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By D. A. Dukelow, K. Li, G. C. Smith

Decarburization in the Fe-C system by oxygen top blowing has been studied in laboratory -scale experiments. It is shown that equilibrium models fail to explain or predict either the course of refining or endpoint conditions, giving results which either are incompatible with the chemistry of the system or do not satisfy material balance requirements. Also the path of decarburization was found to vary even for heats made under apparently identica1 conditions. A promising approach to analyzing the decarburization results is to relate oxygen efficiency fm carbon removal to bath carbon content. This relationship for Fe-C heats shows the same range of oxygen efficiencies as is obtained in pilot-plant and commercial heats using hot metal-scrap charges. This implies that oxygen transfer is primarily controlled by the decarburization reaction itself, independent of other refining reactions. Therefore, it should be possible to study separately decarburization and slag-metal reactions. DECARBURIZATION is probably the most important reaction in steelmaking. Not only is it a main reaction in the refining of iron to steel but it also provides the stirring action in the bath necessary for the diffusion processes to proceed at reasonable rates so as to make a steelmaking process practical. Kinetics of decarburization in the open-hearth process has been a subject of investigation for many years.&apos;-B It is generally accepted that at steelmaking temperatures the rate of homogeneous C-0 reaction is extremely high and cannot constitute a rate-controlling step. Diffusion of oxygen through a boundary film in the metal phase has been suggested by arken&apos; as rate-determining. Recently, Larsen and sordah16 concluded from experiments in a laboratory furnace that, with oxygen supplied from air or combustion gases, the rate of "steady-state" carbon boil is controlled essentially by a diffusion process of O2, Co2, or H2O through a film of nitrogen above the slag surface. Displacing this diffusion film by a stream of nearly pure oxygen produced a ten-fold increase in the rate of carbon boil with the rates of slag-metal oxygen transfer, bubble nucle-ation, and other steps all apparently able to keep pace. In the top-blown basic oxygen process, however, the transport of oxygen takes a more direct route. and the state of bath agitation is much more turbulent than in the open-hearth process. In addition, direct contact of the gas with the metal phase provides opportunity for direct oxidation of carbon. It is likely that the rate-limiting factor for the decarburization reaction will be different. However, only a few descriptive discussions of the subject have been reported in the literature.10-l2 Studies of the decarburization kinetics based on plant or pilot-plant data are necessarily complicated and are influenced by other refining reactions which occur simultaneously. In order to investigate the mechanism of decarburization, experiments have been conducted in which carbon-saturated iron melts were top-blown with pure oxygen over a range of conditions. It is hoped that this study will form a foundation on which a more basic understanding of this important reaction may be built. EXPERIMENTS One group of blowing experiments was made in a standard 200-lb induction furnace and another group in a 500-lb induction furnace. The furnaces were modified to the general shape of a basic oxygen furnace by adding a rammed refractory cone section to the regular crucible body. Crucible and cone were of high MgO (95 pct) material. A water-cooled lance, 1/2 in. in diam and threaded at one end to take a nozzle, was used for blowing oxygen. The lance with its water and oxygen lines was supported on a cantilever arrangement so that it could be moved up, down, or sideways. Oxygen of 99.5 pct purity was supplied from a cylinder and metered through a rotameter equipped with pressure and temperature gages. Another pressure gage was located at the top of the lance. A schematic diagram of the assembly is shown in Fig. 1. Before each experiment, a weighed amount of ingot iron, containing 0.02 pct C, < 0.01 pct Si, 0.10 pct Mn, 0.019 pct P, and 0.015 pct S, was charged in the furnace and melted down by induction heating. Graphite was then added to the molten charge until it became saturated. When the temperature of the charge reached the desired level, the lance was lowered to a predetermined height above the bath

