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By Boyd Dudley

THE material presented in this paper is an abstract of a thesis submitted by the writer to the faculty of the Massachusetts Institute of Technology, as part requirement for the degree of Master of Science. The investigation was undertaken at the suggestion of Prof. H. 0. Hofman, and it was conducted, under his direction, in the laboratories of the Mining Department of the Institute. The purpose of the work was, first, to study some of the reactions that have been considered as a part of the mechanism of the chloridizing roast, and second, to study the conditions under which nickel oxide and copper oxide may be chloridized. While the production of chlorine gas by various reactions during the chloridizing roast may not be primarily useful in the chloridation of metal oxides and compounds, it nevertheless serves a useful purpose in preventing the dissociation and decomposition of chlorides once they have been formed; for example, the dissociation of cupric chloride into cuprous chloride and chlorine. Therefore it was thought that a study of some chlorine-producing reactions would prove of interest, and the first series of experiments dealt with this phase of the subject. The object of the latter part of the work was to show the possibility of treating heavy sulphide ores, such as those of Sudbury, Ontario, containing much iron and small amounts of copper and nickel, by chloridizing and removing the copper, leaving an iron-nickel oxide product suitable for smelting in the blast furnace for nickel-bearing pig iron. The chloridizing of the copper would, of course, be preceded by a roast for the removal of sulphur, the sulphur oxides being available for the manufacture of sulphuric acid, if under the local conditions this product would be of commercial value.

Jan 12, 1914

By P. A. Boeck

Discussion of the paper of P. A. BOECK, presented at the San Francisco meeting, September, 1915, and printed in Bulletin No. 104, August, 1915, pp. 1539 to 1550. LAWRENCE ADDICKS, Douglas, Ariz.-It does not seem to me that the role played by carrying heat away from one surface to another has been brought out. A cellular construction prevents the motion of air currents. Also in the installation on the top of a reverberatory furnace, that Mr. Krieger mentions, where it stopped the cooling, there is besides the question of overheating. Another complex question, entirely apart from the necessity of not carrying a brick above a certain temperature, is that of not allowing acids and bases to come together at too high a temperature. J. W. BECKMAN.-What cements together the individual cells in the insulating material? Also, how does the material behave in the presence of acids and alkalies, both strong and weak? A. H. KRIEGER, New York, N. Y.-The material is formed or composed of myriads of lace-like skeleton remains of diatoms visible only -under a powerful microscope. The diatom lives in salt and fresh water. On the Pacific Coast there must have been an abundant life of the diatom, because the beds, still in existence in Southern California, are fully 1,000 ft. through, and are hard and strong, standing a pressure of more than 400 lb. per square inch. The beds must have been many ages in forming and the diatoms have become firmly packed together. The samples shown are typical of the entire deposit as it was formed at the bottom of the sea. Once this structure has been destroyed, it is impossible to reconstruct it without artificial bonding materials. With the exception

Jan 12, 1915

DESPITE the very small number of engineers who can get away from their tasks to New York, a point so far from the Mid-Continent and Cali-fornia oil fields, where the real important, engineering progress in the industry is being made, the attendance was remarkably good, and it was generally remarked that all the sessions were "snappy," and there was no drag. This was largely because, under instructions from the chairman, very few papers were permitted to be read, and the "high lights" of each paper were pre-sented orally as an introduction to the large and varied discussions, many of which were prepared in advance. The round table discussion on petroleum engineering research problems, conducted by W. E. Wrather, proved a greater success than was anticipated, considering the difficulty in getting many of the men to discuss such problems. There has been no crystallization of opinion heretofore of what are important engineering research problems, as distinguished from pure science problems, and a digest of the discussion will be made available so as to present the results obtained. It is hoped that further round table discussions, as well as committee work, in the meantime summarizing problems appear-ing in papers published the last two to three years, will enable the oil industry to determine intelligently which of the problems are most important for immediate attack. The roundtable discussion on petroleum engineering educational problems, conducted by H. C. George of the University of Oklahoma, was equally fruitful, and since managers of companies, consulting engineers, and pro-fessors cooperated in these sessions, a cross-section of their opinions on improving the curricula for training the large number of petroleum engineers, which the industry can absorb in-the next few years, was obtained.

