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By Robert B. Fulton

Staurolite, an iron aluminum silicate mineral, is used industrially as the source of aluminum in portland cement manufacture in areas where the aluminum constituent is not economically available from shale or argillaceous limestone. It is also used as a high value- in-use sand blasting agent and as a premium grade foundry sand. It is produced by E. I. du Pont de Nemours & CO. as a coproduct in titanium mineral production in Florida where it was first recovered on a commercial scale in June 1952 from the Pleistocene sand deposit known as Trail Ridge. In the Trail Ridge deposit it comprises about 36 of the heavy minerals, the principal other heavy mineral constituents being ilmenite, leucoxene, rutile, zircon, kyanite, sillimanite, and tourmaline. Staurolite and the other silicate nonconductive heavy minerals are separated from the conductive titanium minerals on high-tension separators. The silicates are then separated from one another magnetically, the staurolite being relatively magnetic. In the total processing, 200 tons of raw sand yield 7 tons of heavy mineral concentrate from which about one ton of staurolite is recovered. Staurolite production is approximately 100,000 net tpy. No other commercial production of staurolite is known. This process yields staurolite concentrates of the characteristics given in [Table 1]. These concentrates are sold as three products with the size distribution of subrounded particles shown in Table 2. All three grades are used in sand-blasting for cleaning metal, for paint removal, and for cleaning buildings. Staurolite compares favorably with lower unit cost abrasives, such as boiler slags and mineral aggregates, in applications where the abrasive is used only one time and is not recovered. Because it is hard, fine, clean, and dense it can reduce blasting time, with less material reportedly being required

Jan 1, 1975

By J. H. Wiggins

This paper first pictures the economic phase of evaporation losses and the actual evaporative conditions in handling and storing crude and gasoline in the United States; then follows a discussion of some of the theories of physics involved in evaporation loss and lastly an application of these theories to handling oil and gas on producing properties. GRANTING that about 600,000,000 bbl. of light oil will be produced in the United States this year and taking the Bureau of Mines' statement that 7 1/2 per cent. of the total crude production will be lost before the finished gasoline is shipped from the refinery, the volumetric evaporation will be 45,000,000 bbl. of the cream of the gasoline. This is a conservative figure and is equivalent to 1,890,000,000 gal. The real value of this liquid is at least 150 per cent. of the value of an equal volume of motor fuel. At only 10 c. per gal., the value lost is $189,000,000; at 15 c. per gal. the loss is $283,000,000. If 750,000,000 bbl. of light and heavy oil are produced here this year and the average price per barrel is $1.333, the gross return to producers will be $1,000,000,000 and the net returns about $200,000,000, if the cost of production is only $1 per barrel. Thus, the evaporation bill is about 20 per cent. of the gross income and is equal to the net income of the crude-oil producers. Two other comparisons with popular phases of the petroleum industry will help give an adequate conception of the evaporation problem. These are: cost of preventing evaporation compared to cost of cracked gasoline and volume of gasoline evaporated compared to volume of gasoline manufactured from natural gas.

Jan 7, 1924

By R. J. Teitel

The Pb-U system has been investigated by X-ray, thermal, and microscopic analyses. Two pyrophoric intermetallic compounds were found; UPb3 and UPb. The crystallographic structure of UPb3 is reported. A phase diagram was drawn for the system showing three eutectic and one syntectic reaction. AS a result of the interest in uranium metallurgy, the Pb-U system has been investigated. Practically no quantitative data appears in the literature concerning this system. Chips were machined from bars of high-purity uranium obtained from Ames Laboratory and the lead was 99.9 pct high-purity grade from Bel-mont Smelting & Refining Co. The chips were pickled in a dilute solution of nitric acid, washed in water and then alcohol, and dried prior to use for alloy preparation. The lead was simply sheared from the pig with no chemical treatment. Lead and uranium were placed in graphite crucibles and loaded into an induction furnace. In order to insure good alloy formation, the lead was loaded above the uranium to wash the uranium chips into the melt. After the charge was held at the desired preparation temperature for 15 to 30 min, it was allowed to cool in the crucible. The entire melting operation was accomplished in an atmosphere of helium (double charcoal refined grade with no further treatment). The procedure was to outgas the furnace by first evacuating it to 10-% m Hg, admitting helium to 8 psi gage and sealing the furnace off. An optical pyrometer focused on the charge through a hole in the crucible cover was employed for thermal measurements. Usually a 50° to 70°C correction had to be added to the instrument value. The most suitable alloy preparation temperature range was found between 1220° and 1280°C. The reason for this is explained by the phase diagram, Fig. 7. Above this temperature range two liquids separate preventing alloy formation upon cooling at a reasonable rate. On the other hand, below this range the uranium was coated with a layer of both compounds and the rate of reaction was diminished by diffusion processes. The fastest reaction rate occurred in this narrow range of temperature because only UPb coats the uranium and it evidently does not protect the uranium as well as UPb,. Apparatus and Procedures The development of apparatus and techniques was determined by the peculiar properties of the alloys. All the alloys were pyrophoric, and, consequently, the alloys had to be protected from oxidation by handling them in a dry box or inert atmosphere furnaces. Other operations performed outside of this equipment had to be done as quickly as possible. Thermal analyses were conducted in a furnace and arrangement similar to that described by the author.' Graphite crucibles having a thermocouple well in the bottom were used to contain the prepared alloy, while a helium atmosphere protected the melt from oxidation. The furnace was outgassed by pumping a 10-3 mm Hg vacuum until the furnace had been heated to 400°C. Then helium was admitted and the furnace sealed under 8 psi gage pressure. Chromel-alumel thermocouples were used for thermal analysis and the accuracy of thermal measurements was judged to be k 5°C. At first, an attempt was made to use platinum-platinum-rhodium thermocouples, but evidently lead vapors attack it at high temperatures forming low melting alloys. These lead vapors had direct access to the thermocouple because the graphite crucible was porous. A differential temperature control was used to regulate thermal analyses. The thermal gradient across an alundum tube placed between the windings and the crucible was maintained constant by a controller.

