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By E. C. W. Perryman

BEFORE describing the methods used for fabricating uranium into various shapes and sizes it is necessary to illustrate briefly the unusual conditions under which uranium has to operate when used as a fuel element in a reactor. During reactor operation, for every fission that occurs two atoms of intensely radioactive fission products are produced together with two or three neutrons. The neutrons that are ejected possess several m.e.v. of energy and when one of them strikes an atomic nucleus, that atom acquires up to 105 e.v. of kinetic energy. This is large enough to displace the atom from its lattice position and send it shooting through the crystal, displacing other atoms out of their lattice positions. The net result is that a large number of vacancies and interstitial atoms are formed within the crystal lattice which sometimes have profound effects on the physical and mechanical properties of the material in question.

Jan 1, 1957

By E. S. Machlin

The possibility that formation of voids under creep-rupture conditions may take place by the condensation of vacancies has been investigated theoretically. It has been concluded that nucleation of voids under creep-rupture conditions by vacancy condensation is highly improbable. However, growth of pre-existant voids by vacancy condensation is probable. A number of predictions made in this theory have been verified by the data. It has been predicted and checked that the product of rupture life and steady-state creep rate for preannealed metals and single phase alloys is an approximately invariant quantity, independent of stress, temperature, and atomic number for a given type structure. The direction of the effect of cold work on this product has been predicted and found in agreement with experiment. A number of experiments to evaluate the vacancy condensation mechanism further are described. SEVERAL papers have appeared recently which speculate on the origin of voids formed at grain boundaries under stress.' ' The object of this paper is to examine quantitatively the proposition that the voids produced in a creep test are a result of vacancy condensation. A result of this paper is a theory of creep-rupture. Void Nucleation Application of standard nucleation theory" to the problem of void nucleation leads to the following conclusions: 1—Homogeneous nucleation of voids requires a supersaturation ratio (concentration of vacancies in supersaturated to that in saturated solution) of 400 for a reasonable surface energy of 1000 erg per cm-and 1.4 for the improbably low surface energy of 10 erg per cm. 2—Heterogeneous nucleation of voids at plane interfaces between two phases requires a supersaturation ratio of 2.5 for a typical contact angle of 145 3-—Void nucleation about a solid particle may be accomplished at a supersaturation ratio of 1.17 for a typical value of work of adhesion? of 60 erg per The work of adhesion is the surface work 10 replace two solid-vauor surfaces by a solid-solid interface. enr ' between an oxide and a metal in the presence of a surface active element such as sulphur. Estimates of the supersaturation ratio at which voids are produced in diffusion experiments yield a maximum of 1.01. Inasmuch as the foregoing mechanisms of void nucleation probably will not operate at this level—too low a surface energy is required—the investigatol. is led to the conclusion that voids must already exist. That is, nucleation of voids probably does not occur. Rather, existing submicroscopic voids grow out to visible size. Already existing voids might be produced during solidification or working. Supercritical sized parlicles which contain cracks may act as heterogeneous void nuclei. Gas pockets may act as void nuclei. Experiments are desired to determine the nature of the heterogeneous void nuclei which grow out to voids in both diffusion and creep experiments. Void Growth Void growth might occur in at least two possible ways, depending upon whether the already existing void nuclei are at grain boundaries or within the grains. In the case of a spherical void far from a crystal boundary, vacancies are generated during creep as a consequence of the migration of suitable dislocation jogs' and are also annihilated at sinks. Under these conditions, a steady-state concentration of vacancies is built up in the crystal, defined by the condition that for any differential volume the rate of generation of vacancies in that volume equals the rate of annihilation of those vacancies." This equality would lead to the development of a gradient of vacancy concentration radially outward from the void surface up to a radius where the vacancy lifetime becomes equal for all directions of vacancy migration. The distance over which this vacancy concentration gradient extends equals about 2vD,T* where D, is the vacancy diffusivity and T:' the vacancy lifetime in a crystal outside the gradient in a zone of constant vacancy concentration. The vacancies generated in the region over which the gradient exists will annihilate more often at the void than elsewhere. Approximately a little over one-half the vacancies generated in the gradient zone will annihilate at the void. Hence, the growth rate of the void is given by on where R is the radius of void in centimeters, is the atomic volume, and R is the rate of generation of vacancies, number per centimeter" per second. R D and T* may be estimated in terms of other physical parameters." In particular, R = n.j e/b [3] where n is the average number of vacancy produc-

