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By Roussey Roussev

The use of chemical additives on grinding is of significant importance considering the high energy consumption of grinding processes. My research indicates that the dispersant approach explains the effects, in this particular case of wet grinding. Further, the dispersant approach combined with torque measurements give the possibility of clarifying the mechanisms involved when using grinding aids. I find the conclusions derived from the data obtained to be correct and useful for grinding. In general, I agree with the explanations. However, I would like to discuss several additional points that I consider to be important, and in the same time to mention some of my own results from investigations similar to those presented in the study under discussion. The "bed volume concept" and the change of slurry viscosity explain adequately the data plotted on [fig. 3], in conjunction with [Figs. 1 and 2]. However, the significant increase of the average torque in the case of 83% solid with XFS-4272 introduces the necessity of establishing the optimum of percent solid when dispersant is used. For example, the optimum percent of solid for different materials varies. One of the reasons is the material's mass density. On the other hand, it is necessary to determine the concentration of the chemical used. Because of this, it would be interesting to know how the cited concentration was selected.

Jan 1, 1983

Jan 1, 1967

By H. A. MEGRAW

THE meeting of the A. I. M. E. at Wilkes-Barre, Pa., Sept. 12 to 15, inclusive, celebrated the fiftieth anniversary of the Institute. It was at Wilkes-Barre, in 1871, that the foundation was laid for the great institution that now includes in its roster the greatest names. in mining engineering in every civilized country of the world. The founders of the Institute, with rare prescience, established a common ground upon which all mining engineers, whatever particular branch they might consider most pertinent, could stand securely, assured of a deep-seated interest from their brethren similarly minded in other localities. So wise and clear was the vision of the founders that every engineer connected with mining has found it beneficial, not to say indispensable, to maintain his connection with the Institute and to increase his technical enthusiasm through the medium of the valuable technical publications. The little coterie of 1871 has grown to a strong body of more than 10,000 members in 1921, reflecting the glory of the founders in the record of the accomplishments written on the pages of the fifty years of the

Jan 1, 1921

The Western World's gold reserves now exceed 23,000 mt (750 million oz), 65% of which exist in South Africa. Although several major mines are reducing production or closing because of depletion of reserves, new mines or expansions of existing mines are coming on-stream which will maintain an annual production of 684 mt (22 million oz) of gold well into the 1990s. These new operations by the South African mining industry represent the largest expansion since the opening of the Witwatersrand gold fields in 1886. Included in three new mines being opened is that of Anglo American Corporation's Elandsrand plant, their fir& new gold venture in South Africa in seventeen years. Current average grade of South African mines is 8.2 g Au per mt (0.24 oz per st); and while the cost of the Elandsrand 135,000 mt (149,000 st) operation, including mine development, was about $314 million, it is estimated that the cost of a comparable operation started today and completed in the mid-1980s would be of the order of $480 million. New mines to exploit low-grade ore bodies are, therefore, likely to be few in number, and further expansion will undoubtedly be in the form of extensions to existkg operations where cash flow can be used to finance development. The authors' first monograph, "Gold and Silver Cyanidation Plant Practice," devoted a section to South African cyanide plant operation; and it is believed that this new volume would not be complete without a description of Elandsrand, South Africa's newest gold plant. The Elandsrand mine is adjacent to Anglo American's Western Deep Levels on the Far West Rand. The decision to go ahead with the development was taken in mid-1974 from the results of exploration drilling carried out over a period of .lo years. Results of 17 bore holes and 68 intersections of the Ventersdorp Contact Reef had indicated a gold-.bearing reef less than one meter thick at a depth of 1,800 to 3,000 meters (5,900 to 9,840 ft). Preliminary studies indicated a mine of 900 km (560 miles) of underground workings would yield 725,000 kg (23. 3 million oz) of gold from 60 million mt (66 million st) of ore to be milled over a period of 34 years. Eventually, when the mine is in full production, the total hoisting capacity will be 300,000 mt per month (331,000 st) for a milling capacity of 225,000 mt per month (248,000 st). The Elandsrand surface facilities have been built on a low range of 0 hills to take maximum advantage of the 10 slope in transporting ore