Jan 1, 1953

By C. J. Rodgers

The present day success of gravel packs to prevent or retard the migration of unconsolidated sands into the well bore is due to: (I) the use of a saline or non-aqueous, nonsolids drill fluid, (2) proper preparation of the well bore prior to gravel packing, and (3) pressure placement of the gravel. The experience gained from the "pressure pack" method of gravel packing indicates that sand-free fluid production can be maintained for a length of time sufficient to make the operation economically attractive. Data pertaining to the first 15 wells so completed by Gulf indicate that for each dollar spent to effect the completion, there will be a return of more than $2.92. The pressure pack technique of gravel packing is essentially the placing of gravel in and adjacent to the producing formations. This is done with fluid pressure and by the use of a drill fluid that will permit partial or complete loss of returns to the formation during placement. This technique was first intentionally used by Gulf in May, 1950, and since that time has been applied in more than 90 wells. Other advantages claimed for this type of completion are that the pressure placement of the gravel has a scouring effect on the casing perforations, that additional drainage channels to the well bore are created, and that the possibility of shifting of the formations adjacent to the casing is minimized and possibly prevented. During the past few years, the use of gravel to prevent or retard the migration of unconsolidated sands into the well bore has met with a favorable degree of success. Numerous methods and techniques of "gravel packing" have been used, each having its own relative merits, and with varying results. M. L. Cashion1 in 1939 ably reviewed the history of gravel packing to that time. As stated in his paper, ". .. the idea of gravel packing wells is not new." During the period 1939 to 1949, very little if any progress or change in technique in this type of completion was made. However, it was noted in some cases that during the placement of gravel, if there was a loss of drill fluid to the formation, there was a corresponding loss of gravel to the formation. Also, it was noted that in those gravel-packed completions (opposite casing perforations) that "sanded up," there was found to be an absence of gravel in the annular space between the liner and casing, although gravel had previously been placed in this space and no gravel had been removed from the well at the surface. These findings resulted in the placement of gravel with fluid pressure and by the use of a drill fluid that would permit partial or complete loss of returns to the formation during placement. Pressure placement of gravel became an accepted practice in late 1949 and early 1950. Another fact brought to light that has contributed to the current success of gravel pack completions is that drilling fluids containing solids will to some extent cause plugging of the screening medium or blocking of the producing section. The removal of these solids by chemical action, mechanical action, or a combination of the

Jan 1, 1955

By P. H. Turnock, R. D. Pehlke

The effects of mutual interactions between elements on the solubility of nitrogen in liquid iron alloys containing chrormium, columbium, molybdenurn, nickel, or silicon have been determined. The equilibrium nitrogen solubilities in the liquid iron alloys were measured by the Sieverts method. The second-order effects caused by the presence of chrormium, columbium , or silicon in the melt were found to be significant. The solubility of nitrogen in liquid iron alloys containing several alloying elements has also been measured as a function of melt temperature and nitrogen pressure. The heat of solution of nitrogen in microcomponent iron alloys has been found to be a function of the logarithnz of the activity coefficient of nitrogen, irrvespectilje of the composition of the melt. The heat of solution of nitrogen in pure liquid iron was determined to be 1265 ± 450 cal per g-atom of N over the temperatxue range 1600° to 1800°. Sieverts ' law was obeyed for all melt compositions studied in the pressure interval 0.4 to 1.0 atm. The solubility of nitrogen in liquid pure iron and in many dilute binary liquid-iron alloys has been the subject of many investigations. Pehlke and Elliott' made a comprehensive investigation on this subject in which they summarized and compared previous researches. However, the practical application of these solubility studies requires prediction of the nitrogen solubility in the multicomponent alloys encountered in operating practice. The interaction parameter as defined by wagner2 has been used to predict the behavior of a solute in a complex alloy, and a modification of this approach has met with reasonable success in several instances.'1"5 The necessity for extending the nitrogen solubility data on binary alloys is caused by the lack of direct measurements of the solubility of nitrogen in molten alloy steels. A direct comparison between measured solubilities and those predicted for multicomponent alloys based on data in binary systems has been made in only a few instances, and most of these were reviewed by Langenberg,6 who developed a graphical technique for predicting nitrogen solubilities in multicomponent iron alloys. The solubility of nitrogen has also been studied over the entire Fe-Cr-Ni ternary system by Humbert and Elliott.? Both studies compared the solubilities computed from binary iron alloy data with those measured in ternary alloys in the liquid state at 1600°C. Most of the nitrogen solubility measurements referred to above were for iron alloys at 1600°C; thus, the ability to predict nitrogen solubilities in molten iron alloys has been restricted primarily to alloys at 1600°C. Recently, Nelsson8 devised an approximate method for calculating the change in nitrogen solubility in molten iron alloys as a function of temperature, but an assumption of regular solution behavior limits the applicability of the method. Chipman and Corrigan9,10 have developed an empirical correlation. based on the activity coefficient of nitrogen in the iron alloy at 1600°C, which facilitates the estimation of nitrogen solubilities at higher temperatures. This method also has limitations, due to the necessity of calculating the activity coefficient for nitrogen in a multicomponent iron alloy at 1600°C from the nitrogen solubility data for binary iron alloys. The shortcoming of such a straightforward approach to the problem of predicting nitrogen solubilities is the disregard of mutual interactions between elements in a complex iron melt. This investigation was conducted in an attempt to provide a more reliable method of predicting nitrogen solubilities in multicomponent iron alloys. The effects of the mutual interactions between chromium, nickel, silicon, molybdenum, or columbium in iron were studied, using the Sieverts' technique1,7 to measure the effects of alloy composition, temperature, and pressure on the solubility of nitrogen in ternary liquid iron alloys.

