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By Richard Quirk

This report describes methods and techniques employed by The Glidden Co. of Cleveland, Ohio, in explorating an ilmenite-bearing sand deposit in Ocean County, New Jersey, during 1960 to determine ore reserve potential and the feasibility of mining and establishing a milling plant on the property for the production of ilmenite concentrate. The property covered approximately 1,250 acres. Comprehensive sampling by water-jet drilling indicated the deposit averaged 20 feet in thickness and contained 4.5 percent heavy minerals, of which 80 to 85 percent was ilmenite and leucoxene. Average depth of the water table as determined by auger boring was 16.8 feet. Pilot plant tests indicated that circular concentrators in combination with spiral concentrators would recover at least 80 percent of the heavy mineral content of the sands. It was estimated that sufficient ore reserve tonnage had been developed to supply the company's Baltimore chemicals division, pigments department, with a suitable grade ilmenite concentrate for a period of 20 years at the present rate of pigments production. The property was designated as Lakehurst mine and plans are in progress for mining development and plant construction.

Jan 1, 1963

By C. L. Chaney

Investigations were conducted to develop spectrochemical methods capable of determining 0.01 to 100 micrograms of metals in 50 milliliters of solution. The use of gallium hydroxide (Ga(OH)3) as a carrier-precipitant to concentrate metallic ions is described. A porous-cup graphite electrode is used to collect the precipitate. A specially designed plunger permits the electrode assembly to serve as the sample-containing electrode in the subsequent spec-trographic analysis. Analytical curves are presented for antimony, arsenic, beryllium, and zinc. Sensitivities of detection are given for 13 elements. The techniques were applied to identify impurities separated from tungsten, to determine trace impurities in solutions containing high concentrations of magnesium, cobalt, or nickel, and to identify trace impurities in hydrofluoric acid. Laboratory glassware was a serious source of contamination when low levels of zinc were determined.

Jan 1, 1963

By Frank A. Peters

A series of evaluations is being made to determine the relative processing costs of producing metallurgical-grade alumina from low-grade aluminous materials. These evaluations include the estimated operating and capital costs as well as recommendations for additional research and development to improve the processes and to lower their costs. The design for each process is based on published work. The three processes considered in this evaluation are designed to leach alumina as aluminum sulfate from calcined clay with sulfuric acid and to remove the silica residue by filtration. The filtrate from leaching is then purified by one of the following methods: Removal of iron in electrolytic cells using mercury cathodes; removal of iron by chemical precipitation through the formation of an iron-manganese complex; or precipitation of the alumina from an aqueous-ethanol solution, leaving iron in solution. Both the operating and capital costs for these processes are higher than those for the Bayer process. For plants producing 1,000 tons of alumina a day, the estimated operating costs per ton of alumina are: Electrolytic iron-removal process........... $81.35 Chemical iron-.removal process............... 82.08 Ethanol purification process............... 86.17 The investment in mercury is not part of the operating cost since this cost is considered equivalent to catalyst cost which would not be shown. The estimated capital investments for 1,000- ton-per- day plants on a Marshall and Stevens chemical equipment index basis of 240.0 are: Electrolytic iron-removal process...... $116,775,500 Chemical iron-removal process............... 99,418,900 Ethanol purification process................ 94,210,200 These investments include the working capital but not the land for each of the processes. Included in the electrolytic iron-removal process is an investment of $4,859,400 for mercury. Investigation of other methods for removing iron, of the decomposition operation, and of the leaching operation could reduce these costs.