Jan 1, 1981

By Hugh H. Waesche

Of all the military services, the Signal Corps is the most concerned with piezoelectric minerals because of its function as a supply service to the strategic and tactical military forces. Consequently this paper is written from the point of view of one associated with that organization. The Signal Corps is responsible for the research, development, and supply of communications, radar, and components to the using services of the Department of the Army and to some extent the Other branches of the National Defense Department. Their work therefore includes the study of the sources* characteristics, and application of quartz and other piezoelectric materials. These materials have become a vital consideration in strategic planning and are essential for efficient tactical operation by all the Armed Forces. The Signal Corps at the beginning of world War 11 Was respon-sible for both Army Ground and Air Force electronic equipment. Since that time this Army service organization has probably done more in the development of frequency control devices using piezoelectric materials than any other group. The U.S. Department of the Interior, Bureau of Mines, Minerals yearbook of 1945, shows that during the four war years, 1942 through 1945, 9,598,-410 Ib of quartz crystal were imported for all uses and of this total, 5,168,000 lb were consumed to produce 78,320,-000 crystal units for electronic application. Other government records confirm these data which conclusively show that approximately 53 pct of the crystalline quartz imported was consumed in the production of electronically applied quartz crystal units. It may be assumed that some effort was made to maintain a stockpile over demands for all purposes. and this would mean that the actual percentage of quartz used electronically was considerably over the 53 pct figure. These data only emphasize that electronic application of crystalline quartz was the greatest requirement, and per- haps the actual value in this application to national defense is many times greater in importance than is apparent on first inspection. Current electronic research and development programs of the Armed Forces are planned around the fundamental use of piezoelectric minerals for frequency control and this at present, at least, means quartz. Definition and Early Development The word piezoelectricity is formed from combination of the Greek word "piezein". meaning "to press," and "electricity." It is that property shown by numerous crystalline substances whereby electrical charges of equal and opposite value are produced on certain surfaces when the crystal is subjected to mechanical stress. It appears to be intimately associated with the better known property, pyro-electricity and in fact, the two may be manifestations of the same phenomeuon. This property was discovered by Pierre and Jacques Curie in quartz, tourmaline, and other minerals in 1880 while studying the symmetry of crystals. The converse effect, that is, mechanical strain in the crystal when placed in an electrical field, was predicted by the French physicist, G. Lippman, in 1881, and verified by the Curies almost immediately. As has been the case with many discoveries of similar character in the basic sciences, not much attention was paid to this property for man)- years except as an entertaining curiosity. Between 1890 and 1892 a series of papers was published by W. voigt in which the theoretical physical properties were put into mathematical form. The first practical application of piezoelectricity occurred during World War I when professor P. Langevin of France used quartz mosaics to produce underwater sound waves. The same mosaics were used to pick up the sound reflections from submerged objects which were in turn, amplified by electronic means and used to determine the distances to such objects. This device was intended for use as a submarine detector but development was not completed in time for war service although it was used later for determining ocean depths. About the same time, A. M. Nicholson, of Bell Telephone Laboratories, developed microphones and phonograph pickups using Rochelle salt crystals. A major step in the application of piezoelectric quartz came in 1921, when professor W. G. Cady, of wesleyan university, showed that a radio oscillator could be controlled by a quartz crystal; from that date, this use of quartz has increased steadily, reaching its peak in world war 11 as is shown by the figures previously given. Essentially all American electronic equipment for communication, navigation, and radar, utilized quartz crystals for the exacting frequency control required. Crystalline Minerals with piezoelectric Properties QUARTZ Hundreds of piezoelectric crystalline materials are known, most of which are water soluble. Of these, quartz appears to be without a peer for electronic frequency control. Unfortunately, the quartz must be of superior quality. It must be free of mechanical flaws, essen-tially optically clear, free of both Brazil and Dauphiné twinning and must be, for average uses, over 100 g in weight. Because of these stringent requirements, raw quartz of the quality desired is of rare occurrence. In addition to quartz, several other naturally occurring crystalline materials are known to have the piezoelectric property and could perhaps be substituted for quartz in some applications. These

Jan 1, 1950

The following list comprises the names of those persons who became members during the period May 10, 1919, to June 10, 1919. ALAYZA, CARLOS Box 850, Lima, Peru, S. A. BALLARD, P. A Surveyor, Midwest Refin. Co., Custer, So. Dakota. BARNEBL, A. J., JR.... Mech. Eng., The Dorr Co., 101 Park Ave., New York, N. Y. BILLINGS, GOODSELL Platteville, Wis. BRONSON, C. B., Mech. & Met. Engr., New York Central Lines, Room 1520, Grand Central Terminal, New York, N. Y. BUNCE, E. H Met., The New. Jersey Zinc Co., Palmerton, Pa. CHARLTON, D. E. A., Editorial Staff, Engrg. & Mm. Journals 10th Ave. & 36th St., New York, N. Y. DAVIS, JOHN N., Supt. of Mills, Engels Copper Min. Co., Engelmine, Plumas Co., Cal. DUKES, GLENN H., Chief Engr., The Sunday Creek Coal Co.,1001 Outlook Bldg., Columbus, Ohio. ERICKSON, ARTHUR .... Engr., United Smelt., Refin. & Min. Co., Mldvale, Utah. FLYNN, A. E Supt., Rand Consolidated Mines, Ltd., Goudreau, Ont., Canada. HIBBARD, WALTER R 63 Ashley St., Bridgeport, Conn. HOBSBAWN, I. BERKWOOD, Cons. Tech. Chem., Messrs. Gibbs. & Co., Valparaiso, Chile, S. A.