Jan 1, 1957

By Robert H. Merrill

This report summarizes the first phase of studies to determine the design and behavior of an unsupported roof in an experimental room in limestone. The selection of a roof horizon and the design of the room were results of an investigation of the geology of the formation, the physical properties of samples from the proposed roof, and calculations from the theory of gravity-loaded beams. The design of the opening, some physical properties of the roof in place, and the behavior of the roof were checked by tests in a full-scale experimental room. The room was instrumented to measure roof deflection, separations in the roof strata, and incipient failure. The dimensions of the room before instrumentation was installed were 10 by 100 feet; the room was widened in successive increments to 40 by 100 feet. Between widening operations periods up to 6 months were allowed to provide a time test of the roof spans. The results of the measurements of deflection and separations showed that the lowest 6-inch layer in the roof became detached as the room was widened. This layer was eventually removed after standing without failure for about 4 months at room dimensions of 40 by 100 feet.

Jan 1, 1957

Unfortunate occurrences resulting in injuries, loss of life, and destruction of property by explosion, fire, and other mishaps during shaft sinking in the past few years have focused the attention of the Bureau of Mines on the need for safety standards for such operations. Several States have some rules and regulations applicable to local conditions, and several Bureau publications (including some now out of print) cover the hazards that may be encountered in shaft sinking. Certain requirements of the Federal Mine Safety Code and Federal Coal Mine Safety Act may be applied, but there are no definite, uniform standards that will guide those desiring to sink a shaft safely and bring about uniform safety inspections.

Jan 1, 1957

By J. R. Nettle

A method has been developed in the laboratory for successfully electro-refining titanium metal. Refining is accomplished in e fused-salt electrolyte using offgrade metal as the anode and collecting the purified metal at the cathode. The characteristics and requirements of the various alkali chlorides tested as electrolytes are discussed in relation to relative ease of purification and serviceability. The various types of cells designed and tested for electrorefining are illustrated and their method of operation discussed. The individual advantage of each cell and the purpose for which it was designed are reviewed. The magnitude of the cathode current density was found to depend largely upon the quantity of soluble titanium chloride in the electrolyte. The physical condition of the anode also greatly affected the cathode current density.

Jan 1, 1957

By R. L. Fullman, J. W. Cahn

A method is derived for obtaining the distribution of sphere diameters and plate thicknesses (or pearlite spacings) from size distribution functions obtained along randomly oriented lines. The method described offers several advantages over existing methods. IT is often of interest to measure not only the average particle size but also the distribution in sizes of particles dispersed in an opaque material, such as an alloy. Particles of a single size will exhibit a range of apparent sizes on the plane of polish. If the sample contains a distribution of particle sizes, the distribution of observed sizes on the plane of polish is related to the distribution of actual particle sizes by an integral equation, For example, a distribution of sphere sizes, N(r),

Jan 1, 1957

By Jesse A. Miller

ALTHOUGH the element titanium was discovered by William Gregor in 1790, over a hundred years passed before it was put to commercial use. The first commercial application of titanium was as an alloy additive to iron and steel, and the first ferroalloys were produced domestically in 1906. Titanium pigments were developed somewhat later and have been produced in the United States since 1918. The use of titaniferous material in welding-rod coatings first gained acceptance ill the mid-30's. The metal titanium has only had commercial importance since 1948; domestic production for that year was 10 tons. The relative importance of these major uses of titanium in various forms may he gaged by the consumption of titanium dioxide (Ti02) for these purposes in 1954. Of a total of 440,000 short tons of Ti02 consumed in 1954, 95 percent of the total was consumed for pigments; 2 percent for welding-rod coatings; 1 percent for non-titanium-base alloys and carbide; and 2 percent for miscellaneous uses. The titanium-metal industry is in its infancy, but it has more than doubled its output every year from 1948 to 1954, reaching 5,370 short tons in 1954.