Jan 1, 1963

By Walter A. Backofen, Donald H. Avery

Intense primary and cross-slip traces were observed in easy glide on Cu: 6 pct-A1 single crystals deformed in tension. A mechanism of cooperative source operation is developed which recognizes that both the applied stress and that resolved from dislocation arrays contribute to the stress on a source. By considering the stress from arrays, the activation of secondary systems in easy glide and the difference in appearance of slip markings on pure and solid-solution crystals are explained. Furthermore the cross-slip system is predicted to be second favored during easy glide for a large range of orientations. FROM many studies of easy glide in fcc metal crystals, a pattern of observations has developed which still requires full explanation. In pure copper, aluminum, and silver, the easy-glide, slip traces are fine and uniform with steps 50 to 100A on the primary* system.1-4 Yet it has not been at all clear why slip in the pure materials should occur in this way. On the contrary, one might expect, with simple slip and a low hardening rate, that the weakest sources on the primary system would operate extensively to produce strong slip traces. In a brass, however, intense slip steps up to 0.5 are found on both primary and cross-slip system4,6-9 seeger10 has pointed out that in a material of low stacking-fault energy such as a brass, extensive easy-glide cross-slip could not be thermally activated, but rather must originate on the cross-slip plane. In further explanation, the wilsdorfs4 and seeger10 noted that only the cross-slip system would not harden differently than the primary, whatever the latent hardening tendencies of other systems; therefore, in brass, which exhibits high latent hardening, the cross-slip is the only secondary system which could be expected to operate extensively, once it became active. The explanation of how the cross-slip system, on which the applied stress is low, becomes activated has been related, in a nonspecific way, to pileups by Hirsch11 and Honeycombe.l2 In the work to be described, deformation traces on solid-solution Cu: 6 pct A1 single crvstals were studied with conventional light microscopy and a mechanism proposed to explain both the observed activation of secondary systems in easy glide and the difference in appearance of slip markings on pure and solid-solution crystals. EXPERIMENTAL In preparing the Cu-A1 single crystals, rectangular bars approximately 0.4 in. by 0.4 in. by 6 in. were first machined from ingots made by vacuum melting copper of 99.999 pct and aluminum of 99.99 pct purity. They were then packed in powdered graphite and the crystals grown in a modified Bridgman apparatus at a rate of 5 mm per hr under an atmosphere of purified nitrogen. Crystal perfection as indicated by Laue back-reflection spots was good except for the last inch to freeze, which was discarded. Orientations so determined are shown in Fig. 1. Tensile specimens with a reduced gage section were obtained by masking the ends with electrical tape and chemically polishing in a solution of 20 pct HNO3, 24 pct HAc, 52 pct H3PO4, 2 pct Hcl, and 2 pct H20 at room temperature.13 Finally, the specimens were electropolished in a 30 pct ortho-phosphoric acid bath at 12 v. Tensile deformation was performed in an Instron testing machine at a strain rate of approximately 1 pct per min. During easy glide, extensive cross-slip was observed with all crystals, in spite of the low Schmid factor on this system, and in no case was any other secondary trace encountered. A certain sequence of slip-line development was associated with the extension. At yielding, intense primary traces passing completely through the crystal developed at some point on the gage section, generally near the grips; weak cross-slip traces also appeared, extending from the primary traces into the adjacent undeformed crystal, Fig. 2. Further extension led to primary traces adjacent to the first-formed and connecting with those of the cross-