Jan 7, 1919

By Mark L. Requa

(San Francisco fleeting, October, 1911.) DURING the past two years California has developed a new and important oil-field : I refer to Midway. This field produced the famous Lake View gusher, which is credited with a total production in excess of 8,000,000 barrels. Fortunately for the oil industry of the State, this well is now a thing of the past, and nothing save a great crater-like opening marks its location. The pipe is entirely worn away and gone ; and it is a matter of serious doubt if there can be anything done that will cause the well to produce again. Fortunately, also, there have been no, other wells in that field or elsewhere throughout the State that in any way compared with the Lake View. Midway is noted for large wells, of from 500 to 2,000 barrels production; but the decline is rapid, and a few months serve to bring the output down to a few hundred barrels. In the oil-territory heretofore blocked out as proved and probable, there have been, during the year, many changes. Some areas which were expected to be fairly productive have apparently failed; others, more strictly "wild-cat," have come in; while in some of the older fields there are properties which are beginning to show evident signs of exhaustion. The total area of proved territory will therefore probably suffer but small increase, when balances are struck off. The increase of new area has come from extensions of the Midway field, the development of a field in Lost Hills and Belridge, and extensions of the Fullerton-Whittier field in southern California. In these later developments, down to date, the fresh area absolutely proved is not much in excess of 3,000 acres. Recent developments in Coalinga indicate the possible extension of that field to the south, but at great depth. Coalinga is still the most northerly field of any consequence in the State. The Kettleman Hills have hitherto brought in nothing, although a

Apr 1, 1912

By H. W. Mead, C. E. Birchenall

The rates of growth of graphite nodules in cast irons are calculated for a model of a growing graphite sphere surrounded by a shell of austenite through which carbon and iron are diffusing. The carbon is supplied by a cementite-austenite mixture at the outer edge of the shell. The calculated rates from carbon diffusion agree fairly well with the measured values, but the rates based on iron self-diffusion are much too low. Because the iron must be removed for the process to continue, o plastic deformation mechanism is suggested. THERE has been an unfortunate tendency in the literature of growth and dissolution reactions to identify the slope of a plot of the logarithm of the growth or dissolution rate vs reciprocal of temperature with the activation energies determined by diffusion measurements in chemically similar systems. If the solubility limits at the growing or dissolving phase interfaces change appreciably with temperature, such procedures may lead to serious errors in specifying the mechanisms controlling the rates of these processes. A reaction involving the simultaneous growth of graphite from and dissolution of cementite in austenite will be discussed here to show that substantial oversimplifications have been made in earlier studies of this process. From a dilatometric study of the overall y-range graphitization process, Bunin and Danil'chenko' found an apparent activation energy of 90 kcal per g-atom. They concluded that, since this value was much nearer the approximately 68 kcal per g-atom observed for self-diffusion in pure iron than it was to 32 kcal per g-atom for diffusion of carbon in iron, the rate-controlling process must be the diffusion of iron away from the growth interface to provide space for graphite to grow. Bunin and Salli' bolstered this agreement with the observation that graphite forms preferentially at surfaces, cracks, and pores where free volume is present initially. Ziegler, Meinhart, and DeaconQ ad found an apparent activation energy for graphitization of 98 kcal per g-atom. This value, like that of Bunin and Danil'chenko, applies to nucleation and growth occurring simultaneously. It is not generally assumed that nucleation is entirely diffusion-controlled. Treatments such as prior cold-working and prequenching, which strongly affect the rate of graphitization, would be expected to have little effect on diffusion processes occurring at the graphitization temperature. In any case 90 kcal per g-atom is not particularly close to the 54 kcal or lower to be expected for diffusion of iron which is carbon-saturated.' The presence of silicon in iron is said to reduce the activation energy for diffusion,' so its presence in cast irons would be expected to have a similar effect. The growth rates of nearly spherical graphite nodules have been studied by Brown and Hawkes." The initial rate of growth before impingement of adjacent carbon-depleted areas was found to be parabolic, and rate constants were measured at several temperatures. Their apparent activation energy for the growth process only was roughly 45 kcal per mol. Burke and Owen' made growth-rate measurements on several alloys, recording appreciable induction periods, initial nucleation rates, and average radial growth rates based on an assumed linear rate of radial growth. They found that increased silicon content increases the ovel-all reaction rate and the initial rate of nucleation, and decreases the induction period. Assuming 1) spherical nodules. 2) constant volume rate of nucleation, 3) austenite in equilibrium with cementite at positions where the cementite is not depleted, and 4) a constant diffusion distance during the growth of a nodule, they calculated an apparent overall activation energy of 68 kcal per mol, which was related to an activation energy for nucleation of 79 kcal per mol and activation energy

Jan 1, 1957

By T. W. Healy, D. R. Dixon

The mechanism of activation of ZnS by metal ions and the subsequent flotation induced by xanthate has been considered as a surface redox reaction. By ultraviolet (UV) irradiation of ZnS suspensions, the normally inert ZnS is caused to react with xanthate in the absence of activator. By similar UV irradiation, the rate of adsorption-exchange of activator ions at the ZnS-H2O interface is also increased. Mechanisms of these reactions are proposed and compared to current electrochemical and semiconducting models of sulfide flotation.