Jan 1, 1957

With the sinking of the No. 3 Shaft at North Broken Hill Limited, it was necessary to construct adjacent to the shaft a new changehouse for mining and surface personnel.It was also probable that as the older sections of the North and British leases were worked out, all employees at present working in these sections would be transferred to the No. 3 Shaft area. This could ultimately result in all personnel employed by North Broken Hill Limited being concentrated in this area, requiring the construction of new administration offices, workshops, mine store, etc., also in this area.

Jan 1, 1957

Six years ago it was my responsibility to give the presidential address, and now that privilege has come my way again. On that occasion we were gathered atWhyalla and I took the opportunity of putting before members some observations on the problems we then faced in Australia, and some gains we had been able to chalk up during those early postwar years. You may recall that we were then just beginning to emerge from the difficulties of postwar reconstructions - of fuel and power shortages, and a grossly inadequate manpower for the tasks facing us. The expansion of manufacturing industry in Australia greatly stimulated by wartime activities, and by the postwar developments of many institutions - ran ahead of the supporting services and of the supply of labour to do thejobs. For many industries this unfortunate state of affairs had meant operating at rates well below their installed capacities and therefore levels of output insufficient for Australia's rapidly growing needs. When I last spoke to you these problems were still with us, though their intensity was beginning to lessen as a result of vigorous efforts by industry and governments to reduce them. But I must confess that my thoughts on that occasion were full of those problems and of the effect they were having on the iron and steel industry of this country-of the coal shortage, the labour shortage, and the many other difficulties we were then faced with - and all at a time when the stepping up of our postwar expansion programme was of vital concern to all of us.What a different picture it is six years later! How greatly has the scene changed for the better. In 1951 Australia's postwar immigration programme was only in...

Jan 1, 1957

By S. M. Runke

The pegmatite investigations at the Rapid City, S. Dak., Experiment Station during; the pact 3 years have been primarily a study of recovering beryl from nonlithium-bearing pegmatite rock by continuous-testing methods. Beryl concentrates containing 25 to 88 percent beryl were produced from rock that ranged in beryl content from 0.1 to 2.5 percent. The beryl recovery ranged upward from 70 percent but averaged better than 80 percent. Although promising results have been obtained with flotation methods for upgrading these concentrates to standard specifications, additional work is needed to improve and simplify the procedure. In addition, it was demonstrated that several potentially useful coproducts could also be recovered from pegmatite rock. The principal coproducts were mica, feldspar, and quartz. A heavy-mineral product also was made from pegmatites containing tin, tantalum, and columbium. The recovery if these minerals in products meeting the specifications of the commercial users has been reserved for future study. The investigations also included studies on extraction of beryllium from both high-grade beryl and flotation concentrates of medium beryllium content. The procedure investigated consisted of sintering beryl or beryl flotation concentrates with limestone, acid curing the resulting sinter with sulfuric acid to dissolve the beryllium, and water leaching to extract the beryllium. Over 90 percent of the beryllium was extracted by this procedure. Most of the optimum conditions and quantities of reagents were determined for dissolving the beryllium. As aluminum and iron also were taken into solution by the acid, further research is needed on methods of recovering high-grade beryllium salts from the solutions containing these elements.