Jan 1, 1963

Jan 1, 1963

By W. M. Phillips

Processing kaolin clays from the sedimentary deposits of Georgia and South Carolina is described in this article. While the major processing steps are touched on briefly, emphasis is given to the dewater-ing of the clay-water slurries (slips) formed in the processing of kaolin clays. The dewatering steps discussed include gravity settling, centrifugal dewatering, vacuum filtration and thermal drying. Particular attention is given to vacuum filtration and the variables affecting filtration of these kaolin clays. Kaolin consists essentially of the mineral kaolinite, which is a hydrated aluminum silicate (Al2O3 . 2SiO,). Commercial deposits of kaolin occur in several areas of the U. S., but approximately 90% of the kaolin produced in this country comes from Georgia and South Carolina. These deposits are of sedimentary nature and occur in a geological fall line in the Tuscaloosa formation at elevations between 300 and 450 ft above sea level. Over two million tons of kaolin clays are used by industry in the U. S. each year. A big percentage of this tonnage is used in the paper industry for coatings in making glossy and high quality grades of printing papers. In addition, large tonnages are used as pigments; as fillers for rubber, plastic and fertilizers; and in ceramics. Properties of kaolin that make it widely used in the above applications are its particle size fineness, natural whiteness, chemical stability and non-abrasiveness. In addition to these desirable properties, it is relatively inexpensive. The finer coating grades of clays range in price from $15 to $28 per ton while the coarser filler grades sell within a range of $7 to $13.50 per ton. Pure kaolin particles are small hexagonal flat platelets. Above the 2-p size, the particles usually consist of stacks of plates, while below the 2-p particle size they occur as individual flat, hexagonal plates. Since these individual platelet particles provide the most desirable coating and flow characteristics, major importance is given to particle size fractions of 2 p and smaller. Generally, coating grade clays are those with all particles smaller than 15 p and at least 70% of the particles less than 2p. These coating grades also have 50% or more of the particles smaller than 1 µ in size. The extremely fine grades of coating clay currently being produced approach the range of 100% smaller than 2p. The filler grades of kaolin have 100% of the particles passing 325 mesh but have less than 70% of their particles below the 2-p range. Fig. 1 is a schematic representation of the major processing steps involved in preparing kaolin clays for marketing. MINING All kaolin mining is open pit. The ratio of overburden to clay will average 3:1, but this ratio can, of course, be much higher depending upon the grade of the clay and the size of the deposit. Most of the commercially mineable deposits occur from 20 to 120 ft below the ground surface. Both draglines and pans are used in removing the overburden and mining the clay deposit itself. After mining, the most common method of transporting the clay to the processing plant is by blunging or re pulp-

Jan 1, 1963

By Harold Rees

[This report supplements and brings up to date a paper prepared earlier this year for presentation at the Eleventh Pan American Railway Congress to be held in Mexico City, October 18 to 31, 1963. In order to acquaint the reader with the background of this project practically all of the first paper is included in the report.]

Jan 1, 1963

By Richard Stewart

There are highly competitive world markets in most of the minerals being mined today. The high standard of living we enjoy in North America results in ever increasing productivity through mechanization and automation. Conventional underground and open-pit mining practices throughout the world are constantly changing to reflect the engineering advances of our technology. New records in tunneling, shaft sinking and excavating are being established. Larger and faster equipment is in production. Mining operations are being studied in detail to improve materials, methods and machines. Standards and controls are being established to measure the performance of people and equipment. These steps all tend to improve our present performance. In addition to these short-range improvements, however, there are the basic research and applied research studies which are aimed at developing entirely new approaches to our mining problems. Basic research in rock mechanics is coupled with applied research in rock penetration, fragmentation and stabilization.

Jan 1, 1963

By J. H. Schulman, M. H. Buckenham

R. W. Christy (Manager of Sales, Sanitary Engineering Equipment, Link-Belt Co.) and C.D. Rubert (Barrett, Haentjens & Co.) — Messrs. King and Schepman have presented an excellent paper which outlines the general practice in the design of thickener mechanisms. Lifting devices, controls, special applications and underflow pumping arrangements have been reviewed in detail. Pumping arrangements were illustrated which eliminate the need for an expensive tunnel beneath the thickener floor. Most of those illustrated have the common feature of a relatively long underflow suction line extending from the hopper floor to the pump located on the bridge at the periphery of the tank. The authors limit these arrangements to comparatively dilute or thin slurrys. It is implied that dense and coarse concentrates, which are difficult to pump, cannot be handled unless a tunnel is constructed. Fig. 1 shows an underflow pump arrangement which negates the need for a tunnel but which permits the operator to convey a heavy dense slurry. The pump is mounted directly on the fixed hoist platform and the impeller is located at the base of the steel center column. Priming water is not needed. The column

Jan 1, 1963

By John C. Machisak

The Nation's mining and quarrying industries have again met the annual challenge to their ingenuity--that of reducing disabling work injuries among their employees. The effectiveness of management in facing this problem and in meeting this responsibility from the results of the 1961 National Safety Competition. Three hundred ninety-three or 45.3 percent of the mines and quarries participating in the competition established a new record number of participants operating throughout the competition year without a disabling work injury. Another record established in the 1961 contest was the number of participants (868) enrolled in the competition. This annual safety competition was begun in 1925 and is conducted by the Bureau of Mines, U.S. Department of the Interior. It provides for six bronze Sentinels of safety trophies which are awarded each year to the winning participant in each group. Since its inception, the competition has exerted a strong influence in the field of safety promotion. The statistical record of its accomplishments over the years gives strong support to the theory that well-organized and well-administered safety programs are effective tools to be used to reduce the number of disabling work injuries. It stimulates and holds the interest of employees and management in accident prevention. Because of this, mines and quarries participating in the contest have a more favorable safety record than those operations not enrolled.