Jan 1, 1976

By S. H. Moll, R. E. Ogilvie

The investigation of solid-state diffusion phenomena may lead to much information concerning binary alloys. In particular, a study of the concentration gradients present in multiphase diffusion couples can lead to the determination of the solubility limits of the single-phase fields in the phase diagram. The specific concentration gradient which results from the heat treatment of a diffusion couple depends not only upon the time and temperature of diffusion, but also upon the number of phases existing in equilibrium at the diffusion temperature. Such concentration gradients possess sharp discontinuities whose terminal points correspond to the solubilities existing at the limits of the two-phase field in the phase diagram at the diffusion temperature. In general, there will be a discontinuity in the concentration curve for each two-phase field which exists in the phase diagram between the concentration limits of the couple. A number of investigators have analyzed the gradients present in multiphase diffusion couples. 1-8 The iron-titanium phase diagram exhibits a y loop in the temperature range from 900" to 1400°C, and the limit of the a + y field lies at some composition which is less than 1 wt pct Ti for any temperature. It was felt that a diffusion study could yield values not only for the diffusion coefficients involved, but also for the chemical solubilities in the phase diagram. The concentration gradients were analyzed by an X-ray absorption technique developed by Ogilvie.6 The absorption of a monochromatic X-ray beam is measured in steps parallel to the diffusion direction and the resulting intensity gradients are transformed into concentration gradients by applying the laws of X-ray absorption in a binary system. This technique has been applied by ogilvie6 to the systems Ni-Au, Cu-Au, Fe-Cr, and Ni-Cr; by Gelles7 to the systems Be-Fe, and Be-Ni and by Hilliarde to the system Al-Zn. Linear X-Ray Absorption Analysis—The use of X-ray absorption analysis as a tool for determining concentration gradients arises from the fact that the beam is absorbed according to the quantity and species of elements present in the sample and not according to their state of aggregation. This method is more advantageous than the chemical analysis of machined layers since it is less time consuming and less expensive and can analyze a very small area. IF a homogeneous binary alloy (A + B) is analyzed with two different monochromatic X-ray beams I0(2) and lo(2) the following relation between the transmitted intensities, the intrinsic absorption coefficients of A and B for the two different radiations and the weight fraction of each element may be derived.' In (I/Io) (a+b) xa(u/p)a(2) + xb(u/p)8(2) Eq. [1] is independent of specimen thickness and density, but requires that either element A or B possess an absorption edge between the wavelength limits of the two monochromatic beams. I, is evaluated for each radiation by measuring the transmitted intensity through a varying number of foils of a suitable absorber. A plot of the natural logarithm of the transmitted intensity as a function of the number of foils, when extrapolated to zero foils, yields the value of I,. If a plot of the ratio in Eq. [ I] is calculated as a function of xA, then a master curve results. From

Jan 1, 1960

Secretary's Note.—M. Beutter's introductory remarks, being simply a resume of Prof. Hone's paper, with a disclaimer of the intention to criticise it, have been omitted, and the remainder of this contribution lias been somewhat condensed, without omitting any essential statements. M. Beutter, St. Etienne, France* (communication to the Secretary†):—Professor Home observes in $ 47 of his paper that the fluid-compression of steel diminishes piping by forcing the liquid and viscous metal, while the pipe is forming, or after it has formed, into the space so produced, and proceeds to study the different systems of compression, alluding to the four principal ones: Whitworth, Illingmorth, Williams, and Harmet. Having now for many years had in use the last-named process, that of M. Henri Harmet, I shall attempt to explain the difference between it and the three other processes named. The Harmet process does not diminish or close the pipe after it has formed, but prevents it from forming; and I may add that it is the only one of the four which produces this result. It is true that the Whitworth process diminishes the interior hollow by localizing it around the central axis of the ingot, which is afterwards removed by trepanning the hollow forg-ings for which this process has been, I believe, always exclusively used. The Illingworth and Williams processes, which, in my opinion, are applicable only to small ingots, of necessity allow the pipe to form, or (to use the expression of Professor Howe) they allow the surface of the lake of liquid steel to sink into the interior of the ingot, since they involve waiting a certain time before compression, so that (in the case of the Williams process) the ingot-mold can be opened without danger, or (in the case of the Illingworth process) so as to avoid the risk that the steel may enter the grooves produced by the removal of the distance-bars. During the time required for

Jan 1, 1908

By AIME AIME

DESTRUCTION of the plants, machines, utilities, tools, materials, and other essentials for peacetime living penalizes not only the owners of the materials destroyed, but the world as a whole. Specifically, the fundamental fallacy of any proposal for the in- discriminate destruction of the German industrial system is that it fails to differentiate between the wartime and the peacetime economy of the Reich. We are for one simple, clear objective-an effective industrial means to keep Germany from starting another war. This objective should not be con- fused, especially before the war is even won, with the appropriate punishment of Germany or with the international arrangements for the long future to be made around the peace table by the representatives of the Allied Nations after victory is achieved. This paper, therefore, does not deal with broad, complex postwar questions of diplomacy and international policy. "Unconditional surrender" implies disarmament of the German armies, the surrender of all arms, munitions, air- planes, and other ordnance material in stock piles or in process. It also should include the elimination of all German war production facilities, such as ordnance plants, munitions plants, and submarine works, and the control of raw materials required by war industries.