Jan 1, 1957

By C. Norman Cochran, James L. Brandt

ALTHOUGH gas in aluminum and its effect on aluminum products have been the subject of a number of papers, not many quantitative determinations of the hydrogen content of solid aluminum and its alloys have been recorded in the literature. For solid aluminum samples, four investigators have reported hydrogen contents which appear reasonable compared with the hydrogen solubility of 0.7 ml per 100 g, STP, in molten aluminum at 660°C established by Ransley and Neufeld' and verified by Opie and Grant' and Ransley and Talbot. Sloman," who used a vacuum fusion procedure, reported the hydrogen content of some high purity aluminum as 0.66 ml per 100 g, STP. Griffith and Mallett, employing the tin fusion method, reported the internal hydrogen content of six different aluminum alloys as ranging from less than 0.1 ml per 100 g, STP, for 1100 alloy to 0.7 ml per 100 g, STP, for 4043 alloy (previously 43S, a 5 pct Si alloy). Eborall and Ransley," using a solid extraction of the gases at 600°C, reported hydrogen contents ranging from 0.1 ml per 100 g, STP, to 1 ml per 100 g, STP. Ransley and Talbot reported that several thousand analyses on 99.2 pct and higher purity aluminum as well as Duralumin type alloys indicated hydrogen contents ranging from 0.1 ml per 100 g, STP, to 0.5 ml per 100 g, STP.

Jan 1, 1957

By A Guinier

RECIPITATION in alloys is undoubtedly one of the most essential phase transformations in metallurgy and, besides, it is a phenomenon of great interest to physicists. It seems then that it can be chosen as a topic for an Annual IMD Lecture. Of course, the subject is a very wide one and I shall discuss here only a very restricted part of it. I should like to show why it is now considered that there is, at the beginning of the process, a stage distinct from the real precipitation, which is the pre-precipitation. We shall be chiefly interested in the atomic structure of the metal in this preprecipi-tation stage. Numerous reviews on this subject have been published recently.', ' The latest was given by H. K. Hardyh t the last meeting of the Institute of Metals in London. One of the most complete articles has been written by the late Dr. Geisler." I should like, at the beginning of this lecture, to pay a tribute to the memory of our friend Arthur Geisler. Some of the ideas which will be developed here are different from those advocated by him. But everybody knows the considerable progress in experiment and in theory which we owe to him and, personally, I deeply feel how fruitful have been the long discussions which we have had during many years. Experimental Basis of the Precipitation Problems Let us recall the essential facts pertaining to the problem of the precipitation. The starting point and the final one are well known. The initial stage is the supersaturated solid solution before quenching. The dissolved atoms replace some of the atoms of the solvent at the points of a definite lattice. It is generally considered that the distribution of the atoms is completely random, and that the lattice distortions are relatively weak. These assumptions are only an approximation. It has now beenproven", that, in some cases, the dissolved atoms have a tendency to segregate to form very small nuclei. These fluctuations of composition are greater than the normal statistical fluctuations in a purely random alloy. We shall see the role played by these nuclei later. The final state is obtained by a very long annealing at such a temperature that an equilibrium is reached in a reasonable time. The alloy is then composed of a matrix which is a saturated solid solution, much poorer than the initial one. Imbedded

Jan 1, 1957

By H. I-Lieh Huang, O. D. Sherby, J. E. Dorn

RECENT investigations1-4 have suggested that the total plastic strain, C, for high temperature creep under a given stress can be correlated by means of a temperature-compensated time, te- where t is the duration of test, e is the base of natural logarithms, aH is the activation energy for creep, R is the gas constant, and T is the absolute temperature. A typical set of data on which this deduction was based is given in Fig. la. Inasmuch as the e-in t curves for the various temperatures are identical except for their displacement along the In t axis where f and are appropriate functions. If the increase in creep rate with an increase in temperature is exclusively ascribable to a single process involv- ing thermal activation, (T) should equal RT and therefore it = constant [2] where ?= te Assuming the validity of this relationship, ? = ?2 at the same strain, or where the subscripts refer to two alternate test conditions.

Jan 1, 1957

By Robert L. Rough

The 1954 field tests consisted of six experimental shots in relatively deep holes in a sandstone similar to many oil-bearing sandstones. Water-injection measurements were made before and after each shot to establish the change in conductivity of the fluid caused by the shot. The pressure pulse produced by the shot was recorded in nearby holes to monitor the shot and to determine if any relation existed between the change in conductivity and the nature of the pressure pulse. The results of water-injection tests showed the range of conductivity of fluid before and after shooting with two different types of explosives. Because of the large spread in data for similar shots, not enough information was available to evaluate the differences in increased conductivity produced by the two explosives or any relation between the increased conductivity and the nature of the pressure pulse. However, these results, with the results of other tests involving explosive shots in rock, provide guidance for future research on the oil-well-shooting problem.