Jan 3, 1927

By Charles C. Hall

The following procedure in estimating mineral oil when mixed with vegetable or animal oils, is the result of a long series of cxperiments based on the method suggested by Sir William Thompson and Mr. A. H. Allen, in a paper read before the Royal Society.* Four to five grams of the oil under examination are weighed out into a porcelain capsule of 75 C.C. capacity. Thirty C.C. of a 10 per cent. solution of potassium-hydrate in alcohol are added, and the capsule covered with a watch-glass is placed in a water-bath heated to about 93' C. The mixture of oil and alkali should be stirred frequently, and after three-quarters of an hour it is boiled with stirring. This will secure the complete saponification of all the vegetable or animal oil. After the boiling has been continued some time, and most of the alcohol is expelled and a thick scum of soap forms on the surface, a little bicarbonate of soda is added to convert the excess of caustic alkali into carbonate. When the contents of the capsule have become pasty an equal bulk of fine, clean sand is stirred in. This makes the soap granular, and facilitates the removal of the last traces of alcohol. The capsule is now heated for two hours more on the water-bath. After cooling, the contents of the capsule are transferred to a short-necked funnel, having a thin plug of asbestos, and washed with petroleum-ether, or some other light petroleum spirit. The ether dissolves out the mineral oil from the soap, and is best collected in a quarter-liter flask having a short neck. The ether can be applied conveniently and effectively by a small washbottle. Care must be taken to effect a complete removal of the oil

Jan 1, 1883

By Charles E. Locke

The little stamp-mill in the mining laboratory of the Massachusetts Institute of Technology and the work done by it have been well described by Prof. R. H. Richards and E. E. Bugbee in a paper read at the Albany meeting of the American Institute of Mining Engineers, February, 1903.' As run for student class-work the mill contains a feeder, stamps, plate, and vanner. Results in the past indicate that the work of these machines is just as efficient as that of a regular mill handling the same class of ore. It has been the custom to obtain ore principally from Nova Scotia, mainly because it is the nearest source of supply, and also because there is a considerable saving in freight-cost as compared with other districts. The gold in Nova Scotia ores is notoriously coarse, and for this reason it is almost impossible to obtain satisfactory results by sampling and fire-assay, unless an extremely large lot of ore is crushed and all of the contained gold pellets are saved. A very interesting and most extraordinary example of this fact has been presented by a recent run in the Technology stamp-mill. Since the capacity of the mill is about 60 kg. per hr., and since in about 5-hr. run the students in any one section have an opportunity to make the necessary study of machines, it usually happens that several runs are made from one lot of ore. When the shipment is received it is first dried and weighed, put through the Blake breaker, set at 1 or 1.5 in., and the crushed product is piled in a cone on the sampling-floor. When the crushing is completed the ore is usually stored away in barrels for future use; it is aimed to have each barrel of

Jan 1, 1914

By Caner Zanbak

Deformational behavior of a rock mass can be modeled with a constitutive law based on theories of elasticity, and plastic and viscous deformation. For most rock types, such constitutive models may be used with confidence because there is no geochemical interaction between the rock-forming minerals and water. However, if volume changes in the rock due to geochemical phase transitions are predicted, then these volume changes must be converted into mechanical parameters and must be included into the constitutive laws. In this paper, geochemical phase transitions between anhydrite (CaS04) and gypsum (CaS04-2H20) will be brought to the attention of researchers in rock mechanics. Hydration of anhydrite to gypsum may yield volume increases up to 62.6 percent and dehydration of gypsum to anhydrite may cause volume decreases up to 38.5 percent. If one were to convert the volume increases in hydrating anhydrite into strains and calculates the required stresses to restrict the expansions, the magnitude of stresses will be found at GPa levels. Such stresses on swelling anhydrite layers cannot be provided by geologic media. Therefore, the host rocks will deform under these high stresses. On the other hand, under increasing stresses, geochemical transition of anhydrite to gypsum may stop after some hydration of anhydrite, and anhydrite and gypsum systems may become stable. Changes in temperature and solution compositions in the anhydritel gypsum system also control the stability of the geochemical system, and therefore, the extent of volume changes. A similar conceptual model can be drawn for volume decreases due to dehydration of gypsum to anhydrite. In this case, stress reduction on the gypsum layer may cause extensive fracturing and changes in the state of stress in the host rock mass.

Jan 1, 1984

By C. E. Arnold

A BRIEF description of this installation was included in a recent paper by H. Kenyon Burch.1 The purpose of the present paper is to amplify Mr. Burch's description, as it is felt by the writer that the subject merits more than passing attention. In making a comparison between the common method of hoisting men in mine shafts, and elevator practice in high buildings, the former shows to great disadvantage both as regards safety measures and smoothness of operation. It is surprising that in view of the inducements offered, the step of applying the building equipment direct to the mine shaft has not been taken before, as in many respects the conditions of service are similar, and the objects to be attained are identical. Even without doing this, it is certain that safety to life and limb in the usual method of hoisting men underground can be greatly enhanced by the application to the mine hoist, of some of the features of the building elevator. In the case under consideration, the elevator cage runs in a vertical, concrete-lined shaft compartment 5 ft. 11 in. by 5 ft. 6 in. (1.8 by 1.68:m.) in section and 585 ft. (178 m.) deep, while the counterweight runs in the pipe and ladder compartment of a twin shaft 102 ft. (31 m.) distant. The section of the division of this compartment occupied by the counterweight measures 2 ft. 4 ¼ , in. by 3 ft. 10 ½ in. (0.72 by 1.18 m.), and the counterweight is made in the form of a small cage which. suffices to carry two men for the purpose of making inspections or repairs in the pipe and ladder way.