Jan 1, 1944

By Walter E. Hopper

(Wilkes-Barre Meeting, June, 1911.) I. LOCATION AND EXTENT. THE Caddo oil-field, shown in Fig. 1, is located in Caddo parish, northwestern Louisiana. The known producing territory of oil is covered by townships 19 N, 20 N, 21 N, 22 N, and ranges 15 and 16 W., shown in Fig. 2. The center of the field may be taken as Oil City, 24 miles north of Shreveport, on the Kansas City Southern railway. Shreveport is the second largest city in the State, and is the connecting point of five rail-road-lines. Drilling at the present time, however, is going on all over northern Louisiana, especially in Caddo and the neighboring parishes. II. HISTORY AND DEVELOPMENT. Natural gas escaping at the surface is found at numerous places in northwestern Louisiana. At Shreveport, the plant of the Shreveport Ice & Refrigerating Co. has been lighted by natural gas for 20 years. The well was drilled for water, but was abandoned on account of the gas. A test well, put down in 1905 near the western limits of Shreveport, was driven to 1,650 ft., and encountered indications of gas and oil at various depths, but did not succeed in finding enough to be profitable. Attention was first attracted to the Caddo field in 1895 by indications in water-wells from 40 to 60 ft. deep, in which the pressure of natural gas was noticeable. This indication of gas in a shallow well led to the drilling of the first well in the Caddo field, the old Savage Brothers & Morricell, or the Caddo Lake Oil and Pipe Line No. 1. The rig for this well was erected in May, 1904, and drilling began in June, 1904. The well was bailed Mar. 23, 1905, with a small amount of oil. It was deepened July, 1905, and converted into a "gasser " Jan. 3, 1906. It was abandoned January, 1907. In consequence of the finding of oil in the Savage well, drilling-operations were pushed with energy; and in April, 1905, four wells were drilling. Great trouble was experienced with

Apr 1, 1911

By P. Duwez, C. B. Jordan

A. J. SHALER*—I should like to congratulate the authors for having carried out such a precise set of experiments. It has been found useful, in sintering experimental compacts in vacuo, to make certain that the residual gas is not one which reacts with the metal. Since traces of oxygen can be kept away only with great difficulty, the technique is often adopted of using a "getter " of powder in the vicinity of the compacts, and, in addition, of permitting a small hydrogen leak to flow into the vacuum chamber. Did the authors use similar devices? This paper brings up a question concerning the definition of the word ' sintering.' The authors restrict its use to the adhesion between particles. Kuczynski, in a paper presented at this meeting, applies the word to the growth of areas of contact between particles. I have used it to mean both these phenomena and also the dimensional changes which continue to take place after the first two have run their course. May I suggest that we should come to an agreement on the use of these words ? Fig 1 and 2 show an interesting feature: extrapolation of the curves to zero time does not give a densification parameter of zero. The higher the temperature, the higher is the intercept on that axis. These observations agree with the concept of a practically instantaneous densification taking place while the compact is being brought to heat. Such a change may be brought about by plastic deformation and primary creep. The stress pattern causing this first rapid flow is, to my mind, due to the force of attraction between the surfaces of opposite particles in the regions immediately flanking their common areas of contact. The stress is not temperature-sensitive, but at room temperature plastic deformation only proceeds until the metal in the area of contact can support it elastically. As the metal is heated, the elastic limit falls, and further plastic flow occurs. At the higher temperatures, this is followed by primary creep, and finally by the steady-state rate-reaction which the authors are seeking. If they were to recalculate their densification-parameter values, using, not the initial density of the cold compact, but the density after the compacts have been brought to temperature, the systematic deviations from linearity in Fig 3 and 4 might be eliminated. Such initial densities might be obtained by extrapolating the curves of Fig 1 and 2 to zero time. I am naturally pleased to see that such a very well done series of experiments leads to a heat of activation (for the densification process in hydrogen) that is much higher than that for self-diffusion, in confirmation of the less elaborate results reported by Wulff and myself (Ind. and Eng. Chem., (1948) 40, 838). J. T. KEMP*—I would like to comment on Dr. Shaler's remarks. There are apparently different interpretations of the word "sintering." It seems to me that an accurate definition of our word is essential in all metallurgy. May I point out, in this connection, that in practical metallurgy the word "sintering" has been applied to a bonding process in the preparation of ores and flue dust for fur-nacing. It would be unfortunate if in the area of powdered metallurgy we should establish a definition that is essentially different in meaning. F. N. RHINES*—I think that I can answer the question by saying that I see no essential difference between the use of the term "sintering" in extractive metallurgy and in powder metallurgy; physically the same things are going on. I admit sintering is used for different end purposes in the two cases. When we resort to the sintering of lead ore mixture we are doing so to obtain a chemically reactive, loose texture of some rigidity. This is only a difference in use. After all, in powder metallurgy we sometimes deliberately produce a very porous material which has just a little strength, just as in the case of sinter cake. P. DUWEZ (authors' reply)—We agree that it would be helpful to have well-established definitions of such terms as "sintering." Since the question has now been raised, the time might be appropriate for its consideration by some suitable committee of one or more of the metallurgical societies. In answer to Dr. Shaler's first question, no getter nor hydrogen leak was used in our vacuum experiments, except insofar as the guard disks (used to reduce friction between specimens and trays) may have acted as getters. Dr. Shaler's statement that extrapolation of the curves of Fig 1 and 2 does not lead to zero densification at zero time apparently overlooks the logarithmic