Jan 1, 1967

By D. W. Lillie

Property changes produced by irradiation of Al-0.4 wt pet Li alloys at 270°C to a burnup of 0.155 pct of all atoms are described. Metallographic evidence of the formation of internal pores and the concentration of gases at grain boundaries is shown. Some conclusions are drawn concerning desirable property characteristics for resistance to radiation swelling. RADIATION induced gases are of great practical significance in nuclear engineering since they affect the behavior of fissionable fuels and control rod materials. In fuels the gases xenon and krypton are the major offenders, producing serious em-brittlement at low irradiation temperatures and gross swelling at high irradiation temperatures. In control rod materials containing boron, the production of helium from the B 10 (n, 0) Li7 reaction produces similar reactions. Since the trend in reactor design is for operation at increasingly high temperatures, the phenomenon of high-temperature swelling by these induced gases has been the subject of considerable recent study. The objectives of such work have been to obtain engineering information and quantitative data on the effects in specific fuels and control rods and to obtain further understanding of the mechanism of gas damage so that more intelligent corrective steps can be made. Analogue systems are often useful for the latter objective and in this case alloys containing Li are suitable in view of the reaction Li6 + n - He4 + He 4. Both products are gases and no serious radiation problem is produced to complicate post irradiation handling. Considerable caution is, of course, necessary in any operations in which tritium release is possible. The present program was initiated to provide a detailed study of the effects of He + H3 generated by irradiation in Li-bearing alloys. The results on Mg-Li solid solution alloys have been reported elsewhere.' This paper presents information on irradiation of an A1-0.4 pct Li alloy in which the lithium was present as highly enriched Li6 in order to maximize the radiation burnup. PROCEDURE The original intent in the selection of the alloy content was to have Li in solid solution at all temperatures. It became apparent, however, that the solubility of Li in A1 was substantially lower than that reported in the original reference consulted.' This was substantiated by the work of Nowak3 who reported solubility of less than 0.01 pct Li at 100°C. The alloy used (0.4 pct Li) was therefore two phase at room temperature. The irradiation temperature was estimated to be about 270° C, and at that temperature all or almost all of the Li would be soluble under equilibrium conditions. The precise state of the alloy under irradiation is not known. Aluminum used was 99.996 pct purity (max. impurities Si 0.002 pct, Mg 0.001 pct, Fe 0.0005 pct, and Cu 0.0005 pct). The lithium was obtained from Oak Ridge National Laboratory; 96.1 + 0.1 pct of the lithium was ~i~, but chemical impurities were 0.25 pct Ca, 0.05 pct Fe, 0.02 pct Na, 0.02 pct Cu, 0.01 pct Sr, and 0.01 pct Ba. The two metals were melted in an alumina crucible in a resistance heated furnace in an atmosphere of helium. A l-in. ingot was cast in an iron mold, machined to %-in. round, hot swaged (350°C) to 0.080-in. round, cold swaged to 0.060-in. round, and finally cold drawn to 0.040-in. round. Four-inch wire lengths were then cut and annealed at 250°C for 4 hr in helium. Irradiations were carried out in a VT hole in the Argonne CP-5 reactor. The wires were held in an aluminum jig, sixteen wires per capsule, and were maintained in a helium atmosphere for maximum heat transfer. Eight wires of pure aluminum and eight of Al-Li alloy were placed in each capsule. Argome Laboratory statements were accepted as establishing flux and exposure levels. These were based on previous experience and flux map-