Jan 12, 1917

[This paper was presented for the author, who is now in the National service, by H. M. Chance, and was illustrated by a working model built to the plans shown in the Bulletin, for February, 1918, p. 268. For more convenient operation, a small motor-driven centrifugal pump was attached to the overflow outlet (5, Fig. 1, p. 267) delivering to the inlet, 4. The pressure of ingoing water was then adjusted by a valve at 4, and was indicated by the column of water in a vertical glass tube connecting with the pressure chamber; an average pressure of 15 in. of water column was maintained during the demonstration. The sand used in the test was beach sand, which had simply been passed through a 20-mesh screen; about 45 per cent. was finer than 80 mesh. The circulation of water was at the rate of about 5 gal. per square foot per minute, and the rising velocity of the water in the box as a whole (not the velocity of the jets) was 6 in. per minute. At this consistency, the specific gravity of the fluid mass was between 1.55 and 1.60. Mr. Chance estimated that it would be possible to maintain a fluid mass of this consistency, 3 ft. deep, and with an area of 50 by 60 ft. with an expenditure of 15-hp. Mr. Chance then showed how a lump of coal would float on the fluid mass, and also made a separation of slate from coal on a small scale in a wire cage submerged momentarily in the fluid. The following demonstration relates to a matter not contained in the original paper, and was presented as of interest to the operators of cyanide and other lixiviation processes dealing with fluid mixtures of varying specific gravity.-Ed.]

Jan 4, 1918

A. H. Bromly, Zihuatanejo, Guerrero, Mexico (communication to the Secretary*):—The following criticism of what "is offered as a summary which may be found useful by mining engineers," is not dictated by any captious spirit, but in the intereet of historical and scientific accuracy. The States of Queretaro and Oaxaca have produced sufficient silver to warrant more extended notice. Referring to Pachuca, State of Hidalgo, the eomewhat loose and inexact statement is made that "the ore-depdsit is an andesite, intermixed with quartz-veins, rich from the surface." A better description mould be,—the ore-deposits consist of quartz-veins in andesite. It is notable that many of the rich shoots worked in recent days did not come to surface. In consequence, Pachuca is often quoted by the ill-informed as a camp in which values improve with depth, the truth being that the veins carry shoots, or clavos, some of which were exposed at surface and some not. The name of " electric plow," applied to the mechanical stirrer of recent use, is certainly not to be recommended. The stirrer, or agitator, consists essentially of a traversing gang-plow, operated by power through shafting; drums, and wire-rope. The fact that in certain plants the motive-power used is electricity does not make it an electric plow. Such a name suggests a machine of which the motor is an essential and integral part; which is not so in this case. A lathe in a factory driven by water-power is not called a hydraulic lathe. My experience agrees with Dr. Raymond's note as to azulapue, which in some districts is also applied to blue copper carbonate. The El Oro, Esperanza, and Mexico mines should be allocated to the State of Mexico; the Dos Estrellas being in Michoacan, as stated. The El Oro quartz certainly does not appeal to me

Jan 1, 1910

Dr. Arthur H. Elliott has been connected with the gas industry for upward of thirty-eight years and was a chemist to whom the industry is deeply indebted for the application of the science of chemistry to its problems and processes. He was born in London, England, in 1851, and was the son-of a physician. While a child he was taken to France, where he received his early education, learning to speak the French language before his native English. His father having destined him for the medical profession, he commenced his studies on his return to England, but his attention being attracted to chemistry, he gave up the study of medicine to pursue that of chemistry. While still a student, he obtained a reputation as an iron and steel analyst, publishing two methods of analysis, one for the determination of sulphur .and the other for the determination of carbon in cast iron. On his graduation from the School of Mines at South Kensington, he left England intending to go to Australia, where an uncle resided, having in mind also the possibility of a trip to China. On his arrival in New York, he met Professor Charles F. Chandler, to whom he had a letter of introduction, and who induced young Elliott to remain. He graduated from Columbia College with the degree of Doctor of Philosophy in 1883. He became demonstrator in chemistry at the College of Pharmacy and afterward professor of chemistry and physics at the same college. He became connected with the Municipal Gas Lighting Co. in May, 1880. In. November, 1.884, when consolidation took place, he became engineer-chemist of the Consolidated Gas Co., which position he held until May, 1910, when he resigned, but was retained as consulting chemist until his death. Recently Columbia University conferred on him the honorary degree of Master of Science.