Jan 1, 1950

By S. G. Cupschalk, J. J. Wert, R. A. Buchanan

The uniaxial deformation of thermally ordered and disordered polycrystalline Cu3Pt was studied by means of the X-ray line - broadening analysis according to Warren and Averbach and the extension of this analysis to ordered fcc materials by Mikkola and Cohen. Because of the heat treatment history, extinction had a pronounced effect on the X-ray spectra of ordered and disordered C%Pt at small plastic strains. After an appropriate correction for extinction, the long-range order in thermally ordered ChPt was found to decrease at a slow constant rate with plastic strain. Furthermore, the antiphase domain probability increased at a constant rate to 17.5 pct strain. The effective particle size behavior indicated that the stacking fault energy is lower in ordered than in disordered Cu3Pt. Analysis of the stress-strain curves shouled that ordered Cuzt has a slightly lower yield Point but a much higher work-hardening rate than disordered Cu3Pt. THE presence of long-range order in a solid-solution alloy has a marked effect on its mechanical properties. While this effect has been known qualitatively for many years, it was not until recently that detailed investigations have been performed to determine the exact role long-range order plays in this strengthening mechanism. The development of an advanced, quantitative. X-ray diffraction analysis by Warren and Averbachl and the extension of this analysis to the L1, type super lattice by Mikkola and cohen2 have greatly accelerated research in this field. The research reported in this paper consisted of two primary phases. The first phase was to determine the effect of long-range order on the tensile properties of polycrystalline Cu3Pt. This objective was accomplished by comparing the stress-strain behavior of thermally ordered CusPt to that of thermally disordered CusPt. The second phase of the research was to determine the difference between the atomic arrangements in thermally ordered and thermally disordered Cu3Pt as a function of uniaxial deformation and thereby gain a deeper insight into the mechanism by which long-range order affects the tensile properties. This second objective was accomplished by applying the Warren-Averbach method of peak profile analysis to the X-ray diffraction patterns obtained from ordered and disordered Cu3Pt after given amounts of uniaxial deformation. EXPERIMENTAL PROCEDURE The Cu3Pt was prepared by vacuum melting and casting. After a homogenization anneal, the ingot was cold-rolled to sheet form. Two tensile specimens with gage sections of 2.50 by 0.500 by 0.115 in. were carefully machined from the sheet. The specimens were polished with a final step of 600-grit paper to insure smooth diffracting surfaces. Finally, one specimen was heat-treated to yield an average grain diameter of 0.016 mm and an initial degree of long-range order, S, of 0.825. The other specimen was water-quenched from above the critical temperature, 645"C, to yield an average grain diameter of 0.017 mm and zero long-range order. The heat treatment history of each specimen is shown in Table I. The tensile tests were performed utilizing a Research Incorporated Model 900.95 Materials Testing System. This unit employs a closed-loop feedback system which maintains a constant strain rate through an extensometer clipped to the gage section of the tensile specimen. A strain rate of 1.32 i0.02 x 10"4 sec-' was employed in testing both specimens. In the X-ray diffraction analysis, a General Electric XRD-5 diffractometer equipped with a pulse-height analyzer set for 90 pct efficiency was employed. The goniometer speed selected was 0.2 deg, 20, per min. Filtered Cu radiation was used for all peaks and all peaks were chart-recorded. Because of nonuni-form grain size. it was necessary to spin the specimens during X-ray analysis in order to obtain reproducible integrated intensities. The spinning rate was 2000 i100 rpm. The application of the Warren-Averbach method of peak broadening analysis to a diffraction pattern is very time consuming if done manually. In this research, the calculations involved were performed with the aid of a computer program by wagner.3 As reported by Wagner, the program is written in Fortran TV computer language. It was modified to Fortran I1 so as to be handled by the IBM 7072 computer at Van-derbilt University. In the X-ray diffraction analysis of uniaxially deformed Cu3Pt, the 100, 200. 400. 111, and 222 reflections were recorded from the initially ordered sample after 'plastic strains of 3.0, 6.0, 9.0, 12.0,