Jan 1, 1961

By D. C. Jillson

WORK in recent years1-' has indicated a complexity of the processes of deformation of metal crystals not previously appreciated and not fully accounted for by any hypothesis so far advanced. Furthermore, the nature and mechanism of formation of nuclei of recrystallization have not been determined precisely. The deformation of single crystals of zinc has been studied frequently, but the purity of the zinc and the perfection of the specimens sometimes have been given little consideration. Methods have been developed recently that readily yield zinc single-crystal specimens of high quality.5 In the present work, such specimens were deformed in various ways under various conditions, and deformed specimens were annealed to obtain information regarding recovery, recrystallization, and grain growth. The paper attempts to correlate and evaluate previous data, as well as to present new data, in order to determine areas in which more detailed work might be done most profitably. Tests at temperatures from the freezing point (419.46°C) to room temperature revealed glide only on basal planes in a close-packed direction (100)*, as reported by Mark, Polanyi, and Schmid6 and others. Markings probably similar to those observed by Kolesnikov7 and Boas and Schmid8 were noted in specimens stretched at elevated temperatures, but it seemed clear that these were not caused by prismatic or pyramidal slip (see second paragraph of section on Phenomena Involving Bending of the Basal Plane). Twinning Twinning on the octahedral plane of a face-centered cubic metal has been pictured as a process of simple homogeneous shearing along that plane in a [112] direction. It was recognized by Mathewson and Phillipsv and others""" that the (102) twinning of zinc required a somewhat more complex mechanism and might be considered as a homogeneous shearing of (102) planes in a [211] direction plus slight adjustments of atoms to positions of greater stability or lower energy, or as a single movement of each of the atoms in the same sense into the final positions. Gough and Cox" modified Mathewson's mechanism to obtain a more stable lattice configuration, but it is not clear that they succeeded, and their mechanism requires movement of some of the atoms in a sense opposite to that of the overall twinning movement. They also suggested that twinning may occur as a result of previous basal slip. This conclusion was based on the observation that twinning caused by alternating torsion was clearest and most profuse at positions for maximum basal slip rather than for maximum stress on (102) planes in the close-packed direction (not the twinning direction), and no mechanism was described. It might be wondered whether resolution of stresses on the twinning plane in the twinning direction would have afforded a simpler explanation. If twinning is essentially a simple homogeneous shearing along the twinning plane, it would seem that twins should grow by a smooth, continuous mechanism, and, indeed, that a simple reversal of stresses should reverse the shearing and de-twin the crystal. Cylindrical tablets 1/8 to 1/4 in. thick were cleaved from singlle-crystal specimens and were squeezed, perpendicular to a second-order prism plane, to give a tensile stress perpendicular to a first-order prism plane. A "click" was heard and a thin, needle-like twin appeared on the basal cleavage face. If squeezing was continued smoothly, the twin, viewed at magnifications up to X500, grew smoothly and quietly (fig. 1). X-ray examination verified that the twinning was of the (102) type. Rotating the compression axis 90" to reverse the stress then caused a smooth, continuous shrinkage and ultimate disappearance of the twin (fig. 2). The squeezing also caused a rumpling of the basal

Jan 1, 1951

IN comparing the living conditions of the worker or peasant of the past with those existing today, his-torians might point out many strange contrasts. From the Doomsday Book we learn that at the time of Wil-liam the Conqueror the 1,375,000 inhabitants of Eng-land and Wales owned less than 1000 horses and 5000 oxen. Even as recently as 1871 when England and Wales had a population of 31,845.000, the total number of horses in the country was estimated at 1,110,000. Compare the necessary drudgery of labor in those days with conditions in Canada today where a population of less than ten million people own 3,500,000 horses. Re-member that there is also a turbine installation in` this country of more than four million horse-power, besides steam boilers and locomotive and automobile engines which reduce the traction and hand labor of the farm and factory. Frequently, poetic license has glossed over the poverty and hardship of the common people in the "good old days," and the imagination has created an idyllic world, far from being justified by the condi-tions which actually prevailed. Simon Patten's de-scription of the Middle Ages as "A Thousand Years Without an Ice Box" came nearer portraying the true situation. No one is likely to forget that the discovery of America was an incident in Europe's attempt to find a short route to the Indies, but the fact is usually for-gotten that the summer diet in Europe in 1400-an ice-less age-was such that spices were more precious than gold. Though the glamor of the Indies may never sur-round the modern refrigerator, certainly the modern housewife is likely 'to feel that the applied art called "cookery? may attain to higher levels with the assist-ance-6f such an adjunct. Those who have spoken slightingly of the uniformity of the modern apartment and have eulogized some of the exceptional hand-made furniture which has been bequeathed by former generations, have failed to com-pare modern house furnishings with those in the typical peasant's hovel. Machine-made furniture, though with-out particularly good lines, contrasts quite favorably with the pile of rags in the corner, and the poorest gas or oil stove is better than an open fire on a dirt floor. The scientist's application of the theories of physics, chemistry, biology and mathematics .to practical prob-lems has brought about a series of kaleidoscopic trans-formations in agriculture, industry and commerce. Large scale production, improved means of communica-tion and the prevailing higher standard of living are terms which imply a very human meaning when in-terpreted as actual changes in individual living. Though the student and the teacher may deprecate the influence of commercialism upon science, humanity as a whole has received great benefits from the close relationship which has developed between science and industry, and industry in turn has done much for science through the building and endowment of laboratories and by supply-ing funds to maintain research workers.