Jan 7, 1918

THE TRANSACTIONS of the Institute for the early years display but Little interest in physical metallurgy-indeed, it is striking how thoroughly process metallurgy absorbed attention until quite recent years. The first volume carries no article that can be strictly described as physical metallurgy, unless one on the rolling and hammering of ingots be doubtfully so described. Nor does the second volume contribute more the interest then was in mining, and in production methods, both ferrous and nonferrous, with much attention to the new methods of making steel. The third volume records papers on: the condition of carbon in gray and white iron, a paper devoted to chemical rather than microscopic analysis; the annealing of spiegeleisen; phosphorus and carbon in iron and steel, similarly chemical. Much attention was given, and continued to be given for years, to the manufacture and behavior of rails. The question of the nature of steel appeared early (Vol. 11)-What is Steel, by A. L. Holley-where arguments on nomenclature were already active; and Holley also bemoans, in modern spirit, the Inadequate Union of Engineering Science and Art; Pearse wrote on cast iron for guns (reflecting again the ironic beneficence of war in metallurgy), and said that Captain Walbach was the first to insist on chemical analysis of gun irons; he quotes Major Wade's study of comparative hardness, using penetration hardness measurements (Brinell was to come later), and quotes the important Reports on the Strength and Other Properties of Metals for Cannon, by H. C. Baird, Philadelphia, 1855, in which the advanced state of tensile testing at the time is shown. Hewitt, in Vol V, comments upon the function played by technical schools and technical societies upon the growth of metal-

Jan 1, 1948

EVERY English-speaking mining, engineer or geologist knows that some terms used by his profession are not rigid but vary regionally; for example: what is called a vein by some, is called a lode by others and is known as a reef to their Australian colleagues. There are parallels in, the German language. Since, in addition, the meaning of some words may change considerably in 450 years-and other words may disappear completely-and not only the terminology but the concepts of a science are subject to drastic changes over such a long period of time, translating the Bergbüchlein posed some interesting problems. Old German texts and glossaries such as C. T. Delius' Anleitung zu der Bergbaukunst (1773), Minerophilus' Neues and Curieuses Bergwercks-Lexicon (1730), and H. Veith's Deutsches Bergwörterbuch (1871) proved useful sources of information when defini¬tions of obscure terms were needed. The task of translating was made even more challenging by the author's personality. As Ulrich Rülein von Kalbe was primarily a physician, his information must have been mostly secondhand. Since the nomenclature of the miners of Saxony, where he gathered his material on silver ores, undoubtedly varied from that of the German miners in Hungary, for instance, who probably supplied him with data on gold ores, it is not astonishing that he is not consistent in his use of some expressions. To give an example: there is every indication that Flöz and schwebender Gang (see footnote p. 21) are used interchangeably in spite of his occasional disapproval of such usage. It is obvious that he was an educated man with a questing and active mind and, although he apologizes-not wholly sincerely, one might suspect-for the simple

Jan 1, 1949

By P. E. Demmler

PHOSPHORUS combines with copper in various proportions, forming true alloys, some of which are of commercial importance. These materials find wide application as deoxidizers and as a means of introducing phosphorus into other alloys, as in phosphor-bronze. Phosphor-coppers containing 10 and 15 per cent. of phosphorus are the commercial grades that are most generally offered. Each has certain advantages when used in making other alloys. The 10 per cent. grade of phosphor-copper has an advantage over the 15 per cent. in that it has a much lower melting point and can be prepared by certain methods with a much lower loss in phosphorus. The 15 per cent. grade has the advantage of lower freight rates per unit of phosphorus and, by the method to be described, a uniform product can be prepared with practically no loss of phosphorus. Alloys of copper and phosphorus containing any desired percentage of phosphorus lower than 15 per cent. can be prepared by melting together the requisite amounts of copper and 15 per cent. phosphor-copper. Processes for making phosphor-copper may be divided into two classes as follows: (1) Those depending on the smelting of phosphate rock or superphosphate of calcium with copper or copper-bearing materials, and coal or other carbonaceous material; (2) those depending on the direct combination of metallic copper and elemental phosphorus. A number of formulas for preparing phosphor-copper according to the first method have been published. The Metal, Industry' gives-the following: Superphosphate of calcium, 60 lb.; granulated copper, 301b.; finely powdered coal, 10 lb. Similar formulas are given by Brannt2 and others, and detail 'variations are covered by patents, such as those of L A Jeffs3 and H A Webster.4