Jan 1, 1963

By Brian F. Dyson

The surface tensions at 1550°C of some Fe-S alloys (in the range 0.008 to 0.052 wt pct S), Fe-Sn alloys (0.31 to 48.4 wt pct Sn), Fe-P alloys (0.038 to 2.38 wt pct P), Fe-Cu alloys (2.15 to 22.8 wt pct Cu), and Fe-1 pct C-S alloys (0.005 to 0.076 wt pct S) along with the surface tension of the base iron have been measured by the sessile-drop method. A mean value of 1754 dynes per cm was found for the surface tension of the base iron. Sulfur was found to be highly surface-active, the surface-tension results being in quantitative agreement with existing data. Tin and copper were found to be less surface-active than sulfur while phosphoms was completely nonsurface-active. The surface tensions of Fe-1 pct C-S alloys were found to be lower than those of the Fe-S alloys containing the same sulfur content. This was shown to be a mmzifestation of the increase in the thermodynamic activity of suZfur by carbon. It is only in recent years that attempts have been made to measure the surface tension of liquid iron of known high purity.1-3 Earlier measurements4-7 were made on liquid iron containing variable amounts of what are now known to be surface -active solutes. The exact value of the surface tension of liquid iron is still, however, open to some doubt. Halden and Kingery' reported a value of 1720k 34 dynes per cm at 1570°C, Kozakevitch and Urbain8 gave 1790k 25 dynes per cm at 1550°C, while Van-Tszin-Tan et al. obtained a value of 1865k 37 dynes per cm at 1550°C. The first systematic investigation into the effect of controlled solute additions on the surface tension of iron was made by Halden and Kingery.' They showed that sulfur and oxygen were highly surface-active, whereas nitrogen was only slightly active, and carbon inactive. A subsequent investigation by Kingery indicated that two other group-6B elements, selenium and tellurium, were also surface-active. This highly surface-active nature of sulfur and oxygen has recently been substantiated by Kozakevitch and Urbainla and Van-Tszin-Tan et al. l1 Kozakevitch and Urbainl2 have also conducted an experimental survey of the effects of a number of metals on the surface tension of liquid iron. Their surface-active nature was, in all cases, less than that of the group 6B elements. The present investigation was undertaken to study in more detail the surface tensions of dilute Fe-S alloys and to measure the surface tensions of binary alloys of iron containing phosphorus, copper, and tin. The effect of sulfur additions on the surface tension of Fe-1 pct C alloys was also determined. EXPERIMENTAL PROCEDURE The sessile-drop method was employed in the present investigation. An apparatus was built similar in principle to that described by Humenik and Kingery.lS It consisted of a horizontal silica tube, which could be evacuated to pressures less than 10-5 torr, with its central portion surrounded by a water jacket within which was a high-frequency coil. This generated heat in a tantalum susceptor placed inside the silica tube, which in turn radiated heat to the specimen mounted on a recrystallized alumina plaque. Temperatures were measured by an optical pyrometer and photographs of the molten drop were taken on a fixed-focus plate camera giving a magnification of X2. Surface-tension values were determined from the resultant drop using the method described by Baes and Kellogg.l4 The high vapor pressure of molten iron made it necessary to conduct all the experiments under a 1/4 atm of argon (greater than 99.995 pct purity). The analysis of the base iron used in the investigation is given in Table I. Each sample was approximately 3 g in weight and had a hemispherical base to ensure a uniform advancing contact angle on melting. The iron alloys were prepared individually in the sessile-drop apparatus by drilling a hole in the top of each sample and adding the required amount of solute, the drops being analyzed after the experiment. This method of preparation had the advantage of ensuring a consistent minimal contamination by oxygen due to refractory attack and also allowed surface tension to be measured at the same time. Every precaution was taken to ensure that the specimen was not contaminated by grease when it was introduced into the apparatus, the samples being cleaned in acid, dried in alcohol, and rinsed in petroleum ether. All handling was done with tweezers. Once the specimen had been placed inside the susceptor, the furnace was evacuated and the Sample leveled. The furnace was then degassed at approximately 1000"C before the argon was introduced. In every case the surface tension was determined at 1550" C.