Jan 1, 1957

By Herty, C. H.

Iron oxide (FeO) plays an extremely important part in the manufacture of iron and steel. In the three major processes- blast-furnace, open-hearth, and Bessemer converter-iron oxide is the chemically predominant compound and controls to a large ex- tent the operation of the furnaces and the composition and quality of their respective products. In order to emphasize the importance of iron oxide in each process, they will be considered individually in some detail. THE OPEN-HEARTH FURNACE. Iron oxide is introduced into the open-hearth furnace in four ways : 1. The scrap charged into the open hearth is oxidized by the furnace gases, the amount of oxide formed depending primarily on the amount and type of scrap charged. It has been found' that with large scrap, 1.7 Ib. of FeO is formed per 100 Ib. of scrap charged, whereas with scrap of medium size about 5.3 Ib. of FeO is formed per 100 Ib. of scrap charged, when the period between the charging of the scrap and the addition of hot metal is 3 hours. 2. The decomposition of the limestone sets free CO, by the reaction

Jan 1, 1957

By R. T. Johansen

A gradual decrease in injection rates commonly occurs as a water-flooding project becomes older. This decrease can be attributed to changes in reservoir conditions, such as swelling of clay minerals, fillup, or gradual plugging of the sand face. However, a rapid decrease in the rate of injection indicates abnormal behavior and is cause for alarm. Extreme plugging conditions can completely stop injections into a formation. Such behavior in wells was the main concern of the tests described in this report. An accepted method of alleviating this condition is by backflowing input wells - closing the supply lines to the wells and allowing the reservoir pressure to force water back into the wellbore and to the surface. If backflowing is not successful, a string of smaller diameter pipe sometimes is run inside the casing, and the sand face is flushed with a waterspray. More drastic treatment is to inject acid into the wellbore to dissolve extraneous matter, or even part of the reservoir material, in an attempt to restore the permeability of the sand immediately around the wellbore. Any of these procedures can he coordinated with bailing and swabbing of the well for cleanout purposes.

Jan 1, 1957

By John J. Gilman

F many years it has been suspected that a correlation existed between pits produced by etching and the density of dislocations in crystals. In 1953, the interest in this correlation was greatly stimulated when Vogel et al' demonstrated a 1:l correlation between etch pits and dislocations in low angle grain boundaries of germanium. About two years ago, the author began attempts to produce etch pits at dislocation sites in zinc mono-crystals. These attempts met with success a year or so ago,' and since that time a survey has been made of the etch pit patterns that are associated with various modes of deformation in zinc monocrystals. Unfortunately, the etching technique that will be described is too delicate for use as an accurate quantitative tool. Nevertheless, it has been of considerable assistance in clarifying the structure of plastically deformed crystals. Technique Many attempts were made to produce etch pits in high purity zinc crystals. It was found that several techniques would produce surface grooves at grain boundaries that had misorientation angles greater than about l°, but no technique was successful for boundaries with smaller angles. Among the things that were tried were: electrolytic CrO, (both etching and polishing concentrations), HNO, in various water and alcohol solutions, dilute HC1, many 0-0,-Na,SO, solutions, Cr0,-HC1 solutions, picral, electrolytic Na,S,O,, and electrolytic NaOH and KOH. A few attempts to use cathodic sputtering and thermal etching were also made.

Jan 1, 1957

By R. R. Wells

This report summarizes the results of laboratory testing of copper-bearing magnetite ore from the Poorman, Bush & Brown, and Copper Center deposits, Kasaan Peninsula, Prince of Wales Island, southeastern Alaska. The ores contain minor amounts of chalcopyrite and pyrite. Intimate association of these sulfides with magnetite necessitates fine grinding for adequate liberation and rejection of copper and sulfur and for the production of high-grade iron concentrate low in objectionable impurities. Laboratory tests indicated that the optimum results can be obtained by flotation of ore ground to minus-100-mesh, with subsequent wet magnetic separation treatment of the flotation tailing. A summary of results obtained by this treatment of the three samples tested is shown in table 1.