Jan 8, 1920

By R. S. Dean

The careful work of Gross and Zimmerleyl has established the fact that the energy actually used in grinding is proportional to the new surface produced. This confirmation of Rittinger's law was made by crushing quartz in a frictionless drop-weight machine and determining the surface of the quartz by its rate of solution in hydrofluoric acid. The details of this procedure have been described adequately elsewhere and need not be repeated here. The resultant data furnish the only available basis for comparing accurately the efficiency of grinding machines. This method is so cumbersome experimentally that it has been little used. As an alternative all sorts of approximations have been proposed. The best of these is complete size analysis by sieving and elutria-tion. Such procedure is very lengthy and difficult to carry out accurately. Furthermore, any sizing method becomes very inaccurate for determining surface with very fine sizes where the ratio of surface to volume becomes very large. To avoid the lengthy and difficult technique of elutriation it has been proposed to estimate the size distribution below 200 mesh from various probability formulas. Such a procedure is at best an engineering approximation; at worst it is a mere guess. Some time ago Dr. V. H. Gottschalk2 found that the coercive forces of magnetite powders were directly proportional to the surface area, regardless of size distribution. It was at once apparent that this furnished a method for determining grinding efficiency quickly and accurately. The only requirement was a single determination of the relation between the work input of the Gross-Zimmerley drop-weight machine and the coercive force of the resultant crushed magnetite. For this purpose Ural Mountain magnetite in definite octahedra was

Jan 1, 1939

By R. S. Dean

The careful work of Gross and Zimmerleyl has established the fact that the energy actually used in grinding is proportional to the new surface produced. This confirmation of Rittinger's law was made by crushing quartz in a frictionless drop-weight machine and determining the surface of the quartz by its rate of solution in hydrofluoric acid. The details of this procedure have been described adequately elsewhere and need not be repeated here. The resultant data furnish the only available basis for comparing accurately the efficiency of grinding machines. This method is so cumbersome experimentally that it has been little used. As an alternative all sorts of approximations have been proposed. The best of these is complete size analysis by sieving and elutria-tion. Such procedure is very lengthy and difficult to carry out accurately. Furthermore, any sizing method becomes very inaccurate for determining surface with very fine sizes where the ratio of surface to volume becomes very large. To avoid the lengthy and difficult technique of elutriation it has been proposed to estimate the size distribution below 200 mesh from various probability formulas. Such a procedure is at best an engineering approximation; at worst it is a mere guess. Some time ago Dr. V. H. Gottschalk2 found that the coercive forces of magnetite powders were directly proportional to the surface area, regardless of size distribution. It was at once apparent that this furnished a method for determining grinding efficiency quickly and accurately. The only requirement was a single determination of the relation between the work input of the Gross-Zimmerley drop-weight machine and the coercive force of the resultant crushed magnetite. For this purpose Ural Mountain magnetite in definite octahedra was

Jan 1, 1939

W. H. LINNEY, Chairman, OSCAR LACHMUND, Vice-Chairman LYNDON K. ARMSTRONG, Secretary-Treasurer, P. O. Drawer 2154; Spokane, Wash. STANLY A. EASTON, S. SHEDD. Mining camps from Mexico to Alaska and from the Pacific coast to the Atlantic were represented by delegates at the 5th Annual Northwest Mining Convention which was held in Spokane, Wash., Feb. 19-24, 1917. About 300 delegates from outlying regions were present, this being fully 100 more than have been counted at any previous mining convention in Spokane. Graham B. Dennis, president of the Northwest Mining Association, made the address of welcome. In part, he said: "Heaven has made us the possessors of an area great enough for an empire, varied enough in climate and possibilities to compass the whole complex field of modern industry. In the development of this broad heritage, we are not only actors for today, but trustees for future ages. "It is to foster this spirit of unity; to create and maintain strong bonds of mutual good will and confidence, that we founded the Northwest Mining Association. Wee support it because we believe it will give us strength; because we believe we shall learn from each other; because, in industry as in every other walk of life, personal contact and establishment of ties of friendship enrich and round out the characters of men." One of the interesting lectures of the week was that on "Alaskan and Russian Gravel Mining," by Dr.' Henry Mace Payne, consulting engineer for the Russian government and Consolidated Goldfields of South Africa. Dr. Payne's illustrations showed the different appliances in use in the countries mentioned. The Resolutions Committee reported back to the Convention six of the seven resolutions that had been presented to it. These were adopted as submitted, with some minor changes.