Jan 1, 1964

By W. J. Rogers, L. J. Dwiggins, R. O. Williams

THERE has been comparatively little work on the importance of strain rate and temperature as variables in the formation of deformation textures. For this reason the present work was started, the choice of compression being in part that of convenience and in part because of the absence of quantitative data in this area. These do not turn out to be important variables within the range studied which permits the results to be condensed into this note. Samples 1/4 in. in diam and 1/2 in. long were machined from 99.9 pct pure commercial aluminum and recrystallized to a fine grain size. A set of five samples were deformed between a spring-driven weight and an anvil resulting in roughly 20 pct strain each time. The strain rate varied because of decle-ration and shortening of the sample but would average about 10&apos; per min. Deformation at temperatures over the range of -76" to 150°C were obtained by heating or cooling the samples. Complete lubrication could be obtained by oil since the short time of contact did not permit its escape. The samples were compressed to a total true strain of 1.4 to 1.6. A larger sample was prepared similarly with spiral grooves in the ends to hold paraffin which provided essentially complete lubrication. This sam ple was compressed slowly at room temperature at a rate of about 2 per min to a total strain of 1.0. Cylindrical samples were carefully machined from these discs with a radial direction as an axis. They came from the center half of the samples and were roughly 1/16 in. in diam. The samples were etched down 15 pct to remove any surface effects. Diffraction data were then obtained for six different kinds of planes by the use of the Norton technique as applied to a fiber texture. Direct comparison between the raw data failed to reveal any significant difference between any of the samples and consequently the data from only one sample was completely reduced. The particular sample had been deformed at O°C The background was subtracted from the intensity data which were averaged over the four quadrants and then normalized to random. These data were then used to obtain fiber-axis distribution charts as previously described.2 For this sample the (422) plane was also run to assist in this inversion. The final result, Fig. 1, provided a comparable fit to that previously obtained from fiber data. About 85 pct of the material forms an elliptical texture around the <110> direction. The radius (at half height) is 5.5 deg along the (111) boundary and 8 deg along the (100) boundary. The remaining 15 pct forms a ridge running from this texture to near the <311> direction. The regions around the (100) and (111) planes are devoid of material. The earlier qualitative results of ~arrett~ are in complete agreement with the present results. The possibility has been dis-cused that the material around the <311> results from friction between the sample and compression plates.4 The present results are considered proof that such is not the case because of the uniformity of sample deformation and the requirement of axial symmetry before fiber-axis distribution charts can be accurately obtained. Recently results have been obtained to show that strain rate and temperature are important variables in the extrusion of aluminum.5 Perhaps the most important observation was that the partial recrystal-lization occurred even at room temperature. Strain rate was considered to be a factor only in that it produced a temperature change. There are many differences between the two experiments, the most important possibly being that their material was roughly ten times the purity of the present material. The present experiment, however, may not be as definitive as desired in this respect since it has been shown that compressed aluminum recrystallizes without a texture change6 although supplementary

Jan 1, 1961

By Samuel Taylor

IT is customary for the president of an engineering society, in his annual address, to describe either some engineering problem with which he has beer connected or to review the work of the society during his administration. My first thought, this being the sesquicentennial year of our nation, was to review the advance in coal mining for the past fifty years, during which period I have been more or less intimately con-nected with the bituminous coal industry, and have personally witnessed most of the great changes which have occurred in methods and machinery used in the production of coal, but preparation of the requisite address would take more time than could be spared to prepare it, and its presentation would consume so much time that it .would not be suitable. The new arrangement providing for giving the presi-dent&apos;s address at the business meeting makes it more .appropriate to review the work of the Institute during the past year, together with some suggestions which appeal to me as being of advantage to the future wel-fare of the Institute, which I will try to do briefly. The work of the business office has been reviewed in the Secretary&apos;s report and it will not be necessary for me to dwell on it. Suffice it to say, it seems to be going along very well. Additional work could be done which would be to the advantage of the Institute, if we had the money with which to defray the necessary ex-pense incident to it, but I will refer to this again later. I would be derelict if I did not refer to the splendid work of the Secretary and the Assistant Secretary. Keeping in touch with all the sections, which number now about 26, and affiliated student societies which number 40, besides special committees, and represent-ing the Institute on various boards, provides work enough to occupy the Secretary&apos;s time almost exclu-sively. In addition to this the Secretary and the As-sistant Secretary have the work of editing and publishing the TRANSACTIONS of the Institute; the issuing of the magazine, MINING AND METALLURGY, in the splendid manner in which it goes out to the mem-bership is no light task and I think they should receive the commendation of the membership for this work.

Jan 3, 1927

By Paul Queneau

FEW of us who waded ashore on the Norman beaches realized the importance of coal to a successful invasion. General Eisenhower and his staff had been aware of the essential need for coal and an able Solid Fuels Section had been set up under the direction of Colonel Robert P. Koenig, of Indiana. This organization met the requirements of the invading armies on their march to the Rhine. East of the Siegfried Line enemy territory, the Army Engineers were called upon for assistance. When the Engineers were advised that, in addition to their normal duties, they were to occupy and place in operation the coal mines in the Twelfth Army group area, plans were drawn up overnight and action was initiated immediately. The Sixth Engineer Special Brigade, a versatile outfit which made a notable record D-Day on Omaha Beach, was selected to handle the operation. Within 48 hours of the new assignment an advance command post was set up cm the west bank of the Rhine at Homberg, just below German-held Duisburg. The 368th Engineer General Service Regiment was assigned to the Brigade, and the British 44th Pioneer Group, including specialist personnel, was also attached. This large British unit was added because most of the mines would shortly come within the British zone of