Jan 1, 1957

By John C. Machisak

Statistical data on injuries in the metal and nonmetal industry of the United States first became available to the Bureau of Mines by collecting reports from the operators for the calendar year 1911. Since then reports have been collected annually. The present bulletin, covering the calendar year 1954, is the 31st publication (1933-34 was published as Bulletin 398) containing statistical data on injuries at metal and nonmetal mines and related plants, and it 1s the first such bulletin to be published since 1942. The last publication was Bulletin 461, Metal and Nonmetal-Mine Accidents in the United States, 1942. The unpublished statistics for 1943-53 may be found in the Appendix of this bulletin. The Bureau of Mines is authorized to collect data on injuries and related employment at metal and nonmetal mines, but there is no Federal law that compels operators to submit such information. Therefore, all materials submitted are voluntary responses to the Bureau's requests for information. The figures presented herein may not be complete for the entire industry, nevertheless, every effort has been made to make them so, and the data given are believed to be representative of the hazards to which metal and nonmetal workers are exposed. Moreover, the figures are comparable as between States-which is significant in view of the lack of uniformity among the States as regards classes of plants covered by State laws, classes of injuries covered by State reports, and other factors that tend to make it impracticable or impossible to compare the injury experience of one State with that of another or comprehend the relative importance of the various causes of injuries in the industry as a whole.

Jan 1, 1957

By John Chipman, Peter J. Koros

The distribution of copper between liquid silver and liquid iron, Fe-C, and Fe-C-Si alloys was studied at 1600°C. From the data and the activity of copper in silver obtained from the phase diagrams, the activity coefficients of copper in iron up to 3 atomic pct are log y, = 0.90 — 2.4 N, and y": = 8.0. The effect of carbon up to saturation is expressed as log y = 1.8 Ni. The effect of silicon up to 11 atomic pct is insignificant. SLOWLY rising copper content of steel being produced is focusing attention on the lack of information on the behavior of copper in liquid steel. Chou' measured the activity coefficient of copper in liquid iron through its distribution between liquid silver and iron. He obtained a value of 9.12 at infinite dilution. Chipman' calculated the activity coefficient of copper in liquid iron at 1600°C from the phase diagram and obtained a value of 12. Ameiln and Pfeiffer- investigated the possibility of removing copper from liquid steel through the use of lead, silver, and bismuth as solvents. They also calculated that the activity coefficient of copper in liquid iron would be increased five or sixfold by addition of 4 pct C. Langenberg and Lindsay' are investigating the effectiveness of lead and sodium sulfide in removing copper from liquid iron. The experimental method was similar to that used by Chou' and Chipman and Floridis." Silver, copper, and iron were melted together, the copper distributing itself between the two layers so that at equilibrium a,.,, (in Ag) - a,.,, (inFe) and N,.,, (in Ag) yc,, (inFe) (in Ag). [21 N,.,, (inFe) Thus, from the concentration of copper in each layer and the activity coefficient of copper in liquid silver, the activity coefficient of copper in liquid iron can be calculated. The effect of an alloying element such as carbon on the activity coefficient of copper can also be determined from its effect on the distribution, provided the new element is essentially insoluble in silver. The one serious limitation of this method is the increasing mutual solubility of silver and iron in the presence of a third component. The mutual solubilities of pure iron and silver are negligible, but increase with increasing copper concentration beyond the range investigated. Ag-Cu System—The activity coefficient of copper in silver at 1600°C had to be estimated, since direct experimental data are not available. Kawakami" measured the heat of mixing of Ag-Cu alloys at 1200°C by a calorimetric technique. Scheil' calculated the heat of mixing in this system by use of the phase diagram, assuming that the solution is random and that the heat of mixing is independent of temperature. The terminal solid solution may be assumed to obey Raoult's law within the requirements

Jan 1, 1957