Jan 5, 1917

By W. D. Donnelly, M. L. Rudee

THE crystallography and morphology of ?-Al3Fe precipitates in an A1 + 0.5 wt pct Fe alloy have been studied by transmission electron microscopy. The alloy was cast in cylindrical ingots, 15 cm in diameter and 60 cm in length, and cooled slowly. The measured composition was 0.527 wt pct Fe, 0.001 wt pct Mg, and 0.003 wt pct Cu. Spectrographic analysis revealed no additional trace impurities. Thin slices were cut from the ingot and reduced by more than 95 pct by rolling to a thickness of 0.1 mm with no intermediate annealing treatments. These thin sheets were then vacuum-annealed for 1 hr at 612°C and air-cooled in their capsules. Thin foils for examination in the electron microscope were prepared by electropolishing. The precipitate is found in the form of oval platelets on the (110) planes of the matrix. The major axes of the platelets are parallel to the (110) directions of the matrix, and vary in length from 1/2 to 2 p. The thickness is about 1/10 µ. Examples of platelets, both in the plane of the foil and normal to the foil, are shown in Figs. l(a) and l(b), respectively. lack' found that ?-A13Fe (more correctly Al13Fe4) belongs to the monoclinic system. Using Black's structural data and simultaneous electron-diffraction patterns from the matrix and precipitates, the habit planes and directions were determined to be: (001)? 1 (110)Al [100]?|| H [001]Al The orthogonal crystallographic axes of the precipitates are accurately in the habit plane, while the measured coincidences of the directions are only within 10 deg. The major axis of the platelet is parallel to [010] in the 0. This orientation corresponds to the direction of nearest registry of the lattices.

Jan 1, 1964

By M. Nicholas, D. M. Poole

The diameters of sessile drops have been found to increase linearly with time in five reacting binary metal systems. The spreading rates of the drops are markedly dependent on temperature and on prior alloying of the solid with the lower melting point metal, hut are independent of the drop volume, wetting atruosphere , solid-surface roughness, and prior alloying of the drop with the substrate metal. A mechanism has been suggested that relates the linear-spreading rate to lateral diffusion of the liquid-metal atoms into the solid at the drop edge. An Arrhenius- type equation has been derived that describes the temperature dependence 0) the spreading rate, and although the agreement between the actual and the predicted pre-exponen-tial terms is poor that between the activation energies is excellent and the variation in the spreading rate of copper on Ni-Cu alloys produced by different extents of alloying can be predicted with considerable accuracy. CHEMICAL interactions frequently change the wetting behavior of solid-liquid systems causing, for example, "secondary spreading1 of sessile drops beyond the size defined by the surface and interfacial tensions of the unreacted components. The kinetics of the contact-angle decreases associated with this spreading are similar for many systems, but few studies have been made with the objective of determining whether the similarities are a reflection of a common mechanism. Some workers2,3 have assumed the secondary spreading is controlled by changes in the liquid surface and liquid-solid interfacial tensions and hence by the composition of the liquid, and contact-angle changes measured by the vertical-plate technique have been used to follow the course of liquid-solid chemical reactions.4 Other processes that have been invoked to explain these time-dependent changes in specific systems include the removal of adsorbed gas from the liquid-solid interface.5 penetration of containment layers on the solid Surface,6 interdiffusion,1,7 reori-entation of the solid surface into a wettable configuration: vapor-phase transport of the liquid onto the solid in advance of the drop,9 and, from vertical-plate studies. capillary flow between oxide layers and the solid surface.10 One of the reasons for the profuseness of these suggestions may be the complexity of the contact-angle change kinetics. However, in an analysis of secondary spreading gold and copper on UC,11 it was found that the diameter of the contact area between the sessile drop and the solid surface showed a simple linear increase with time although contact-angle changes were more complex. To check whether the linearity was merely fortuitous! additional exploratory work was conducted with four reacting metal-metal systems: Au on Ni. Cu on Ni, Cu on Fe, and Ag on Au. Linear spreading was observed in every case even though the kinetics of the contact-angle changes were complex. A further detailed study of the kinetics of linear spreading of five reacting metal-metal systems has been made with the object of determining the mechanism involved. The influence of variables such as temperature, drop volume. and the initial composition of the drop on the linear-spreading rate has been measured and compared with those predicted by a number of possible mechanisms. The systems employed in this study (Cu and Au on Ni and Pt, and Ag on Au) were selected because of the availability of potentially relevant chemical and physical property data. the simplicity of their phase diagrams at the wetting temperatures, and the ease of experimentation. EXPERIMENTAL TECHNIQUES The purities of the metals used in the study were: copper, 99.9 pct; gold. 99.96 pct; nickel, 99.2 pct; platinum 99.99 pct; and silver, 99.999 pct. The wetting tests were performed in a split tantalum tube vacuum resistance furnace of a conventional design. The furnace element was held vertically and was 1 $ in. in diam and 6 in, long. Viewing ports were provided in the water-cooled chamber to enable the specimens to be observed in both the horizontal and vertical planes. The temperature in the hot zone of the furnace could be held at 1500" i 5°C for an indefinite time. The surfaces of the solid-plaque metals were ground flat on Microcut paper and both the sessile drop and substrate metals were ultrasonically cleaned in methyl alcohol prior to their insertion in the furnace. After loading, the furnace was pumped down to a pressure of 2 x 10-5 mm of mercury and degassed for 30 min at 900° to 950°C. The temperature was then increased at more than 100°C per min to that used in the wetting test. The vacuum at the wetting temperature was better than 5 x 10-5 mm of mercury. Dewetting and retraction of the drop on cooling did not occur and the contact-area diameters, therefore, were measured after solidification with a vernier traveling microscope. The diameters quoted later are arithmetic means of ten measurements. The standard error of the mean never exceeded 3 pct and was often less than 1 pct.