Jan 1, 1946

1944 WALTER HULL ALDRIDGE New York, N Y 1946 PETER M ANDERSON Johannesburg, South Africa 1946 CHARLES CAMSELL Ottawa, Ont, Canada 1946 CHARLES AUGUSTUS CARLOW Fife, Scotland 1949 ERLE V DAVELER New York, N. Y 1951 EVERETTE LEE DEGOLYER Dallas, Texas 1946 CECIL H DESCH London, England 1946 WILLIAM FRASER London, England 1917 HERBERT HOOVER New York, N. Y 1941 DANIEL COWAN JACKLING San Francisco, Calif. 1950 ZAY JEFFRIES Pittsfield, Mass 1939 HENRY KRUMB New York, N Y 1942 ESSINGTON LEWIS Melbourne, Vic, Australia 1944 WALTER C. MENDENHALL Washington, D. C 1942 PAUL DYER MERICA New York, N Y 1938 A M PORTEVIN Paris, France 1934 T A RICKARD Victoria, B C, Canada 1946 JOHN R SUMAN Houston, Texas 1946 WONG WEN-HAO Chungking, China

Jan 1, 1952

By S. F. Shaw

IT IS generally recognized that the natural gas absorbed in petroleum plays the leading r6le in moving the oil through the sands to the well and supplies the energy that delivers the oil to the surface when the wells are flowing. It is the purpose of this paper to note the amount of oil that could be lifted by this gas if 100 per cent. efficiency were obtained and the efficiencies actually obtained in the use of this gas. An article in MINING AND METALLURGY,&apos; stated that in a Wyoming field, with a pressure of 300 lb. per sq. in., there would be absorbed 65 cu. ft. of gas per barrel, or 1.55 cu. ft. per gal. of oil. The writer does not know if data have been obtained, by experiment, for pressures beyond those indicated in this article, therefore, for the purpose of illustration, he has projected this curve to obtain figures for pressures greater than 300 lb., although probably experiment will show that the extended line is not quite correct.

Jan 1, 1926

By Alexander Deussen

The figures listed in a table for Gulf Coast fields given by L. P. Teas1 in 1934 are so greatly at variance with results that I have obtained from a serious study of this subject over a number of years, that I am disposed to challenge the correctness of Mr. Teas&apos; figures as an accurate representation of acre-foot yields of Gulf Coast fields, and as regards at least two of the fields listed by Mr. Teas I desire to "put into the record" some figures that, according to my study, are more nearly in accord with what I conceive to be the actual facts. Upon investigation I find that Mr. Teas&apos; figures, inadvertently no doubt, arc not what they purport to be. Apparently the figures were arrived at by considering as thickness of the producing formation the net thickness of producing rock corresponding "to the total of the net portions of the producing zones which actually yield oil into the drill hole"—and in following this method I am under the impression that Mr. Teas was acting under instructions of the Institute in the preparation of this paper, in order to get comparable figures from the several fields of the United States. Apparently the author interpreted these instructions to mean that in the absence of cored thicknesses of producing horizons the actual number of feet of screen set in the various producing zones was to be taken as the basis for arriving at the thickness of these zones and the "acre-foot" yields. It is obvious that in many instances only 20 ft. of screen, or even 10 ft. of screen, might be set in a well, when there might be actually 100 ft. of oil sand present. In the early operations in the Gulf Coast it was usual to set much less screen than the amount of sand. It follows that the "acre-foot yields" so arrived at would be much greater than those found by using the full amount of sand. In Mr. Teas&apos; table, it was indicated that up to the end of 1933 "acre-foot" yields had been obtained in the several fields as listed in Table 1. A casual inspection of these yields will show that certainly they do not properly reflect the amount of oil produced from an acre-foot of the