Jan 11, 1927

By David T. Peterson

Calcium metal was found to deoxidize thorizcm at 1000° to 1200° C. The reaction kinetics were determilled and related to the diffusion coefficients of oxygen in thorium. The solubility of oxygen in thorium, the minimum oxygen concentration, and the diffusion coefficient were determined from 1000° to 1200°C. This firocess results in the lowest oxygen concentrations zohich have been reported for thorium metal. FOR many years it has been known that calcium metal will reduce thorium oxide to thorium metal. This reaction has been the basis for several methods of preparing thorium metal. From the equations giv-by Kubaschewski and vans, ' AF" for the reaction Cao, + Tho,(,) - CaO(,, + Th(,) was calculated and found to be -3.4 kcal at 1000°C, -2.5 kcal at llOO°C, and -2.0 kcal at 1200°c. Thorium is very slightly soluble in liquid calcium, and the solubility of calcium in solid thorium is very low. Consequently these metals would be in essentially their reference states. If thorium containing oxygen were equilibrated with liquid calcium between 1000° and 1200°C, the oxygen content of the thorium would have to be below the solubility limit in thorium. Oxygen is one of the impurities most difficult to remove from thorium and is the most abundant impurity in metal prepared by almost all known methods. Fortunately, oxygen does not have a large influence on the properties of thorium because the solubility in solid thorium is very low. EvenT in thorium containing 100 ppm of 0, particles of thorium oxide can be observed in the microstructure. In view of the incompatibility of thorium oxide and liquid calcium and the low solubility of thorium oxide in thorium, the deoxidation of thorium by this method was investigated. For thorium containing an amount of oxygen well in excess of the solubility limit, the reaction should proceed in the following sequence. The oxygen content of the thorium matrix near the surface would be depleted by the diffusion of oxygen to the surface. At the surface, the oxygen would react with calcium to form calcium oxide. To maintain equilibrium within the thorium, thorium oxide would dissolve to keep the matrix saturated. Consequently, the thorium-oxide particles would disappear first at the surface and then the particle-free rim would grow in thickness. If the rate-controlling step were the diffusion of oxygen through this layer of thorium which was growing in thickness in direct proportion to the amount of oxygen removed, the well known parabolic time law should be observed. If the oxygen concentration at the surface of the thorium and at the inner surface of the deoxidized rim were known, the diffusion coefficient of oxygen in thorium could be calculated from the parabolic rate constant. EXPERIMENTAL PROCEDURE The thorium metal used in this study was prepared by calcium reduction of ThF, by the method described by Wilhelm.' The analysis of this metal is given in Table I. The carbon was determined by combustion, the oxygen by the HC1-insoluble residue method, nitrogen by the Kjeldahl method, and the other elements by emission spectroscopy. A section of this ingot was hot rolled at 600°C to 1/4 and 1/8-in. thick plates. Specimens approximately 7/8 in. square were cut from these plates, and all surfaces of the specimens were cleaned and smoothed by filing with a clean file. Individual specimens were placed in 1-in. diam by 2-in.-long tantalum capsules. Approximately 1 g of clean, high-purity calcium was placed in the capsules and an end closure arc-welded in place. The tantalum capsules were sealed in Inconel crucibles to protect the reactive metals from oxidation. The entire loading procedure was done in a glove box filled with pure argon. The loaded crucibles were placed in a muffle furnace, controlled within 2OC of the desired temperature, for a measured length of time. After the specimen had cooled to room temperature, it was sectioned perpendicular to the large faces and through the mid-point of two of the sides. The sectioned specimen was mounted and polished through Linde A abrasive. The rim which was free of thorium-oxide particles could be clearly observed microscopically as mechanically polished. Twenty measurements of the thickness of the rim were made at equally spaced points far enough from the end of the

Jan 1, 1962

By Nobuhiro Takahashi

PROLOGUE The Yaguki mine, which is located near the southern end of the Tohoku region, Japan, near the coast of the Pacific Ocean, had had a long history as a copper mine, but had not been operated since 1925. About 30 years later it was reopened by Nittetsu Mining Company, and in 1958 a small flotation and magnetic separation plant, a so-called test plant, started production. The ball mill the author first met, a 8x4x4x7 ft tricone mill, called No.1 mill, had started running at that time. With his experience in initial, running of this mill he realized that the ball mill was not simply a preparatory process to flotation, but a determinant factor for flotation performance, an energy-consuming and costly process, and that its operation control was an important task in the plant (1). The working part of an operating ball mill is the ball load inside, whose properties govern the grinding performance. Its size distribution affects the efficiency greatly and the capacity is nearly proportional to its weight. When a ball mill operates for a long period of time with a constant and consistent addition of renewal balls, wear and renewal of balls are balanced, and an equilibrium ball load is formed. A stable equilibrium load is the primary requirement for a stable ball mill operation. However, renewal ball size would be the most influential factor affecting efficiency and capacity of operating ball mills. To improve efficiency, to increase capacity, or to get finer product, attempts to find out the optimum size assortment of renewal balls should be made. When re-