Jan 1, 1967

By L. C. Michels, O. G. Ricketts

The disorientations between s?nall grains, whose growth has been arrested at an early stage of recrys-tallization, and the deformed matrix in cold-rolled aluminum single crystals were determined using transmission Kikuchi line and electron diffraction patterns. The orientations of the recrystallized grains were found to be random, and the disorientations of these grains with the matrix weve found to be intermediate to large. This leads to the conclusion that the observed vecrystallization began in small areas of large disorientation present in the cold-worked structure. heavily cold-worked thin sections of aluminunz single crystals and of polycrystalline aluminum and nickel were produced directly by a mechanical technique. The specinlens thus prepared were heated with the electron beam to bring about vecrystallization during observation in the electron microscope. Motion pictures taken du.ring heating and the electvon, microg.raphs taken both before and aftev heating allowed the recrystallization process to be traced to its ovigin. Re cvystallized grains originated in very s,mall regions of the cold-worked structure and developed through rapid migration of high-angle boundaries. The boundaries either were present as such in the matrix or were formed out of dense dislocation networks. SIGNIFICANT advances have been made in recent years in the study of nucleation of recrystallization using the technique of transmission electron microscopy of thin metal foils. Bollman1 in a study of heavily rolled polycrystalline nickel found support for the Cahn-Cottrell2,3 theory of nucleation. According to this theory nuclei form by the initially slow growth of subgrains formed through polygonization. During this initial period of slow growth (the incubation period) the migrating boundary of the subgrain increases its disorientation with the cold-worked matrix and thereby increases its mobility to become a rapidly migrating high-angle boundary. Bailey4,5 investigated the annealing behavior of several metals deformed both in tension and by rolling and concluded that recrystallization took place through the migration of high-angle boundaries. With low deformations these boundaries were present in the metal before deformation. With high deformation it was not possible to tell whether the boundaries were pieces of the original grain boundaries or were produced either during deformation or by polygonization during ameal- ing. Direct observation during heating of metal foils indicated that subgrains form by polygonization and grow at an uneven rate. The grain size obtained decreased with decreasing foil thickness indicating that the foil surface resists boundary motion. Votava,6 in heating stage experiments on rolled copper, observed nuclei to appear suddenly and grow in jumps of differing magnitude. However, he found no special dislocation configurations where the nuclei appeared. Fujita,7 as a result of a study of subgrain growth in heavily worked aluminum, concluded that the boundary of a recrystallized grain initially forms from the boundary of a group of subgrains. This occurred by a process of deposition of vacancies and dislocations in the group boundary as the boundaries within the group disappear. HU8,9 directly observed a similar process in heating stage experiments on 70 pct rolled Si-Fe single crystals. The growth of subgrains appeared to proceed by a coalescence mechanism. The observed fading away of the boundary between two subgrains was explained by the moving out of dislocations from the disappearing boundary into the connecting or intersecting boundaries around the subgrains. The subgrain size and degree of disorientation with the surrounding structure were thus increased. With the increase in disorientation occurred a corresponding increase in boundary mobility, which eventually allowed the boundary to migrate rapidly. This process was observed to occur within "microbands" consisting of parallel narrow segments disoriented by a few degrees present in the as-rolled structure. The conclusion of Rzepski and Montuelle10 that growth is preceded by the coalescence of blocks through disappearance of their common boundaries supports this view. In contrast to Hu's coalescence model for nucleation were the conclusions of Walter and ~och.""~ Working with the same material as Hu, of the same orientation and rolled to the same reduction, they concluded that nucleation occurred by the Cahn-Cottrell mechanism. They observed, in agreement with Hu, that recrystallization began in the "microband" regions which they referred to as "transition" bands. Bartuska13 studied subgrain growth in heavily rolled nickel using a beam heating method in the electron microscope. He concluded that nuclei for recrystallization form from the largest most perfect subgrains present in the cold-worked structure by rapid intermittent migration of parts of subboundaries. In rare instances he observed subgrain growth by coalescence. EXPERIMENTAL PROCEDURE The materials used in this study were 99.999 pct A1 supplied by A.I.A.G. Metals, Inc., and 99.999 pct Ni supplied by Johnson and Matthey and Co., Ltd. The Hitachi HU-11 electron microscope, with uniaxial