Jan 1, 1936

By Alexander Deussen

The figures listed in a table for Gulf Coast fields given by L. P. Teas1 in 1934 are so greatly at variance with results that I have obtained from a serious study of this subject over a number of years, that I am disposed to challenge the correctness of Mr. Teas&apos; figures as an accurate representation of acre-foot yields of Gulf Coast fields, and as regards at least two of the fields listed by Mr. Teas I desire to "put into the record" some figures that, according to my study, are more nearly in accord with what I conceive to be the actual facts. Upon investigation I find that Mr. Teas&apos; figures, inadvertently no doubt, arc not what they purport to be. Apparently the figures were arrived at by considering as thickness of the producing formation the net thickness of producing rock corresponding "to the total of the net portions of the producing zones which actually yield oil into the drill hole"—and in following this method I am under the impression that Mr. Teas was acting under instructions of the Institute in the preparation of this paper, in order to get comparable figures from the several fields of the United States. Apparently the author interpreted these instructions to mean that in the absence of cored thicknesses of producing horizons the actual number of feet of screen set in the various producing zones was to be taken as the basis for arriving at the thickness of these zones and the "acre-foot" yields. It is obvious that in many instances only 20 ft. of screen, or even 10 ft. of screen, might be set in a well, when there might be actually 100 ft. of oil sand present. In the early operations in the Gulf Coast it was usual to set much less screen than the amount of sand. It follows that the "acre-foot yields" so arrived at would be much greater than those found by using the full amount of sand. In Mr. Teas&apos; table, it was indicated that up to the end of 1933 "acre-foot" yields had been obtained in the several fields as listed in Table 1. A casual inspection of these yields will show that certainly they do not properly reflect the amount of oil produced from an acre-foot of the

Jan 1, 1936

By Pol Duwez, Paul Pietrokowsky

The crystal structure of the compound TisGeS has been determined from X-ray powder diffraction data. Related silicon and tin compounds have been found to be isomorphous. Unit cell dimensions, axial ratios, and parameters for equivalent atomic positions are given. THERE is, at present, only meager information pertaining to the solid state reactions of titanium with the elements in group 4B of the periodic table (silicon, germanium, tin, and lead). The only two compounds whose crystal structure has been established are TiSi² and TiGe² (references 1 and 2 respectively). These two compounds are isomor-phous and have an orthorhombic symmetry D242h— Fddd. The titanium-rich regions of the constitution diagrams of titanium-silicon, titanium-tin, and titanium-lead have been investigated by Craighead et al.³ While valuable information concerning the alpha solid solubility of these three elements in titanium was obtained, no light was shed on the existence or nature of the titanium-rich compound in these systems. The present study is concerned with the crystal structure of the intermediate phases Ti5Si ?, Ti³Ge³, and Ti5Sn³, which were found to be isostructural. The alloys were prepared by mixing the pure metal powders in the desired proportions, pressing the mixture into pellets, and melting them in an electric arc furnace in the presence of a helium atmosphere.& After melting, the specimens, weighing approximately 5 g, were sealed in evacuated quartz vials, homogenized at 1038°C for three days, and quenched from that temperature. Powder diffraction patterns were made with a 143.2 mm diam Debye-Scherrer X-ray camera in which the Ievins and Straumanis film arrangement was utilized. Filtered copper radiation was used throughout the entire investigation. A study of the powder patterns of a series of alloys of various compositions indicated the presence of a compound around a composition corresponding approximately to a ratio of 3 titanium to 2 silicon, germanium, or tin. From a visual examination of the diffraction patterns, it was evident that the silicon and germanium alloys were iso- morphous. For small angle reflections, the powder pattern of the tin compound was analogous to that of the silicon and germanium compounds, but after the first ten reflections, the similarity was no longer clear. The powder pattern of the germanium compound was selected for indexing, since it exhibited a weak small angle reflection and clearly resolved doublets in the back-reflection range. Good agreement between observed and calculated values of (1/d)² was found by indexing the pattern on the basis of hexagonal symmetry. For the hexagonal system:

Jan 1, 1952

By R. J. Woody

Design of the most economic continuous counter-current decantation (CCD) circuit is based on selection of the number of stages and the wash volume that will give the minimum summation of the following items: 1) Capital and operating costs of the CCD circuit. 2) Capital and operating costs of the precipitation circuit. 3) Value of the dissolved product lost.

Jan 1, 1959

By J. B. Cohen

In an investigation of the microstructure of shock-loaded metal specimens1 C. S. Smith found that there was little distortion of grain boundaries or change in external dimensions, although the hardness corresponded to that produced by severe rolling. Furthermore, the hardness of individual grains was independent of the deformation structures present; grains with no markings were as hard as those heavily populated with markings. These markings which resemble twins do not appear in copper until high shock-loads of the order of 200 kb are applied. It appears that due to the high velocity of a shock wave and its sharp front, heavy deformation takes place on a submicroscopic scale. In this work an attempt was made to examine this deformation, particularly at a load below which macroecopic markings appear. The broadening of 200 and 400 diffraction peaks was examined from the face of a poly crystalline sample normal to the direction of the shock wave. These peaks were chosen because the elastic constants in copper are such that residual strains would be greatest in the <100> directions; hence, the strain-broadening contribution to these peaks would be large in comparison to other sets. Also the broadening due to stacking faults and microtwins would be greatest with this set.2 A complete Fourier analysis of these peaks was made, as described by warren,&apos; using the Stokes correction with peaks from an annealed sample.3 With the aid of the U. S. Army Ordnance Corps EDVAC computer and a curve matching program, sixty sine and sixty cosine coefficients were obtained for each peak. The last of these was about 1.5 pct or less of the largest coefficient, indicating good representation. Transverse sections from a 1.5 in. rod of as-drawn electrolytic tough-pitch copper were reduced in cross-sectional area about 50 pct by cross rolling. Disks 1.5 in. in diam were recrystallized at 275 °C for 30 min and then at 300°C for the same time. The faces were polished and deeply etched in nitric acid to remove 25 mils. The grain size was 0.02 mm. Laue back-reflection patterns indicated the sample was well recrystallized. The two diffraction peaks from this sample were recorded on a Norelco diffractometer using filtered copper radiation. Peak intensities were kept less than 600 cps to assure linearity of the counter and circuitry. This sample was then placed between two rods of the same material and diameter. The top rod was 2.25 in. long and the bottom rod 1 in. long. (In