Jan 1, 1963

By E. R. Drevdahl

It has been suggested that we at the University of Arizona present a paper covering the origin, philosophy, and results of the College of Mines program in the field of computers and operations research. I have worked with the program since its beginning, and I will try to outline the developments as they have taken place. The formal development of the educational and research program in the field of Operations Research and Computer Applications at the College of Mines, University of Arizona, began in early 1957. During the year, the University offered its first formal instruction in computer programming. This was my first introduction to computers, and it did not take long to realize that this new tool had a potential that could be profitably utilized by the mining industry. In March 6f 1957, the University Computing Center began operations with its IBM 650 computer. This machine was the only computer of this size in the local area at this time, The first programming effort was in machine language and the programming cost could only be justified for repetitive-type of problems. The progress in the computer field moved very rapidly and with the development of the many compiler and assembly programs and the addition of sub routines to the computer library, the scope of problems that could profitably be investigated by computers expanded rapidly.

Jan 1, 1963

The first stage in the refining of lead blast furnace bullion is the removal of copper and this is normally done as a batch process in open kettles,A number of attempts have been made in the past to establish fontinuous processes operating in reverberatory type furnaces, but the growth of accretions in the furnace has always presented a serious problem.This has been overcome in the plant of the Broken Hill Associated Smelters Pty Ltd at Port Pirie by the construction of a reverberatory furnace and ancillary cooling system of novel design.Although a number of mechanical and metallurgical problems still remain to be solved, it is claimed that a workable continuous copper drossing process has been established.

Jan 1, 1963

By Howard M. Stainer

Published X-ray mass absorption coefficients were compiled and tabulated. These coefficients are required for various X-ray analytical techniques. Values obtained from 28 authors are listed for 87 elements with both experimental and calculated points included; the wavelengths range from 4.01 to 68 A. Representative graphs are presented for six elements (lithium, nitrogen, iron, silver, holmium, and uranium. A 37-item supplementary bibliography is also included.

Jan 1, 1963

By David A. Edgecombre

This paper discusses modern practices in the extrusion of steel. Particular emphasis is given to a description of the Ugine Sejournet method of extrusion, involving the use of glass as a hot work lubricant. Other methods are also mentioned. A brief history of extrusion is presented; present practices in the quality extrusion of tubing and solids are described; and the future potentials of the) process as a tonnage producer are briefly discussed. The advantages of extrusion and the reasons for the use of a glass lubricant, as well as the various methods of using glass, are given. The process, as described, is being used in the manufacture of large commercial quantities of stainless steel tubing and sections. This extrusion process is an essential and unique means of forming such atomic-age materials as titanium, zirconium, molybdenum and other super alloys all of which are materials required in the creation of nuclear installations.

Jan 1, 1963

By Ganesh P. Mohanty, James J. Wert

THE brittleness of the intermetallics usually render their deformation studies at ordinary temperatures using conventional techniques inadequate. On the other hand, although X-ray line broadening measurements is not a complementary technique, it provides a means for gaining limited but useful information on the cold worked state of these materials. In the present instance, a study of the effects of cold work in the lead telluride intermetallic compound was carried out by analyzing the diffraction profiles of the deformed and the corresponding annealed samples. An ingot of PbTe was prepared by induction melting high-purity lead and tellurium in a quartz crucible under an atmosphere of argon. After homo-genization, the ingot was ground to -325 mesh at room temperature, and using a polished die the cold- worked powder was pressed into the form of flat faced briquets for diffraction measurements. A spectrometer with 0.125 deg per min scanning velocity, CuKa radiation, pulse height analyzer, and a proportional counter were employed in the X-ray measurements, and the powder peaks were collected from the sample in fully cold-worked state and after it had been annealed to relieve the effects of cold work completely. For reliable estimates of the peak extremities, small angular ranges where the tails merged into the background were point counted. Fourier inversions of the experimental peaks were carried out in an IBM 705 computer using the procedures introduced by stokes.' Both the cosine and sine components of the Fourier series were used to take into account any peak assymetry arising