Jan 1, 1976

By P. Ramachandrarao, T. R. Anantharaman

EVER since the technique of quenching metals and alloys from the melt (splat cooling) was perfected a decade ago, it has been recognized that the grain size of products solidified by this technique may be extremely small.' The further observation that fcc metals quenched from the liquid state contain very few dislocations has led to the inference2 that metals are subjected to negligible or no stresses during the rapid solidification characteristic of the "gun" or "piston-and-anvil" technique. Evidence for the incidence of appreciable densities of stacking faults has, however, been obtained in case of some splat-cooled fcc and hcp alloys,3 although not for pure metals. In the light of these earlier observations it was considered desirable to study X-ray line-broadening effects, if any, in fcc metals rapidly cooled from the melt. In the present work pure silver (>99.99 pct), aluminum (>99.99 pct) and lead (>99.9 pct) were quenched from the liquid state from temperatures about 50°C above the melting point by the "gun technique" and the resulting foils were subjected to X-ray examination in a Philips Diffractometer. The quenched foils (up to -10 u thick) did not generally stick to the substrate surface and could be easily transferred to the Diffractometer without introducing any plastic deformation. The profiles of the first five reflections from the foils were recorded in each case with Cu Ka, radiation at the slowest available scanning speed of 1/8 deg per min. To correct for instrumental broadening, profiles were also recorded from the metals annealed in vacuo at suitable temperatures. The integral breadths of the X-ray reflections were arrived at by a procedure described earlier.' There was a distinct suggestion of preferred orientation in the recorded intensities of reflections from aluminum and lead foils. Such an effect was not observed in case of silver. In addition, the integral breadths of X-ray reflections from splat-cooled aluminum and lead were not significantly different from those recorded for the annealed metals. The analysis was therefore continued only for silver where the X-ray line broadening was appreciable. The pure diffraction broadening, B, was evaluated for each X-ray reflection (hkl) from silver from the observed, B, and instrumental, b, breadths with the aid of each of the three equations due to Scherrer,5 Anantharaman and Christian,6 and Warren and Biscoe,7 respectively: Bs= B-b BAC=B- b2/B Table I gives the values of particle size, 71, the lattice strain, E, arrived at by the use of the following well-known relations and on the assumption that all observed diffraction broadening could be attributed to lattice strain or particle size, respectively: E = 1/4 cos ? n= B cos ? where A is the wavelength of X-radiation and 0 is the Bragg angle. As no significant peak shifts or asymmetry could be detected in the profiles from the foils, the possibility of any significant contribution due to twins or stacking faults was ruled out. The absence of faults is by no means surprising since pure silver is known to develop stacking faults only on severe deformation and the stacking fault densities recorded so far for even silver filings have been extremely low.' The very low values for percentage mean deviation from the mean value for the particle size in Table I strongly suggest that all observed broadening in splat-cooled silver can be attributed only to small particle size. This conclusion receives further support from the lowest mean deviation recorded for data computed from the Scherrer equation based on Cauchy profiles that are considered characteristic of particle size broadening. Further analysis for separation of particle size and lattice strain effects was considered unnecessary in view of the very large mean deviations obtained for strain values and also the earlier results suggesting absence of even detectable strain in metals and alloys quenched from the melt. It is to be stressed in this connection that the particles are actually grains and not cells formed by walls of high dislocation density usually encountered in deformed samples. As such, the absence of strains is not surprising. The present results are probably the first to record X-ray line broadening due only to small particle

Jan 1, 1970

By Courtenay de Kalb

THE Exposed Treasure gold-mine has, for the past four years, been one of the largest producing mines of Southern California, its annual output having constituted 1 per cent of the total gold and silver production of the entire State. At the present moment the property is idle, owing to the large quantity of water encountered oil the lower levels, which will require the installation of a powerful pumping-plant before operations can be recommenced. Moreover, a prompt change in the character of the ore has occurred at water-level, which makes imperative an extensive campaign of development in the region of the unoxidized ores before a plant adapted to their treatment can be definitely decided upon. The character of the changes encountered in these deeper ores makes the geology of this deposit a matter of importance, not only for the immediate district, but for the desert region of Southern California in general, where many mines exist having in the oxidized belt conditions that, in many respects, resemble those in the Exposed Treasure mine. The deposit is situated in an apparently isolated butte about 2.5 miles south from the town of Mojave, on the Mojave desert; The butte, though apparently isolated, is in fact geologically part of an extinct volcano, known as Soledad butte, which rises out of the plain 1,5 miles SW. of the mine, to an altitude of 4,650 ft. above sea-level. Other buttes also rise from the desert plain toward the south and east, and again to the westward, all being closely related geologically to Soledad butte,-the whole constituting a single system as to origin and time. Since the end of the period of active volcanism in this region, there has been extensive denudation, the ancient plateau having been dissected during an epoch of apparently exces-

Jan 1, 1907

By L., Ormsby

DRILLING and blasting practices in the Morenci open pit have undergone considerable modification in recent years. Changes in the character of the ground being mined, modifications of working conditions, and continuous experimentation have been the contributing factors.

Jan 1, 1950

By I. D. Hagar

WHEN the history of American business during these momentous war years is written, an absorbing chapter will be devoted to the Maclntyre Development, in northern New York. It will tell of a timely mining project, deep in the wilds of the Adirondacks, blasted into being by Axis torpedoes. It will recount the labors of 1500 engineers and workmen, miles from a highway, rail line, or power source, who built a huge enterprise in a few short months' time. And it will list these major contributions to the war effort: more than a quarter million tons per year of ilmenite, source of titanium dioxide-man's most opaque white pigment-to be used in paints for warships, tanks, guns, planes and the plants that build them; as a co-product, over 500,000 tons each year of magnetite-an important type of iron ore- to help feed the cavernous maw of America's wartime steel industry.