Jan 1, 1961

By Clyde E. Williams

MODERN steelmaking has gradually evolved from an inefficient small-scale operation, utilizing tiny units, to a highly efficient one utilizing large units almost completely mechanized. The leading position of the United States in the steel industry is due to the possession of easily assembled high-grade raw materials and large-scale highly developed plants. Modern integrated steel operation is largely one of material handling. Mining and transportation of iron ore, coal, and fluxes, coking the coal in by-product ovens, smelting the ore with coke and limestone in blast furnaces, converting the resulting pig iron into steel in the Bessemer, or in the open hearth when supplemented with scrap, and fabricating the resulting steel ingots in the shapes of commerce all are done on a huge scale, mostly by machinery, most of the labor being employed either in operating the machine or keeping it in repair. At the same time the quality and uniformity of the product have been greatly increased by the development of scientific knowledge and operating skills. Thus, the steel industry in this country is highly developed both mechanically and technically.

Jan 1, 1942

Jan 1, 1921

By Arthur F. Taggart

TO all Mineral Dressers, but particularly to those in the Coal and Industrial Minerals Divisions: Ted Counselman, retiring after two years at the helm of the Milling Committee, pointed with pride to the continued growth of that committee, and sang the swan song "Why ain&apos;t we a Division of Mineral Dressing?" Our genial Secretary pointed out, handily, that, you see, the way the Institute is divided there are several blocks running across this way here, and one running all the way down here, and another running part way down here, and they all cut across each other like this, and anyway the miners want to be a Division now, so why not you Mineral Dressers be good and not upset the big Institute organizational chart? And anyway again, Divisions have vested interests, and a Division of Mineral Dressing would take something away from Coal and something from Industrial Minerals, and any good institutional man can see that a Division would never give anything up. It was all quite confusing, and apparently not too convincing, because then the Milling Committee went ahead and voted unanimously it is a good idea, let&apos;s see what the other fellows think about it as well.

Jan 1, 1944

By John P. Goheen

Considerable work has been done in developing a pyrometer to measure the temperature of molten brasses, bronzes, and aluminum in the crucible. On account of the high melting points and the amount of zinc and sulfurous fumes given off from molten brasses, the conditions are somewhat severe for a thermocouple of standard design; but satisfactory results are obtained with a portable pyrometer, 3 ft. (0.9 m.) of connecting lead wire, and a special 5-ft. nickel-nickel chromium thermocouple, composed of rods 1/4in. (6.35 mm.) in diameter. The lower 12 or 24 in., as desired, may be made detachable so that new tips may be connected at little trouble or expense. The portable instrument need not be of the extreme high-resistance type, as the movable parts of the galvanometer of a lower resistance instrument may be better constxucted to withstand the continuous handling such an instrument receives. Platinum-platinum rhodium thermocouples, protected with porcelain and graphite tubes, have been used, but the lag in registering the temperature is too great. It has been found that the range of temperature for various brasses is as follows: Red brasses...............2200-2250" F. (1205-1234" C.) Yellow brasses............2250-2400" F. (1234-1318&apos; C.) Bronzes..................2300-2550" F. (1260-1400" C.) A recent test with a portable pyrometer having a range of 2600" F. with a bare 1/4 in. heavy exposed couple 5 it. long and a handle attached at the upper end showed that the temperatures of molten aluminum under varying conditions in an oil-fired crucible furnace and one of the Simplex type were as follows: CRUCIBLE, OIL-FIRED FURNACE SIMPLEX FURNACE Temperature of metal in furnace....... 1540" F. (837" C.) 1530" F. (834" C.) Temperature in ladle after skimming at furnace......................... 1480" F. (805" C.) 1440" F. (784" C.) Temperature in ladle after skimming at floor near mold................... 1440" F. (784" C.) 1430&apos; F. (778" C.)