Jan 1, 1970

G. D. Kneip, Jr., and J. 0. Betterton, Jr. (Union Carbide & Carbon Corp., Oak Ridge, Tenn.)—The authors have contributed to the theory of zone melting by considering the effects of the solidification of the final zone on the distribution curves for the finite length bar. However, they do not consider in sufficient detail the restrictions imposed by the particular metals involved. Eq. 4 has the analytical solution which is equivalent to Pfann's' equation for normal solidification of the final zone. For distribution coefficients less than one, it is apparent from this form of the equation that, as the solidification approaches completion, the concentration attains extremely large values which are inconsistent with the density of physical materials. The necessary restrictions then are that the solute concentration cannot exceed the density of the alloy, or more frequently, the solubility limit in the solid phase. Secondly, the distribution coefficient cannot be constant from 0 to 100 pet solute unless the liquidus and solidus coincide over this whole region. It would thus be more correct to impose limits on the solubility such as would be indicated by a typical eutectic diagram. Furthermore, in this case the assumption that the distribution coefficient remains constant is more likely to be realized. Eq. 4 should then be replaced by the following C,,(x) =k/L-x [ ?11 3 C11 (x)Ddx - ?11 4 Cn(x)dx= k[Cn (L-l)/k] [ L-x/l]x-1 L-l = x = L-l [kCenterlie/Cn (L-l)]1/k-1 The typical shape for the distribution curve in the final zone is indicated schematically in Fig. 12 for the simple eutectic case. The solidification proceeds according to Pfann's' expression until the concentration reaches the maximum solubility in the solid phasc. At this point, the concentration changes abruptly to the eutectic composition and remains at this value for the duration of the solidification. The width of the flat region, and the back reflection of this effect into the concentration curve on subsequent passes, depends upon the ratio of the eutectic concentration to the original concentration, upon the distribution coefficient, and upon the number of passes. Similar effects on the concentration curves in the first zone length would be expected in many systems for which the distribution coefficient is greater than one, and where the maximum solubility is not too much larger than the original concentration. The discussers agree with the authors that the assumption that the liquid is uniform in concentration should be considered with caution. Kneip and Better-ton' have shown, however, that in floating zone refining of zirconium, using induction heating, the distribution of iron agrees with theory which assumes a uniform liquid composition. Hence, in this case, the experimentally realized distribution coefficient agrees with the present phase diagram within the experimental uncertainty. L. Burris, Jr., C. H. Stockman, and I. G. Dillon (authors' reply)—The authors are happy to have received the comments of G. D. Kneip, Jr., and J. 0. Betterton, Jr., which provide additional insight into the zone refining process. It is true that the equations developed are inapplicable if the solute solubility in the solid phase is exceeded. However, this restriction on the use of the equations was clearly stated in the paper. A closer approach to

Jan 1, 1957

By Charles Maier

IT has long been supposed that when crystalline materials are com-minuted the energy used in the production of increasingly smaller grain sizes is not entirely dissipated as heat but that a certain portion is "stored" as a part of the internal energy of the material. This portion usually has been called the "surface energy" of the particles. The practical interest of the Bureau of Mines in this subject in connection with the energy requirements of crushing processes has led to the author's attempt to measure the "stored" energy in finely divided calcite by heat-of-solution methods1. The experiments on calcite showed that "storage" of energy could not be proved for this material, because fine grinding caused a lack of chem-ical homogeneity evidenced by loss of carbon dioxide and subsequent adsorption of water on the surfaces of the calcite particles. When thermochemical correction was made for composition changes the cor-rected heat of solution was less for fine material than for coarse. Con-tinuation of the experimental work into the problem of comparing work and heat in the deformation of metallic crystals, where the calorimetric difficulties were less, showed, however, that in the case of copper and aluminum a real discrepancy between work and heat could be shown. similar results had previously been obtained by Farren and Taylor2 and Hort3 and more or less simultaneously with the author's work by