Jan 1, 1942

By Richard A. Queeney, Lance G. Peterson

ESTIMATES of the stacking fault free energy of copper reported in the literature show an extensive divergence of results. Based on measurements of dislocation node radii, Thornton et al.7 find the lower limit of stacking fault energy to be 60 ergs per sq cm: Jossang and coworkers4 estimate the same value should be less than 40 ergs per sq cm. Assuming stacking fault free energy to be twice the coherent twin boundary free energy, Valenzuela8 reports 72 ergs per cm, while Inman and Khan2 cite a value of 24 ergs per sq cm. which can no doubt be accounted for by almost complete absence of interstitials in solution. However, the minute concentration was sufficient to permit observable recovery of dislocation damping. Assuming a dislocation density of 1010 CM -2 and an average loop length of 0.5 , a concentration of interstitials as low as 0.01 at. ppm is sufficient to reduce dislocation damping by more than a factor of ten. The concentration of interstitial solute atoms in Ferrovac E-0.15 pct Ti was thus estimated at 0.01 at. ppm < (C + N) < 2 at. ppm. The absence at elevated temperature of strengthening due to interstitials, Fig. 1, was therefore anticipated in the titanium alloy. The temperature dependence of the flow stress below 300°K was unaffected by addition of either titanium&apos; or zirconium.&apos; Observed, however, was an initial difference in the absolute value of the flow stress below 320oK, Fig. 1. Grain size may account for the difference; the grain diameter of Ferrovac E was 30 to 45 µ and that of Ferrovac E-0.15 pct Ti 65 to 90 µ. Although second phase particles in the form of titanium carbides and nitrides precipitated in the Ferrovac E-0.15 pct Ti alloy, the spacing was too large to produce any strengthening effect. The mechanical properties measured, therefore, were inherent to the bcc lattice. 1W. C. Leslie and R. J. Sober: Trans. ASm, 1967, vol. 60, pp. 99-111. 2 H. Conrad: Journal of Metals, 1964, vol. 16, pp. 582-88. 3 A. S. Keh and W. C. Leslie: Materials Science Research. H. H. Stadelmaier and W.W.Austin, eds., vol. 1.pp. 208.50, Plenum Press, New York, 1963. 4A. S. Keh, Y. Nakada, and W. C. Leslie: Dislocation Dymmics, Rosenfield, Hahn, Bement, Jr., and Jaffe, eds., pp. 381-406, McCraw-Hill Book Co., New York, 1968. &apos;W. J. Bratina, J. T. McCrath, and H. E. Rosinger: Can. Met. Quart., in press. 6 W. J. Bratina, J. T. McGrath, and D. Mills: Suppl. Trans. Japan Inst. Metals. 1968, vol. 9, pp. 436-43. &apos;H. E. Rosinger and C. B. Craig: Can. Met. Quart., In press. %. Mills. J. T. McGrath. and W. J. Bratina: ScriptaMet,, 1968, vol. 2, pp. 311-13. The purpose of this note is to present the results of a direct measurement of the stacking fault free energy in copper. The present method avoids both the question of interaction forces of nodal dislocations and the assumption that the coherent twin boundary free energy is one-half that of a stacking fault. Fig. 1 shows a transmission electron micrograph of a stacking fault intersecting a high angle grain boundary in copper: Fig. 2 is a schematic representation of the intersecting interfaces. To produce the specimen, pure copper was rolled to 0.002 in. thickness and annealed for several hours at 875°C. These foils were strained in tension to l04 µ in. per in., and rean-nealed to 8 min. Recrystallization and/or grain growth were not observed during the second anneal, indicating that intersections such as Fig. 1 are equilibrium configurations. Many such stacking faults were observed, but few were noted as intersecting grain boundaries in well-illuminated areas. The intersection of Fig. 1 was well away from the specimen edge. Since similar defects have not been observed in fully recrystal-lized and annealed copper, it is felt that this defect is due to the tensile straining. Electron transmission

Jan 1, 1970

By F. D. Delve

RECENT studies by the author on the reduction of titanium from TiO2-bearing slags have been accompanied by difficulties that are attributed to

Jan 1, 1959

By E. N. Smith, J. C. Redmond

The increasing need for materials capable of withstanding higher operating temperatures for various applications such as gas turbine blading and other parts, rocket nozzles, and many industrial applications, has brought consideration of cemented carbide compositions. The well known usefulness of cemented carbides as tool materials is attributable to their ability to retain their strength and hardness at much higher temperatures than even complex alloys. However, it has been found that the temperatures encountered in cutting operations do not approach by several hundred degrees1 those involved in the applications mentioned above where the interest is in materials possessing strength and resistance to oxidation at temperatures of 1800°F and above. At these latter temperatures, the tool type compositions which are made up essentially of tungsten carbide are found to oxidize very rapidly and to produce oxidation products of a character which offer no protection to the remaining body. As a further consideration, the density of the tungsten carbide type compositions is high, from about 8.0 to 15.0. The refractory metal carbides as a class are the highest melting materials known as shown by Table 1 which summarizes the available data from the literature for the carbides of the elements which are sufficiently available for consideration for these uses. The density is also included in the table, since as mentioned above it is an important consideration in many of the applications for which the materials would be considered. It has been established that in the tool compositions the mechanism of sintering with cobalt is such as to result in a continuous carbide skeleton and that the properties of the sintered composition are thus essen- tially those of the carbide.2 On the hypothesis that this mechanism holds to a greater or less degree in cementing most of the refractory metal carbides with an auxiliary metal, it appears from Table 1 that titanium carbide compositions would offer possibilities for a high temperature material. Titanium carbide has extensive use for supplementing the properties of tungsten carbide in tool compositions. Although the literature contains several references to compositions containing only titanium carbide with an auxiliary metal,3,4,5,6 it may be inferred from the meager data that such compositions were deficient in strength and were considered to have poor oxidation resistance.7 Kieffer, for instance, reports the transverse rupture strength of a hot pressed TiC composition at 100,000 psi as compared to up to 350,000 psi for WC compositions. The work described herein was undertaken to determine the properties of compositions consisting of titanium carbide and an auxiliary metal and to improve the oxidation resistance of such compositions. It appeared possible that the inclusion of one or more other carbides with titanium carbide might improve the oxidation resistance and also that this might be more desirable than other means from the point of view of maintaining the highest possible softening point. Consideration of the available carbides in Table 1 suggests tantalum and columbium carbides because of their high melting points and general refractoriness. The work on improving oxidation resistance was concentrated on the addition of tantalum carbide or mixtures of tantalum and columbium carbide. The auxiliary metals used included cobalt, nickel and iron. It was also desired to learn the general physical properties of these compositions. Experimental Procedure The compositions used in this study were made by the usual powder metallurgy procedure applicable to cemented tungsten carbide compositions. The powdered carbide or carbides and auxiliary metal were milled together out of contact with air. In some cases cemented tungsten carbide balls and in other instances steel balls were used to eliminate any effect of tungsten carbide contamination. A temporary binder, paraffin, was then included in the mix and slugs or ingots were pressed with care to obtain as uniform pressing as possible. The ingots were presintered and the various shapes of test specimens were formed by machining, making the proper allowance for shrinkage during sintering. Thereafter the shapes were sintered in vacuum at temperatures of from 2800 to 3500°F. Final grinding to size was carried out by diamond wheels under coolant. The titanium carbide used contained a minimum of 19.50 pet total carbon and a total of 0.50 pet metallic impurities as indicated by chemical and spectrographic analysis. It was found by X ray diffraction examination with