Jan 1, 1923

By John P. Goheen

Considerable work has been done in developing a pyrometer to measure the temperature of molten brasses, bronzes, and aluminum in the crucible. On account of the high melting points and the amount of zinc and sulfurous fumes given off from molten brasses, the conditions are somewhat severe for a thermocouple of standard design; but satisfactory results are obtained with a portable pyrometer, 3 ft. (0.9 m.) of connecting lead wire, and a special 5-ft. nickel-nickel chromium thermocouple, composed of rods 1/4in. (6.35 mm.) in diameter. The lower 12 or 24 in., as desired, may be made detachable so that new tips may be connected at little trouble or expense. The portable instrument need not be of the extreme high-resistance type, as the movable parts of the galvanometer of a lower resistance instrument may be better constxucted to withstand the continuous handling such an instrument receives. Platinum-platinum rhodium thermocouples, protected with porcelain and graphite tubes, have been used, but the lag in registering the temperature is too great. It has been found that the range of temperature for various brasses is as follows: Red brasses...............2200-2250" F. (1205-1234" C.) Yellow brasses............2250-2400" F. (1234-1318&apos; C.) Bronzes..................2300-2550" F. (1260-1400" C.) A recent test with a portable pyrometer having a range of 2600" F. with a bare 1/4 in. heavy exposed couple 5 it. long and a handle attached at the upper end showed that the temperatures of molten aluminum under varying conditions in an oil-fired crucible furnace and one of the Simplex type were as follows: CRUCIBLE, OIL-FIRED FURNACE SIMPLEX FURNACE Temperature of metal in furnace....... 1540" F. (837" C.) 1530" F. (834" C.) Temperature in ladle after skimming at furnace......................... 1480" F. (805" C.) 1440" F. (784" C.) Temperature in ladle after skimming at floor near mold................... 1440" F. (784" C.) 1430&apos; F. (778" C.)

Jan 1, 1923

HAVING shown you before how moulds of statues and also those of guns are constructed, I wish to tell you at present how, if you wish to cast them in bronze, you are further to prepare and arrange these moulds so that they may receive the melted mass of the metals in a friendly manner and without disturbance. I know that you understand that a real and intense heat has been intro-

Jan 1, 1942

By Carmine D. &apos, Lemuel Tarshis, Joel Hirschhorn, Antonio

Vapor-deposited nickel films in the thickness range 700 to 4360A were tested in uniaxial tension utilizing a microtester designed specifically for this study. Contrary to the findings of some investigators, a definite thickness-strength relationship was observed below 3000 A with a four-to sevenfold increase in strength over that of bulk nickel. The films were characterized by high elastic strains and little plasticity. On the basis of these and other reported data, it is suggested that the high strength level in metal films is related to the manner in which they are produced. Vapor deposition, owing to its severe quenching effect. is believed to promote the formation of point defects which inhibit dislocation movement. IN recent years it has been reported that metals, when in the form of thin films, exhibit extraordinarily high strengths. The data published to date have been primarily concerned with silver and gold because of the ease with which these metals can be vapor-deposited and their high resistance to surface oxidation. Previous investigations into the mechanical strength of thin films has uncovered an apparent dichotomy of view on film behavior. Beams and his co-workers have reported a definite dependence of strength on film thickness. Other workers,"-&apos;6 however, in separate studies on the strength of poly crystalline and single-crystal films have found no such thickness-strength relationship. The study of thin-film strength is extremely difficult because of the many variables associated with film preparation, handling, and testing. Moreover, the manner of test employed by different investigators has varied quite radically, ranging from simple uniaxial-tension to biaxial-bulge testing. The work reported herein was conducted in order to determine the mechanical behavior of a structural metal when in the form of a vacuum-deposited thin film and to gain some insight into the reasons for the high strengths exhibited by metals having such a con- figuration. In this study a method of test was chosen which would yield results which are easily interpreted and lend themselves to comparison with properties of the same material in bulk form. Moreover, specimen-preparation parameters and film-handling techniques are set forth so that other investigators can properly compare their findings with ours. EXPERIMENTAL PROCEDURES A) Film Preparation. Vacuum deposition was performed in an 18 by 30 in. bell jar using a standard New York Air Brake Co. vacuum station with a 6-in. oil-diffusion pump. Before evaporation the system was pumped to a pressure of less than 2 x 10"5 torr. A shield was employed to protect the substrates from the emission of contaminants during the critical melting and outgassing of the evaporant. The source consisted of from one to six filaments (0.020 in. diam). The length of each filament was about 5 in. and was placed 6 to 8 1/2 in. from the substrate in such a manner that the substrate face was at 90 deg incidence with respect to the evaporant beam. The temperature of the source was 2000"~ during evaporation. The films were deposited onto a substrate arrangement which was composed of four basic components, that is: 1) a 3 by 1 in. glass slide; 2) a 22-mm sq micro cover glass on 1); 3) a 22 by 50 mm micro cover glass coated with collodion on 1); and 4) a stainless-steel sheet mask containing twelve rectangular openings of 1-mm and 2-mm widths and lengths of 5 mm laid over 3). Thus, test specimens of 1-mm and 2-mm widths are deposited onto a collodion substrate which precludes epitaxial effects in the specirnens. 17-le The rectangular cover glass and square cover glass were positioned in such a manner that a strip of film would be evaporated along the length and across the width of the large glass slide. This boundary of evaporated film was used to determine the film thickness by multiple-beam interferometry. The square cover glass was used for X-ray and chemical analyses. Thickness of the deposits was varied by changing the number of filaments used (one to six). The duration of evaporation was 30 sec for each filamgnt which resulted in a deposition rate of 8 to 20A per sec. Evaporations were all performed at room temperature; however, radiant heat from the source raised the substrate temperature to 40" to 60°C. All substrates were cleaned by ultrasonic agitation in a solution of spectranalyzed isopropyl alcohol. Collodion was deposited on the micro cover glass by immersion in solution of collodion in amyl acetate. B) Thickness Control and Measurement. Film