Jan 1, 1936

By E. Miller, K. L. Komarek, M. Ettenberg

The activity of aluminum in solid Co-A1 alloys has been measured by an isopiestic technique between 850° and 1200°C from 45 to 80 at. pct Al. The activity shows a Precipitous decrease around the stoichzornetric composition of CoAl. Free energies of mixing have been calculated over a limited composition range. Considering an antistructure-vacancy defect mechanism, the degree of intrinsic disorder, a , in CoAl was related to the alunminum activity. Excellent agreement between the calculated and experimental activity curves was obtained for a = 1.25 x 10-4. ThERMODYNAMIC properties of solid aluminum-transition metal alloy are being studied in an investigation of disordering in ordered compounds. In a continuing series of investigations, activities of solid Fe-1,' Ni-A1, kd r-A13 alloys have been measured. From the results for Fe-A1 and Ni-A1, the degree of intrinsic disorder for the equiatomic compounds was calculated2 using equations derived by Wagner and chottk. From the results for Cr-A1 the degree of intrinsic disorder was calculated from equations derived by Orr.' In this paper, the results of the study of Co-A1 alloys are described. Published activity data in the Co-A1 system has been limited to liquid alloys at 1600°C.° A heat capacity study7 of stoichiometric CoAl indicated that a second-order phase transformation occurs at 790° C, attributed to an order-disorder reaction. Oelsen and Middel,' employing the calorimetric mixing of pure liquid metals, obtained heats of formation for compositions from 6 to 90 at. pct Co. Heats of formation for 50 and 78 at. pct Co alloys have also been measured by acid solution calrimetr. The Co-A1 phase diagram, as compiled by Hansen and Anderko,lo is in good agreement with more recent X-ray evidence. The method for measuring activities of aluminum in this study is essentially that employed in the studies of the Fe-1,' i-Al, and r-A13 systems. This isopiestic method entails placing cobalt specimens, in a temperature gradient, in a sealed alumina system containing a pure liquid aluminum source of fixed vapor pressure. The specimens are equilibrated, cooled to room temperature, and their final compositions determined. From the measured temperature of the specimens and the known vapor pressure of pure aluminum the activities of aluminum in the alloy can be calculated. EXPERIMENTAL PROCEDURE The cobalt was 3-mil-thick sheet of 99.9 pct purity (herritt Gordon Mines Ltd., anada). The major impurities were 0.1 pct Ni, 0.014 pct C, 0.018 pct Fe, 0.004 pct S, and 0.005 pct Cu. The aluminum metal had a purity of 99.99 pct (Aluminum Corp. of America) and all alumina parts were 99.7 pct A1,O3 (Triangle RR Grade, Morganite Refractories, Inc.) with major impurities 0.05 pct SiOz, 0.1 pct Fe203, 0.2 pct NazO, and 0.05 pCt K20. Runs 1 to 3 were made with annular cobalt specimens (12 mm ID by 21 mm OD) punched from the sheet. The specimens were deburred and degreased in carbon tetrachloride and in acetone. The samples, each weighing about 150 mg, were then positioned along an alumina rod, a in. OD by 14 in. long, separated by alumina spacers, i in. ID by | in. OD by & in. long. The lower end of the rod was placed in a hole drilled in the center of an 80-g aluminum cylinder. This assembly was put into an alumina crucible, 1+ in. ID by 13 in. OD by 3+ in. high, and the position of each sample was measured to within 50.5 mm relative to the bottom of the crucible. An alumina tube, 28.5 mm ID by 35.5 mm OD by 14 in. long, closed at the top, was slipped over the whole assembly, so that it fitted snugly into the bottom crucible. The entire reaction assembly was tied with molybdenum wire and lowered into a mullite tube, closed at the bottom. A quartz thermocouple tube, closed at one end, containing a t/Pt-10 pct Rh thermocouple, calibrated according to the specifications of the National Bureau of standards,'' was placed along the reaction assembly inside the mullite tube. The temperature of each specimen could be determined by gradually raising the thermocouple and measuring the temperature gradient along the reaction assembly. The combined error in temperature measurement and sample position resulted in a total error of Q°C in the recorded temperature of each sample. The mullite tube was sealed at the top by a water-cooled brass head, connected to a conventional glass vacuum system. The aluminum reservoir is heated to its melting point sealing the alumina system containing the samples. During this process the pressure is maintained below 0.01 li Hg. During subsequent heating to establish the proper temperature gradient and throughout the entire run the pressure is maintained below 2 1 Hg by means of a two-stage mechanical pump. Equilibration runs lasted from 4 to 6 weeks and were terminated by air cooling. The temperature of the liquid aluminum reservoir was brought below its melting point in less than 20 min. For runs 4 and 5, alloy buttons with 49 and 69 at. pct A1 were prepared from the initial high-purity metals by arc melting under purified argon. The alloy buttons were comminuted to powder with an alumina mortar and pestle until the powder passed through a 400-mesh screen, particle size 0.0014 in. Portions of this powder weighing between 50 and 200 mg were placed in small alumina trays, 25 by 15 by 5 mm, which were then

Jan 1, 1969

By A. E. Anderson, H. J. Hilll

Laboratory data for 155 field muds and 77 .shales have been used to develop correlations to estimate the net streaming potential component of the SP. Analysis of these data and comparison with field tests show that streaming potential corrections must be made to obtain an accurate estimate of the electrochemical potential for use in the determinntion of formation water resi-iiviy. The self-potential curve is related to formation water resistivity, and considerable effort within the oil industry has been directed toward clarifying this relationship. The Schlumbergers and Leonardon1,2 recognized that two types of potentials, electrochemical and electro-kinetic, resulted in the net potential variation in the borehole. Most of the later papers have dealt with the electrochemical component and its controlling parameters. The investigations of Wyllie,2" Salisch' and Moore5 provide the most extensive sources of data on streaming potentials across mud cakes. These authors observed streaming potentials of sufficient magnitude to be of critical importance in SP interpretation, if it is assumed that streaming potentials develop only opposite permeable beds. Streaming potentials across shales have been reported by Schenck and by Gondouin, et al.7 Since SP magnitude is the difference in potential opposite shale and sand beds, these authors suggested that the net streaming potential component may be negligible. The present investigation was initiated to evaluate empirically some of the parameters controlling the magnitude of the net borehole streaming potential and to determine whether useful relations between mud properties and net streaming potential could be established. Field muds were used in this investigation. These muds were characterized by the amount and type of chemical treatment utilized for five days before Sampling. Filter loss, mud resistivity, mud density and filtrate resistivity were determined for each mud with conventional methods and apparatus. Mud filtrate pH was estimated with Hydrion pH paper for the appropriate range. Streaming PotentIals Across MuD Cakes Commercial calomel-saturated KC1 electrodes are subject to potential changes attributed to contamination of the very small fiber-tip bridge by particles of clay from the drilling mud.3 To minimize this difficulty, a large diameter bridge (Fig. 1) was constructed with saturated KC1-agar gel and a filter disc of microporous porcelain. Experiments showed that streaming potentials across this bridge are less than 0.2 mv at pressure dif-