Jan 1, 1968

By Joachim J. Hauser

Experiments on latent hardening were peyformed by compressing single crystals along a direction perpendicular to the tension axis. The slope and length of easy glide in the tension test were found to depend only on prior deformation in the same slip plane. Prior deformation on a different slip plane changes the stress level of the resulting stress-strain curve. The yield points appearing upon reloading after prior extension and unloading were related to the end of easy glide. SEVERAL researchers have studied the latent hardening due to deformation of a crystal by slip on a slip System after prior deformation. These experiments can be divided into those in which the prior deformation was on the same plane as the subsequent and those in which the two deformation processes were in different planes. In the former category are the experiments of Buckley and Entwistle,1 Parker and washburn,2 and Haasen and Kelly.3 The latter case has not been studied systematically; it was the main purpose of this investigation to produce this type of latent hardening and explain the results in terms of the existing theories of work hardening. In general, tension producing slip on a certain slip system can be preceded by tension, transverse compression or longitudinal compression, each with predictable dislocation movement and intersection. The intersection of dislocations can lead to glissile or sessile jogs, Cottrell-Lomer locks and other sessile dislocations. The effect on the stress-strain curve could depend on which combination of the former mechanisms is operating. Haasen and Kelly3 have studied the yield points which occur in aluminum and nickel single crystals upon reloading after prior unloading in a tension experiment. They attributed this effect to the anchoring of dislocations occurring during unloading. As Cottrell and stokes4 have shown that dislocations cutting through the "forest" could only lead to reversible changes, they attributed the anchoring to the formation of sessile dislocations during unloading. However, different kinds of sessile dislocations could be formed during unloading, and it was the purpose of this experiment to determine whether Cottrell-Lomer locks are responsible for the yield effect and for the end of easy glide. The case where a longitudinal compression is followed by tension along the same axis is commonly referred to as a Bauschinger test. This type of effect was studied by Buckley and Entwistle1 on aluminum single crystals and by Parker and washburn2 on zinc single crystals. In such a test, the tension and the compression activate the same slip plane with opposite slip directions. The use of sideways compression in the present experiments permits the activation of different types of slip systems and the study of their effect on the easy glide region and on the transition between the elastic and easy glide region. The theory of seeger5 for the flow stress in fee materials is applied to explain the latent hardening. EXPERTMENTAL PROCEDURE All the single crystals used in this investigation had an axial orientation close to <210>, called the "0.5" orientation. This is the orientation for which the tensile axis is 45 deg from both the slip plane and the slip direction. The single crystals were grown from the melt under a helium atmosphere using milled graphite boats,=at a rate of 8.6 mm per min. The silver used in the experiment was 99.98 pct pure. The single crystals had a square cross section about 0.9 by 0.9 cm and a length of 14 cm. The orientation of the specimen was determined within ±2 deg by the Laue back-reflection method. The specimens were annealed at 940&apos; ± 2°C in a helium atmosphere for 24 hr and then furnace cooled over a period of 7 hr. The specimens were electropolished in a solution of 9 pct KCN in water. The specimens were tested in a soft-type tensile machine (the load is prescribed) up to 3 pct strain. The stress was increased continuously at approximately 30 g per mm2 per min. The strain was measured over a 5 cm gage length with a mechanical extensometer employing an optical lever. The strain and stress were measured with accuracies of i 2 X 10-5 and ± 2 g per mm2, respectively. The remainder of the stress-strain curve up to 20 pct strain was obtained in a hard-type tensile machine (the strain rate is prescribed). The strain and the stress were measured in that machine with an accuracy of ±2 pct. The compression tests were performed in the hard-type machine using accurately machined steel blocks without lubrication. The blocks were used so as to apply a uniform compression over a length of 13 cm. The strains were measured on the hard-type machine and with a micrometer.

Jan 1, 1962