Jan 1, 1950

By Gene D. Clayton, Robert R. Dimock

A time-consuming and expensive preshearing program to minimize the adverse effects of blasting on slope stability at Kennecott Copper Corp.&apos;s Ruth Pit in east-central Nevada has been eliminated in favor of down-the-hole, nonelectric delayed blasting which can produce a smooth wall effect and improve blast fragmentation. The new blasting approach resulted from a Kennecott engineering investigation aimed at improving the stability of the extremely variable rock conditions found throughout the pit by reducing the vibrational energy imparted to the walls with conventional bench blasts.

Jan 4, 1977

By Mitchell, Edmund I.

VARIOUS suggestions as to proper fees for engineering services have been put forth by individual practitioners and by the American Institute of Consulting Engineers, the Connecticut Society of Civil Engineers, the Iowa Engineering Society and the Mahoning Valley (Ohio) Engineers, for the guidance of both the engineer and his client. The American Institute of Architects also has a schedule of minimum charges (revised 1908). So far as can be determined, however, the four national societies representing civil, mining, mechanical and electrical engineering have never given consideration to this question. An examination of technical periodicals published during the past decade shows that these schedules make provision for three methods of charging; i.e., (A) a percentage of the cost of the completed project; (B) a per diem rate; and (C) a fixed sum. Suggested minimum charges are as follows:

Jan 1, 1921

By J. B. Cohen

EARLY investigators1-4 reported that additions of beryllium to silver caused embrittlement. The in-termetallic phases which are now known to exist5,&apos; were not known at the time. Solidification appeared to occur by a simple eutectic reation.4,7 (The primary beryllium-rich phase appeared globular, when the liquidus temperature was near the melting point of pure beryllium, and angular when the liquidus was much lower; in discussion of Sloman&apos;s work,4 it was suggested that this difference was due to an intermetallic compound which was not revealed by the polishing technique.) In the investigation reported here, it was found that if the compounds now known to exist were avoided, certain beryllium-silver alloys containing large amounts of the primary beryllium phase possessed sufficient ductility to be cold formed. Alloys containing 14 and 20 at. pct Ag were prepared from vacuum-cast beryllium containing 1.0 to 1.2 pct impurities and silver, 99.99+ pct pure. The elements were melted together by induction in beryllia or alumina crucibles under argon at less than 1 atm pressure. The cooling rate was adjusted by regulating the temperature of the melt and by reducing the power to zero without stopping the water flow in the induction coils, which were in contact with the crucible. Ingots were about 0.75 in. in diam with a grain size of 0.12 to 0.25 in. Microscopic investigation of transverse or longitudinal sections of an ingot cast from a temperature well above its melting point showed that, in general, the compounds did not form, presumably because of rapid cooling; the alloys consisted of beryllium-rich particles in a silver-rich matrix as shown in Fig. 1. A eutectic structure was not observed, probably .due to the low beryllium concentration of the eutectic composition and eutectic divorcement. Within a given grain, the small globules of the primary phase were all oriented in the same direction, as indicated by examination under polarized light; the orientation varied from grain to grain. This suggested that the globules were branches of the same dendrites. If cooling was too slow, a third constituent was observed in the microstructure; because it formed around the primary beryllium-rich globules it was Fig. 1—Ag-Be alloy, 18.6 at. pct Ag, as-cast. Bright field illumination. Etched with an aqueous solution of NH,OH and H2O2. X500. Reduced approximately 21 pct for reproduction. probably the 6 compound. A thin ring around an ingot often contained this constituent. When this compound was present in large quantities, or the silver segregated so that large regions occurred with the beryllium-rich globules in contact, sections from the ingot were brittle. When the compound was initially absent, it was possible to carry out reductions in thickness of 50 pct by cold rolling with only limited edge cracking; failure did not occur until reductions of 80 pct. A typical cross section after cold rolling is shown in Fig. 2. After simple bend tests, microcracks were found; these apparently were difficult to propagate in the two-phase structure, as the specimens continued to behave in a ductile manner after the cracks appeared. Similar cracks would probably be closed during rolling. It is apparent in Fig. 2 however, that the primary beryllium particles undergo extensive plastic deformation. Hardness values of the alloys indicated that some work-hardening occurred during cold working. Fig. 2—Ag-Be alloy, 18.6 at. pct Ag, reduced 83 pct in thickness by cold rolling. Bright field illumination. Etched with an aqueous solution of NH,OH and H2O2. X500. Reduced approximately 21 pct for reproduction.

Jan 1, 1961