Jan 1, 1963

By O. P. Arora, M. Metzger, G. R. Ramagopal

Single-phase aluminum containing 0.0001 to 0.06 pct Cu was studied in strong acid, mainly through observations of hydrogen evolution. The strong influence of copper was exerted almost entirely through the imposition after a certain delay time of an auto-catalytic localized-corrosiott reaction. Additions of cupric ion to the acid produced lower accelerations. The significance of the quantity and distribution of copper was discussed, and the implications for intergranular corrosion and neutral chloride pitting were indicated. AN investigation of intergranular corrosion in single-phase high purity aluminum exposed to hydrochloric acid indicated the copper content of the metal to have an influence on corrosion at lower levels than previously suspected.&apos; The work reported here was a closer examination of the action of copper but dealt with general corrosion to gain the advantage of having a continuous measure of corrosion through the volume of hydrogen evolved, the reduction of hydrogen ion to hydrogen gas being the principal or only cathode reaction in strong hydrochloric acid. Previous work on the hydrochloric acid corrosion of aluminum was sometimes insufficiently structure-conscious and the need for care in evaluating it arises from the low solubility of the iron impurity,&apos; and of some alloying elements, and the known or possible presence in many of the compositions studied of second phases leading to greatly increased corrosion rates.3 These increases are attributed to the presence of low hydrogen-overvoltage cathodes provided by the second phase.3&apos;4 For the present single-phase work, a few studies which used high-purity base material and small copper additions5-&apos; provide the essential information most unambiguously. The corrosion rate was shown to be increased markedly by the introduction into the acid of small quantities of the ions of copper (and of certain other metals) which cement on the aluminum and provide cathodes of low overvoltage.5 When there was sufficient copper in the aluminum, the same result was produced during the course of corrosion leading to a rate which increased with time as the reaction was stimulated by one of its products (autocatalytic reaction). In 2N (7pct) HC1, an accelerating rate was observed at 0.1 pct Cu but not at 0.01 pct.5,7 The present work dealt with corrosion rate and morphology and their correlation with the quantity and distribution of copper catalyst for copper contents from 0.0001 to 0.06 pct. PROCEDURE A lot of high-purity aluminum containing 0.0021 pct Cu, 0.001 pct Fe and 0.003 pct Si (Alloy A) was alloyed with copper to yield aluminum containing 0.014 pct Cu (B) and 0.06 pct Cu (C). Later it was found necessary to include the lower copper Alloy K which contained 0.0001 pct Cu, 0.0004 pct Fe and 0.0004 pct Si. The upper limit for any other element can be confidently estimated as 0.0005 pct. No element other than copper appears to be present in quantities sufficient to have an effect on general corrosion as great as the observed effect of the copper in A, B, and C. The only other heavy metal detected by spectrographic examination was silver (< 0.0001 pct). The acid was made up from a selected lot of 37 1/2 pct CP hydrochloric acid containing 0.1 ppm heavy metals (mainly Pb), 0.05 ppm Fe, and < 0.008 ppm As and from water distilled from 1 megohm-cm demineralized water and believed to have contained negligible quantities of heavy metals influencing corrosion. Acid strength was adjusted to within 0.05 pct HCl of the stated value by using precision specific gravity measurements. Test blanks 10 by 41 mm were sheared from 1.65-mm cold-rolled sheet. Edges were finished by filing. The blanks were annealed in air at 645°C for 24 hr in alundum boats and rapidly water quenched. The anneal is thought to have produced a substantially homogeneous solid solution—for iron, copper, or silicon, for example, the annealing temperature was 200°C or more above the solvus-and the quench is considered to have preserved the high-temperature structure except for the condensation of lattice vacancies into dislocation loops.&apos; The 0.06 pct Cu alloy did not appear unstable in respect to slow precipitation reactions at room temperature since two pairs of tests failed to show significant differences between specimens heat treated 3 1/2 years earlier and specimens heat treated 1 or 2 days before.

