsequent rate of cooling might play a part in this distribution. Analysis of the effect of these variables on plastic properties may lead to a better understanding of the annealed state. Single crystals of zinc which have been strained in simple shear undergo complete recovery of mechanical properties upon subsequent annealing. This behavior is useful because a single specimen can be used repeatedly, thus eliminating the uncontrollable variables introduced by the use of many crystals. The test section of the crystals used for these experiments was a cylinder 1/8 in. thick with a cross-sectional area of about 1/3 sq in. The specimens were acid-machined from spherical single crystals 1 in. in diameter in such a way that the slip plane (0001) was at right angles to the axis of the cylinder. In testing, a shear stress was applied along one of the slip directions, [2110] in the (0001) plane.' All crystals, unless otherwise noted, were grown in a helium atmosphere from molten 99.99 pct pure Horse Head Special Zinc. Fig. 1 is a family of curves obtained from one crystal. Each curve was obtained by deforming the crystal to 10 pct strain at a rate of 3 pct per min, following an anneal of 1 hr at 260°C. The strain direction was reversed every other time so that no progressive change in shape of the specimen took place during the series of tests. Since the stress-strain curve was reproducible within a fairly narrow range under the same conditions of annealing, it was then possible to determine the effect of changes in annealing conditions. A crystal was tested repeatedly as previously described but the annealing temperature and rate of cooling preceding each test were varied (Fig. 2). Two cooling rates were used, approximately 30°C per min and 3°C per min. Annealing was conducted at three temperatures, 200°, 300°, and 400°C. For a given annealing time and rate of cooling the room temperature flow stress was higher the higher the annealing temperature. The increase in flow stress was small as the annealing temperature was increased from 200° to 300°C but rose rapidly when the annealing temperature was raised from 300" to 400°C. Faster cooling from the high temperature produced an even greater strengthening of the crystal. The curves were obtained in the order indicated by the numbers. The stress level associated with a certain annealing treatment was, within the limits of scatter, always the same regardless of the

Jan 1, 1954