Jan 1, 1963

By C. H. Li, J. A. Sarteli, W. Bonfield

The stress to cause a permanent micros train of 2 x 10-6 in. per in. (defined as the microscopic yield stress) in beryllium is found to be very sensitive to surface condition. The initiation of plastic flow in as-machined specimens, which contain a high density of twins and large residual compressive stresses to a depth of about 0.010 in. from the surface, occurs by the nucleation of slip from high stress fields around twin tips in the surface layers. Removal of the damaged surface layers by chemical polishing results in an appreciable increase in the microscopic yield stress, which is attributed to the remoual of stress raising twins rather than to the release of residual stresses. IT is well known that the macroscopic mechanical properties of beryllium are very sensitive to the nature of its surface finish. Matthews and coworkers1 have shown that the tensile strength of rolled beryllium sheet can be considerably enhanced by chemical polishing, presumably due to the removal of the high concentration of notches, twins, and large residual compressive stresses normally found in the surface layers of ground specimens. There was no similar effect of surface condition on the macroscopic yield stress (the stress to produce 0.2 pct strain), a point to which we shall return. To date there have been no extensive studies on the effect of surface condition on the microstrain region of beryllium. Recent measurements2 of the stress to cause a permanent microstrain of the order of 10-6 in. per in. on machined hot pressed QMV beryllium, gave values ranging from about 600 to 3500 psi. Reasons for the considerable scatter in the results were not discussed. In this paper, we wish to show that the microstrain region of polycrystalline beryllium is, in fact, very sensitive to surface condition. The stress to cause a permanent strain of 2 x 10-6 in. per in. which for convenience we will refer to as the microscopic yield stress, can be increased by almost a factor of 2 by minimizing the amount of surface damage. The variation of microscopic yield stress is attributed to the presence of twins in the surface layers, rather than to residual compressive stresses. EXPERIMENTAL PROCEDURE The starting material for this investigation was commercial purity hot pressed QMV beryllium, with an average grain size of about 20 . The effects of surface treatment were assessed by comparing the microstructure with residual stress measurements and microstrain properties. Specimens were prepared for metallographic examination by wet grinding with 240, 400, and 600 papers, followed by polishing with a suspension of fine alumina in warm 20 pct oxalic acid. After this treatment, the surface could be examined, either in the unetched condition with polarized light, or after etching in 2 pct hydrofluoric or boiling 20 pct oxalic acid with normal light. Thin films of beryllium suitable for electron transmission study were prepared from bulk specimens by chemical polishing with hydrofluoric and phosphoric acids, and were examined in an RCA-EMU-3 electron microscope. Residual stress measurements were made by a procedure similar to that of Treuting and Read.3 Specimens 4.0 in. by 0.625 in. by 0.080 in. were prepared by three different machining procedures, namely: turning, grinding, and sawing, in order to introduce different levels of residual stresses. An electrical resistance strain gage was attached to one side of the specimen, and that surface was then protected by an acid-resistant enamel, while the opposite surface was removed by etching approximately one thousandth of an inch at a time. The change in specimen curvature in the longitudinal direction was noted and the residual stress was calculated by the following formula:

Jan 1, 1963

Jan 1, 1963

Calculations of the temperatures of metal, coke, and gas at any level in the cupola furn~ce can be carried out by means of heat balances, using data obtained from experiments with an 18 in. experimental cupola. The results can, to a certain extent, be verified by means of heat transfer calculations.The curves thus obtained, showing the variation of temperature with height in the cupola, provide a valuable picture of the heat transfer processes in a shaft 'furnace.INTRODUCTIONThe Brown Coal Research Laboratory, of the University of Melbourne, has been engaged in recent years on a programme of iron-melting tests in an experimental cupola furnace.Although the ultimate aim of this work is to develop brown coal char as a cupola fuel, most of the experimental work so far has been with conventional coke. The testing programme was designed to provide information on the effect of variables such as blast rate, metal-coke ratio, and coke size on the overall melting process, e.g. melting rate, temperature of metal tapped, and stack gas composition.However, in many cases data were obtained on conditions inside the furnace by measuring temperatures and gas compositions. The aim of the work described in this paper was to qevelop a method for using this data to obtain information on the processes taking place in the cupola.Very little research has been done on the combustion of fuels in shaft furnaces. Early work on this subject, as well as the initial stages of the Brown Coal Research Laboratory's programme, has been discussed by Evans (1959). The use of probes for obtaining information on conditions in the interior of a shaft furnace was pioneered by Belden (1913)...

Jan 1, 1963

By H. R. Ogden, E. S. Bartlett, A. G. Imgram

Notched and unnotched tensile specimens of wrought and recrystallized, oxygmted and hydro-genated tantalum and columbium were tested over a range of temperatures selected to encompass the ductile-to-brittle transition. Increasing the oxygen content of tantalum and columbium increased their strength, and raised their ductility transition temperature, but did not cause a marked deterioration of notch properties below that of commercially pure material. The adverse effects of oxygen were more pronounced for recrystallized structures than for wrought material. The effects of hydrogen are complicated by strain aging or slow strain rate hydrogen embrittlement at -105°F. However, in general, hydrogen had only a minor effect an strength, but markedly increased the effective transition tem-terature and caused a deterioration of notch properties . BCC metals including the refractory metals in Groups Va and VIa (V, Cb, Ta and Cr, Mo, W) can be expected to undergo a ductile-to-brittle transition and exhibit brittle fractures at low temperatures.' Notch embrittlement is associated with this phenomenon, and can be a serious design problem. Table I compares the tensile transition behavior and notch sensitivity of commercially pure Group Va and VIa refractory metals. The Group VIa refractory metals have considerably higher transition temperatures, and become notch sensitive at higher temperatures, than do the Group Va refractory metals. In addition, the Group VIa refractory metals are sensitive to metallurgical structure. Recrystallized structures generally have higher transition temperatures than wrought material of the same composition. The relatively poor transition behavior of the recrystallized structures of these metals is generally attributed to the segregation of interstitial impurity atoms at grain boundaries. Pronounced sensitivity to structure is not evident with commercially pure Group Va refractory metals, however. Since these metals have higher solubilities for interstitial elements than do the Group VIa metals ,4 it can be expected that higher total interstitial concentrations are necessary to develop a comparable degree of grain boundary segregation and to produce a similar sensitivity of transition temperature to structure. Increasing only the concentration of interstitial atoms in solution would tend to increase the flow stress of a metal in relation to its cleavage fracture stress and thereby raise its transition temperature, but would not be expected to cause a marked sensitivity of transition temperature to structure. A research program has been conducted at the Battelle Memorial Institute to evaluate the effects of interstitial oxygen and hydrogen on the transition behavior and notch sensitivity of tantalum and columbium, and to evaluate the effects of structure on "contaminated" material. EXPERIMENTAL PROCEDURES Notched and unnotched tensile specimens of oxygenated and hydrogenated tantalum and columbium with both wrought and recrystallized structures were tested over a range of temperatures selected to encompass the ductile-to-brittle transition Oxygen levels selected for study in both tantalum and columbium were nominally 500 and 1000 ppm, whereas nominal hydrogen contents were 150 and 500 ppm in tantalum and 150 and 300 ppm in columbium. Oxygen and hydrogen additions were made directly to 6-in. lengths of 1/2-in.-diam electron beam melted wrought bar stock, in a Sieverts Apparatus. Subsequent high-temperature annealing was required for homogenization of the oxygenated material, but was not necessary in the case of hydrogenated stock. The oxygenated and hydrogenated bars were then swaged to 1/4-in.-diam rods. Tensile specimen blanks were cut from the 1/4-in.-diam rods and annealed to achieve stress-re-

Jan 1, 1963