Jan 1, 1962

By Clarence O. Babcock

Model pillars of limestone, marble, sandstone, and granite, with length-to-diameter (LID) ratios of 3, 2, 1, 0.5, and 0.25 (0.286 for granite), were broken in axial compression to determine to what extent an increase in end constraint increased compressive strength. Radial end constraints of 13 to 23% of the average axial stress in the pillar, produced by solid steel rings bonded with epoxy to the ends of dogbone-shaped specimens, increased compressive strength somewhat above that of cylindrical pillars without ring constraint. However, when the results were compared with those obtained by other investigators for straight specimens of several rock types taken collectively, with LID ratios greater than 0.5, the resulting strengths were not significantly different. Thus, the amount of end constraint produced by the solid steel rings was about the same as that produced by the friction from the steel end plates. In other tests, a radial prestress of 3000 or 5000 psi was applied prior to axial loading by adjustable hardened steel rings to increase the constraint above that obtained for the solid rings. The average radial constraint stress, expressed as a percentage of the average axial pillar stress at failure for the 3000 psi prestress, was 54.3% for limestone, 40.3% for marble, 44.7% for sandstone, and 23.4% for granite. The average radial constraint stress, expressed as a percentage of the average axial pillar stress at failure for the 5000 psi prestress, was 74.2% for limestone, 51.2% for marble, 61.6% for sandstone, and 29.7% for granite. These constraints increased the compressive strength significantly above the strength of straight specimens and solid-ring constrained specimens. These results suggest that large horizontal stresses in orebodies mined by the room-and-pillar method should increase the strength of the pillars and allow an increase in ore recovery by a reduction of pillar size when major structural defects are absent. One important objective of the U.S. Bureau of Mines (USBM) mining research program is the rational design of mining systems. In the design of room-and-pillar mining operations, pillar strength is a fundamental variable. It is customary to estimate this strength from uniaxial compression tests of rock samples and to correct this value for the length-to-diameter (LID) ratio of the in-situ pillar. This method of estimating pillar strength corrects for pillar shape but does not consider the effect of a large horizontal in-situ stress field that sometimes exists in underground formations. The purpose of the work covered in this report was to determine to what extent the compressive strengths of model pillars of relatively brittle rock loaded in axial compression were affected by lateral end constraint. In previous work, Obert l used solid steel rings bonded to the ends of dogbone-shaped specimens to study the creep behavior of three quasi-plastic rocks -salt, trona, and potash ore - during a test period of 1000 hr. These rings provided radial constraint during the loading cycle of 20 to 50% of the axial stress for specimens with LID ratios of 2, 0.5, and 0.25. He concluded that (1) "for a quasi-plastic material the end constraint strongly affects the specimen strength, and (2) as D/L increases (length-to-diameter decreases), the specimens lose their brittle characteristics and tend to flow rather than fracture." He also concluded that model pillars constrained by rings were better for use in predicting the strength of mine pillars than either cylindrical or prismatic specimens. This conclusion appears to be valid where mine pillars, roof, and floor are a single structural element. In the present study, 460 specimens of four relatively brittle rocks — limestone, marble, sandstone, and granite - were tested to failure. The study consisted of two parts: (1) the effect on the compressive strength of end constraint produced during the axial loading cycle by solid steel rings bonded with epoxy to the ends of the specimens, and (2) the effect on the compressive strength of increased end constraint produced in part by a prestress applied prior to axial loading and in part by lateral expansion of the specimen during the loading cycle. The first part of this study was reported in some detail earlier.2 EXPERIMENTAL PROCEDURE AND EQUIPMENT Model rock pillars of the sizes and shapes shown in Fig. 1 were broken in axial compression when the ends were constrained as shown in Fig. 2. he straight specimens were broken without ring constraint. The specimens of dogbone shape were broken with (1) solid

Jan 1, 1970